首页 期刊 论文 学科刊群 资讯 加盟 关于
EN
image
Article(id=1153986643288642061, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986642063905290, articleNumber=null, orderNo=null, doi=10.19812/j.cnki.jfsq11-5956/ts.20241018002, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1729180800000, receivedDateStr=2024-10-18, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1753061455795, onlineDateStr=2025-07-21, pubDate=1739548800000, pubDateStr=2025-02-15, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1753061455795, onlineIssueDateStr=2025-07-21, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1753061455795, creator=13701087609, updateTime=1753061455795, updator=13701087609, issue=Issue{id=1153986642063905290, tenantId=1146029695717560320, journalId=1149652044408987649, year='2025', volume='16', issue='3', pageStart='1', pageEnd='316', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=0, createTime=1753061455502, creator=13701087609, updateTime=1760070725729, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1183385652272968023, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986642063905290, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1183385652272968024, tenantId=1146029695717560320, journalId=1149652044408987649, issueId=1153986642063905290, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=303, endPage=308, ext={EN=ArticleExt(id=1153986643640963598, articleId=1153986643288642061, tenantId=1146029695717560320, journalId=1149652044408987649, language=EN, title=Determination of residual levels of gamithromycin in raw milk by high performance liquid chromatography-tandem mass spectrometry, columnId=1151895321388347923, journalTitle=Journal of Food Safety & Quality, columnName=Food Analysis and Detection, runingTitle=null, highlight=null, articleAbstract=

Objective To establish an analytical method for the determination of gamithromycin residues in raw milk based on matrix external standard method combined with through type purification column (EMR-Lipid) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acid acetonitrile, purified by the EMR-Lipid through type purification column, gradient eluted through a BEH C18 chromatographic column. Detection was carried out in the electrospray positive ion multiple reaction mode, and quantification was performed using the matrix external standard method. Results Calibration curves were linear in the range of 0.5-20.0 ng/mL with correlation coefficients more than 0.99. The limit of detection (LOD) was 0.5 μg/kg, limit of quantification (LOQ) was 1.0 μg/kg. Gamithromycin showed a matrix enhancement effects in raw milk. After matrix blank curve correction, the average recoveries of gamithromycin at different spiked concentrations ranged from 74.0% to 77.0%, and the relative standard deviations (RSD) of the determination results were from 3.92% to 4.57%. Conclusion This method is accurate, sensitive, stable, simple, and easy to operate, it can be used for the rapid determination and quantitative analysis of gamithromycin residues in raw milk, providing technical support for monitoring the residual amount of gamithromycin in raw milk.

, correspAuthors=Ke-Jing LI, authorNote=null, correspAuthorsNote=null, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=null, magXml=null, pdfUrl=null, pdf=null, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=null, mapNumber=null, authorCompany=null, fund=null, authors=null, authorsList=Mo LI, Xin ZHAO, Hong-Ji ZHANG, Ting ZHOU, Qian WANG, Xiu-Ping ZHAO, Ke-Jing LI), CN=ArticleExt(id=1153986679024112008, articleId=1153986643288642061, tenantId=1146029695717560320, journalId=1149652044408987649, language=CN, title=高效液相色谱-串联质谱法测定生乳中加米霉素残留量, columnId=1151895321958773274, journalTitle=食品安全质量检测学报, columnName=食品分析与检测, runingTitle=null, highlight=null, articleAbstract=

目的 建立以基质外标法定量, 通过式净化柱(EMR-Lipid)结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定生乳中加米霉素残留量的分析方法。方法 样品经酸性乙腈提取后, 由EMR-Lipid通过式净化柱净化, 通过BEH C18色谱柱进行梯度洗脱, 电喷雾正离子多反应模式进行检测, 基质外标法定量。结果 加米霉素在0.5~20.0 ng/mL质量浓度范围内呈现良好线性关系, 线性相关系数大于0.99; 检出限(limit of detection, LOD)为0.5 μg/kg; 定量限(limit of quantification, LOQ)为1.0 μg/kg; 加米霉素在生乳中表现为基质增强效应, 经基质空白曲线校正后, 加米霉素在不同添加浓度平均回收率为74.0%~77.0%, 测定结果的相对标准偏差(relative standard deviation, RSD)为3.92%~4.57%。结论 该方法准确、灵敏、稳定、简单易操作, 可以用于生乳中加米霉素残留量快速测定及定量分析, 为生乳中加米霉素残留监控提供技术支持。

, correspAuthors=李克静, authorNote=null, correspAuthorsNote=
* 李克静(1981—), 女, 高级工程师, 主要研究方向为食品安全检测。E-mail:
, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=og6jb2jc2GRQCATFtq2CbQ==, magXml=Oxb9F3uo4FzzU+Wrwp1Gew==, pdfUrl=null, pdf=jZw8RDhlhKDkNSJry+8ikQ==, pdfFileSize=null, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=null, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=XOEnOg3GuO2uspkf1kh5mw==, mapNumber=null, authorCompany=null, fund=null, authors=

李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

, authorsList=李默, 赵鑫, 张虹吉, 周婷, 王倩, 赵修平, 李克静)}, authors=[Author(id=1183428254036800117, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, orderNo=0, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=825871647@qq.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1183428254116491895, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254036800117, language=EN, stringName=Mo LI, firstName=Mo, middleName=null, lastName=LI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1183428254179406456, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254036800117, language=CN, stringName=李默, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=中检科(北京)测试技术有限公司, 北京 100176 , bio={"content":"

李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

"}, bioImg=null, bioContent=

李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])]), Author(id=1183428254238126714, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, orderNo=1, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1183428254305235580, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254238126714, language=EN, stringName=Xin ZHAO, firstName=Xin, middleName=null, lastName=ZHAO, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1183428254372344445, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254238126714, language=CN, stringName=赵鑫, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=中检科(北京)测试技术有限公司, 北京 100176 , bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])]), Author(id=1183428254431064703, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, orderNo=2, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1183428254498173569, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254431064703, language=EN, stringName=Hong-Ji ZHANG, firstName=Hong-Ji, middleName=null, lastName=ZHANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1183428254552699522, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254431064703, language=CN, stringName=张虹吉, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=中检科(北京)测试技术有限公司, 北京 100176 , bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])]), Author(id=1183428254607225476, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, orderNo=3, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1183428254691111558, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254607225476, language=EN, stringName=Ting ZHOU, firstName=Ting, middleName=null, lastName=ZHOU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1183428254758220423, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254607225476, language=CN, stringName=周婷, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=中检科(北京)测试技术有限公司, 北京 100176 , bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])]), Author(id=1183428254812746377, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, orderNo=4, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1183428254879855243, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254812746377, language=EN, stringName=Qian WANG, firstName=Qian, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1183428254988907148, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428254812746377, language=CN, stringName=王倩, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=中检科(北京)测试技术有限公司, 北京 100176 , bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])]), Author(id=1183428255056016014, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, orderNo=5, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=null, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1183428255123124880, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428255056016014, language=EN, stringName=Xiu-Ping ZHAO, firstName=Xiu-Ping, middleName=null, lastName=ZHAO, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1183428255177650833, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428255056016014, language=CN, stringName=赵修平, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=中检科(北京)测试技术有限公司, 北京 100176 , bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])]), Author(id=1183428255261536915, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, orderNo=6, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=likejing@ccic.com, emailSecond=null, emailThird=null, correspondingAuthor=1, authorType=1, ext={EN=AuthorExt(id=1183428255320257173, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428255261536915, language=EN, stringName=Ke-Jing LI, firstName=Ke-Jing, middleName=null, lastName=LI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=*, address=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1183428255378977430, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, authorId=1183428255261536915, language=CN, stringName=李克静, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=*, address=中检科(北京)测试技术有限公司, 北京 100176 , bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])])], keywords=[Keyword(id=1183428255550943895, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, orderNo=1, keyword=gamithromycin), Keyword(id=1183428255622247064, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, orderNo=2, keyword=high performance liquid chromatography-tandem mass spectrometry), Keyword(id=1183428255685161625, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, orderNo=3, keyword=EMR-Lipid through type purification column), Keyword(id=1183428255739687578, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, orderNo=4, keyword=raw milk), Keyword(id=1183428255806796443, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, orderNo=1, keyword=加米霉素), Keyword(id=1183428255878099612, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, orderNo=2, keyword=高效液相色谱-串联质谱法), Keyword(id=1183428255936819869, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, orderNo=3, keyword=EMR-Lipid通过式净化柱), Keyword(id=1183428256024900254, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, orderNo=4, keyword=生乳)], refs=[Reference(id=1183428257547432627, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2020, volume=128, issue=null, pageStart=118123, pageEnd=null, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=XIAO TS, YANG YQ, ZHANG YX, journalName=Research in Veterinary Science, refType=null, unstructuredReference=XIAO TS, YANG YQ, ZHANG YX, et al. Efficacy of gamithromycin injection administered intramuscularly against bacterial stwine respiratory disase[J]. Research in Veterinary Science, 2020, 128: 118123., articleTitle=Efficacy of gamithromycin injection administered intramuscularly against bacterial stwine respiratory disase, refAbstract=null), Reference(id=1183428257601958580, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=https://www.emea.Europa.eu/vetdocs/PDFs/EPAR/V-129-en6.pdf, language=null, rfNumber=[2], rfOrder=1, authorNames=European Medicines Agency Veterinary Medicines and Inspections, journalName=null, refType=null, unstructuredReference=European Medicines Agency Veterinary Medicines and Inspections. V-129-en6[EB/OL]. (2016-07-25) [2024-10-18]. https://www.emea.Europa.eu/vetdocs/PDFs/EPAR/V-129-en6.pdf, articleTitle=V-129-en6, refAbstract=null), Reference(id=1183428257660678837, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=http://www.ema.europa.eu/docs/enGB/documentlibrary/MaximumResidueLimits-Summaryofopinion/2014/07/WC500169766.pdf, language=null, rfNumber=[3], rfOrder=2, authorNames=EMA, journalName=null, refType=null, unstructuredReference=EMA. Committee for medicine products for veterinary use[DB/OL]. [2024-10-18]. http://www.ema.europa.eu/docs/enGB/documentlibrary/MaximumResidueLimits-Summaryofopinion/2014/07/WC500169766.pdf, articleTitle=Committee for medicine products for veterinary use, refAbstract=null), Reference(id=1183428257711010486, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2018, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=3, authorNames=中华人民共和国农业农村部, journalName=中华人民共和国农业农村部公告第15号, refType=null, unstructuredReference=中华人民共和国农业农村部. 中华人民共和国农业农村部公告第15号[Z]. 2018., articleTitle=null, refAbstract=null), Reference(id=1183428257773925047, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2018, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[4], rfOrder=4, authorNames=Ministry of Agriculture of the PRC, journalName=Announcement No. 15 of the Ministry of Agriculture and Rural Affairs of the People's Republic of China, refType=null, unstructuredReference=Ministry of Agriculture of the PRC. Announcement No. 15 of the Ministry of Agriculture and Rural Affairs of the People's Republic of China[Z]. 2018., articleTitle=null, refAbstract=null), Reference(id=1183428257862005432, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2019, volume=25, issue=4, pageStart=603, pageEnd=610, url=null, language=null, rfNumber=[5], rfOrder=5, authorNames=PAPATSIROS V, TZIKA E, ATHANASIOU L, journalName=Microbial Drug Rssisitance, refType=null, unstructuredReference=PAPATSIROS V, TZIKA E, ATHANASIOU L, et al. In vivo effectiveness of injectable antibiotics on the recovery of acute Actinobacillus pleuropneumoniae-infected pigs[J]. Microbial Drug Rssisitance, 2019, 25(4): 603-610., articleTitle=et al. In vivo effectiveness of injectable antibiotics on the recovery of acute Actinobacillus pleuropneumoniae-infected pigs, refAbstract=null), Reference(id=1183428257924919993, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2017, volume=40, issue=4, pageStart=406, pageEnd=410, url=null, language=null, rfNumber=[6], rfOrder=6, authorNames=BERLIN S, RANDOW T, SCHEUCH E, journalName=Journal of Veterinary Pharmacology and Therapeutics, refType=null, unstructuredReference=BERLIN S, RANDOW T, SCHEUCH E, et al. Pharmacokinetics and pulmonary distribution of gamithromycin after intravenous administration in foals[J]. Journal of Veterinary Pharmacology and Therapeutics, 2017, 40(4): 406-410., articleTitle=Pharmacokinetics and pulmonary distribution of gamithromycin after intravenous administration in foals, refAbstract=null), Reference(id=1183428257979445946, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=http://www.ema.europa.eu/docs/enGB/documentlibrary/EPAR-ScientificDiscussion/veterinary/000129/WC500068716, language=null, rfNumber=[7], rfOrder=7, authorNames=The European Medicines Agency, journalName=null, refType=null, unstructuredReference=The European Medicines Agency. Zactran EPAR scientific discussion[EB/OL]. (2018-07-30) [2024-12-15]. http://www.ema.europa.eu/docs/enGB/documentlibrary/EPAR-ScientificDiscussion/veterinary/000129/WC500068716, articleTitle=Zactran EPAR scientific discussion, refAbstract=null), Reference(id=1183428258042360507, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2023, volume=8, issue=57, pageStart=19, pageEnd=24, url=null, language=null, rfNumber=[8], rfOrder=8, authorNames=孙晨明, 高嫣珺, 徐亚亚, journalName=中国兽药杂志, refType=null, unstructuredReference=孙晨明, 高嫣珺, 徐亚亚, 等. UPLC-MS/MS测定牛血浆中加米霉素方法的建立[J]. 中国兽药杂志, 2023, 8(57): 19-24., articleTitle=UPLC-MS/MS测定牛血浆中加米霉素方法的建立, refAbstract=null), Reference(id=1183428258130440892, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2023, volume=57, issue=8, pageStart=19, pageEnd=25, url=null, language=null, rfNumber=[8], rfOrder=9, authorNames=SUN CM, GAO YJ, XU YY, journalName=Chinese Journal of Veterinary Drug, refType=null, unstructuredReference=SUN CM, GAO YJ, XU YY, et al. Establishment of UPLC-MS/MS method for determination of streptomycin in bovine plasma[J]. Chinese Journal of Veterinary Drug, 2023, 57(8): 19-25., articleTitle=Establishment of UPLC-MS/MS method for determination of streptomycin in bovine plasma, refAbstract=null), Reference(id=1183428258310795965, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=null, pageEnd=null, url=http://www.fda.gov/downloads/animalveterinary/products/approvedanimaldrugproducts/foiadrugsummaries/ucm277806, language=null, rfNumber=[9], rfOrder=10, authorNames=FDA, journalName=null, refType=null, unstructuredReference=FDA. Freedom of information summary original new animal drug application[EB/OL]. (2013-10-24) [2025-1-19]. http://www.fda.gov/downloads/animalveterinary/products/approvedanimaldrugproducts/foiadrugsummaries/ucm277806, articleTitle=Freedom of information summary original new animal drug application, refAbstract=null), Reference(id=1183428258415653566, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2018, volume=39, issue=12, pageStart=180, pageEnd=184, url=null, language=null, rfNumber=[10], rfOrder=11, authorNames=李先强, journalName=动物医学进展, refType=null, unstructuredReference=李先强. 兽用加米霉素研究与应用现状[J]. 动物医学进展, 2018, 39(12): 180-184., articleTitle=兽用加米霉素研究与应用现状, refAbstract=null), Reference(id=1183428258499539647, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2018, volume=39, issue=12, pageStart=180, pageEnd=184, url=null, language=null, rfNumber=[10], rfOrder=12, authorNames=LI XQ, journalName=Advances in Veterinary Medicine, refType=null, unstructuredReference=LI XQ. The research and application status of animal grade streptomycin[J]. Advances in Veterinary Medicine, 2018, 39(12): 180-184., articleTitle=The research and application status of animal grade streptomycin, refAbstract=null), Reference(id=1183428258616980160, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2016, volume=44, issue=31, pageStart=150, pageEnd=152, url=null, language=null, rfNumber=[11], rfOrder=13, authorNames=杨新艳, 侯林, 周德刚, journalName=安徽农业科学, refType=null, unstructuredReference=杨新艳, 侯林, 周德刚. 加米霉素的研究进展[J]. 安徽农业科学, 2016, 44(31): 150-152, 168., articleTitle=加米霉素的研究进展, refAbstract=null), Reference(id=1183428258721837761, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2016, volume=44, issue=31, pageStart=150, pageEnd=152, url=null, language=null, rfNumber=[11], rfOrder=14, authorNames=YANG XY, HOU L, ZHOU DG, journalName=Anhui Agricultural Science, refType=null, unstructuredReference=YANG XY, HOU L, ZHOU DG. Research progress of kanamycin[J]. Anhui Agricultural Science, 2016, 44(31): 150-152, 168., articleTitle=Research progress of kanamycin, refAbstract=null), Reference(id=1183428258788946626, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2015, volume=35, issue=10, pageStart=1708, pageEnd=1712, url=null, language=null, rfNumber=[12], rfOrder=15, authorNames=王忠, 王小莺, 鲍光明, journalName=中国兽医学报, refType=null, unstructuredReference=王忠, 王小莺, 鲍光明, 等. 加米霉素的研究进展[J]. 中国兽医学报, 2015, 35(10): 1708-1712., articleTitle=加米霉素的研究进展, refAbstract=null), Reference(id=1183428258856055491, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2015, volume=35, issue=10, pageStart=1708, pageEnd=1712, url=null, language=null, rfNumber=[12], rfOrder=16, authorNames=WANG Z, WANG XY, BAO GM, journalName=Chinese Journal of Veterinary Science, refType=null, unstructuredReference=WANG Z, WANG XY, BAO GM, et al. Research progress of kanamycin[J]. Chinese Journal of Veterinary Science, 2015, 35(10): 1708-1712., articleTitle=Research progress of kanamycin, refAbstract=null), Reference(id=1183428258914775748, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2019, volume=9, issue=null, pageStart=92, pageEnd=93, url=null, language=null, rfNumber=[13], rfOrder=17, authorNames=李小娜, 梁小菊, 张莹雪, journalName=吉林畜牧兽医, refType=null, unstructuredReference=李小娜, 梁小菊, 张莹雪, 等. 动物专用抗生素-加米霉素的研究进展[J]. 吉林畜牧兽医, 2019, 9: 92-93., articleTitle=动物专用抗生素-加米霉素的研究进展, refAbstract=null), Reference(id=1183428258994467525, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2019, volume=9, issue=null, pageStart=92, pageEnd=93, url=null, language=null, rfNumber=[13], rfOrder=18, authorNames=LI XN, LIANG XJ, ZHANG YX, journalName=Jilin Animal Husbandry and Veterinary, refType=null, unstructuredReference=LI XN, LIANG XJ, ZHANG YX, et al. Research progress on animal specific antibiotic-kanamycin[J]. Jilin Animal Husbandry and Veterinary, 2019, 9: 92-93., articleTitle=Research progress on animal specific antibiotic-kanamycin, refAbstract=null), Reference(id=1183428259095130822, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=25, issue=13, pageStart=82, pageEnd=86, url=null, language=null, rfNumber=[14], rfOrder=19, authorNames=烟利亚, journalName=广州化工, refType=null, unstructuredReference=烟利亚. 液相色谱串联质谱法测定猪肉和牛肉中双氯酚酸、氟尼辛、加米霉素的残留量[J]. 广州化工, 2024, 25(13): 82-86., articleTitle=液相色谱串联质谱法测定猪肉和牛肉中双氯酚酸、氟尼辛、加米霉素的残留量, refAbstract=null), Reference(id=1183428259166433991, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=25, issue=13, pageStart=82, pageEnd=86, url=null, language=null, rfNumber=[14], rfOrder=20, authorNames=YAN LY, journalName=Guangzhou Chemical Industry, refType=null, unstructuredReference=YAN LY. Determination of residual levels of diclofenac, flunixin, and kanamycin in pork and beef by liquid chromatography tandem mass spectrometry[J]. Guangzhou Chemical Industry, 2024, 25(13): 82-86., articleTitle=Determination of residual levels of diclofenac, flunixin, and kanamycin in pork and beef by liquid chromatography tandem mass spectrometry, refAbstract=null), Reference(id=1183428259229348552, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2018, volume=54, issue=9, pageStart=99, pageEnd=103, url=null, language=null, rfNumber=[15], rfOrder=21, authorNames=王艳艳, 王红霄, 邓菲, journalName=中国兽医杂志, refType=null, unstructuredReference=王艳艳, 王红霄, 邓菲. 牛可食性组织中加米霉素残留量的液相色谱-串联质谱检测方法的研究[J]. 中国兽医杂志, 2018, 54(9): 99-103., articleTitle=牛可食性组织中加米霉素残留量的液相色谱-串联质谱检测方法的研究, refAbstract=null), Reference(id=1183428259304846025, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2018, volume=54, issue=9, pageStart=99, pageEnd=103, url=null, language=null, rfNumber=[15], rfOrder=22, authorNames=WANG YY, WANG HX, DENG F, journalName=Chinese Journal of Veterinary Medicine, refType=null, unstructuredReference=WANG YY, WANG HX, DENG F. Study on the detection method of residual streptomycin in edible tissues of cattle by liquid chromatography tandem mass spectrometry[J]. Chinese Journal of Veterinary Medicine, 2018, 54(9): 99-103., articleTitle=Study on the detection method of residual streptomycin in edible tissues of cattle by liquid chromatography tandem mass spectrometry, refAbstract=null), Reference(id=1183428259388732106, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2022, volume=58, issue=4, pageStart=59, pageEnd=64, url=null, language=null, rfNumber=[16], rfOrder=23, authorNames=李伟岭, 范小平, 杨芳, journalName=中国兽医杂志, refType=null, unstructuredReference=李伟岭, 范小平, 杨芳, 等. 高效液相色谱-串联质谱法检测猪可食性组织中加米霉素残留[J]. 中国兽医杂志, 2022, 58(4): 59-64., articleTitle=高效液相色谱-串联质谱法检测猪可食性组织中加米霉素残留, refAbstract=null), Reference(id=1183428259447452363, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2022, volume=58, issue=4, pageStart=59, pageEnd=64, url=null, language=null, rfNumber=[16], rfOrder=24, authorNames=LI WL, FAN XP, YANG F, journalName=Chinese Journal of Veterinary Medicine, refType=null, unstructuredReference=LI WL, FAN XP, YANG F, et al. High performance liquid chromatography tandem mass spectrometry for detecting residues of streptomycin in edible pig tissues[J]. Chinese Journal of Veterinary Medicine, 2022, 58(4): 59-64., articleTitle=High performance liquid chromatography tandem mass spectrometry for detecting residues of streptomycin in edible pig tissues, refAbstract=null), Reference(id=1183428259543921356, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2023, volume=44, issue=9, pageStart=247, pageEnd=252, url=null, language=null, rfNumber=[17], rfOrder=25, authorNames=陈心怡, 李丽苏, 刘佳娜, journalName=食品工业, refType=null, unstructuredReference=陈心怡, 李丽苏, 刘佳娜. 等. 同位素内标-液相色谱-串联质谱测定牛奶中加米霉素[J]. 食品工业, 2023, 44(9): 247-252., articleTitle=同位素内标-液相色谱-串联质谱测定牛奶中加米霉素, refAbstract=null), Reference(id=1183428259602641613, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2023, volume=44, issue=9, pageStart=247, pageEnd=252, url=null, language=null, rfNumber=[17], rfOrder=26, authorNames=CHEN XY, LI LS, LIU JN, journalName=Food Industry, refType=null, unstructuredReference=CHEN XY, LI LS, LIU JN, et al. Isotope internal standard liquid chromatography tandem mass spectrometry determination of streptomycin in milk[J]. Food Industry, 2023, 44(9): 247-252., articleTitle=Isotope internal standard liquid chromatography tandem mass spectrometry determination of streptomycin in milk, refAbstract=null), Reference(id=1183428259715887822, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=1, pageEnd=9, url=http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html, language=null, rfNumber=[18], rfOrder=27, authorNames=李丽苏, 岳振峰, 赵凤娟, journalName=分析试验室, refType=null, unstructuredReference=李丽苏, 岳振峰, 赵凤娟, 等. EMR-Lipid通过式固相萃取结合同位素稀释-高效液相色谱-串联质谱法测定牛奶中磺胺溴二甲嘧啶和磺胺乙氧嗪残留量[J/OL]. 分析试验室, 1-9. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html, articleTitle=EMR-Lipid通过式固相萃取结合同位素稀释-高效液相色谱-串联质谱法测定牛奶中磺胺溴二甲嘧啶和磺胺乙氧嗪残留量, refAbstract=null), Reference(id=1183428259803968207, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=1, pageEnd=9, url=http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html, language=null, rfNumber=[18], rfOrder=28, authorNames=LI LS, YUE ZF, ZHAO FJ, journalName=Chinese Journal of Analysis Laboratory, refType=null, unstructuredReference=LI LS, YUE ZF, ZHAO FJ, et al. Determination of sulfabromodimethazine and sulfaethoxypyridazine residues in milk by EMR-lipid solid phase extraction combined with isotopic dilution-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analysis Laboratory, 1-9. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html, articleTitle=Determination of sulfabromodimethazine and sulfaethoxypyridazine residues in milk by EMR-lipid solid phase extraction combined with isotopic dilution-high performance liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1183428259866882768, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=26, issue=4, pageStart=316, pageEnd=322, url=null, language=null, rfNumber=[19], rfOrder=29, authorNames=胡珀, 卜媛媛, 金鹏, journalName=食品与药品, refType=null, unstructuredReference=胡珀, 卜媛媛, 金鹏, 等. QuEChERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定蜂房及其制剂中10种真菌毒素[J]. 食品与药品, 2024, 26(4): 316-322., articleTitle=QuEChERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定蜂房及其制剂中10种真菌毒素, refAbstract=null), Reference(id=1183428259975934673, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=26, issue=4, pageStart=316, pageEnd=322, url=null, language=null, rfNumber=[19], rfOrder=30, authorNames=HU B, BU YY, JIN P, journalName=Food and Drug, refType=null, unstructuredReference=HU B, BU YY, JIN P, et al. Simultaneous determination of ten mycotoxins in vespae nidus and its preparations by QuEChERS EMR-Lipid combined with isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry[J]. Food and Drug, 2024, 26(4): 316-322., articleTitle=Simultaneous determination of ten mycotoxins in vespae nidus and its preparations by QuEChERS EMR-Lipid combined with isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1183428260047237842, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=15, issue=11, pageStart=220, pageEnd=228, url=null, language=null, rfNumber=[20], rfOrder=31, authorNames=申磊, 柳溪, 羊银, journalName=食品安全质量检测学报, refType=null, unstructuredReference=申磊, 柳溪, 羊银, 等. Captiva EMR-Lipid技术结合液相色谱-串联质谱法测定畜禽肉及内脏中4种抗生素残留[J]. 食品安全质量检测学报, 2024, 15(11): 220-228., articleTitle=Captiva EMR-Lipid技术结合液相色谱-串联质谱法测定畜禽肉及内脏中4种抗生素残留, refAbstract=null), Reference(id=1183428260139512531, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=15, issue=11, pageStart=220, pageEnd=228, url=null, language=null, rfNumber=[20], rfOrder=32, authorNames=SHEN L, LIU X, YANG Y, journalName=Journal of Food Safety & Quality, refType=null, unstructuredReference=SHEN L, LIU X, YANG Y, et al. Determination of 4 kinds of antibiotics residues in meat and viscera of livestock and poultry by Captiva EMR-Lipid technology combined with liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2024, 15(11): 220-228., articleTitle=Determination of 4 kinds of antibiotics residues in meat and viscera of livestock and poultry by Captiva EMR-Lipid technology combined with liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1183428260215010004, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=11, pageStart=1032, pageEnd=1041, url=null, language=null, rfNumber=[21], rfOrder=33, authorNames=邱巧丽, 潘胜东, 王立, journalName=色谱, refType=null, unstructuredReference=邱巧丽, 潘胜东, 王立, 等. 基于EMR-Lipid分散固相萃取-超高效液相色谱-串联质谱法同时测定牛肉中17种全氟烷基化合物[J]. 色谱, 2024, 42(11): 1032-1041., articleTitle=基于EMR-Lipid分散固相萃取-超高效液相色谱-串联质谱法同时测定牛肉中17种全氟烷基化合物, refAbstract=null), Reference(id=1183428260294701781, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=42, issue=11, pageStart=1032, pageEnd=1041, url=null, language=null, rfNumber=[21], rfOrder=34, authorNames=QIU QL, PAN SD, WANG L, journalName=Chinese Journal of Chromatography, refType=null, unstructuredReference=QIU QL, PAN SD, WANG L, et al. Simultaneous determination of 17 perfluoroalkyl substances in beef by EMR-Lipid dispersive solid-phase extraction and ultra performance liquid chromatography tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2024, 42(11): 1032-1041., articleTitle=Simultaneous determination of 17 perfluoroalkyl substances in beef by EMR-Lipid dispersive solid-phase extraction and ultra performance liquid chromatography tandem mass spectrometry, refAbstract=null), Reference(id=1183428260386976470, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=40, issue=3, pageStart=324, pageEnd=336, url=null, language=null, rfNumber=[22], rfOrder=35, authorNames=温馨, 谭淑铧, 林庆昶, journalName=分析科学学报, refType=null, unstructuredReference=温馨, 谭淑铧, 林庆昶, 等. QuEChERS dSPE EMR-Lipid-GC-MS/MS测定动物源性食品中205种农药及13种代谢物残留量[J]. 分析科学学报, 2024, 40(3): 324-336., articleTitle=QuEChERS dSPE EMR-Lipid-GC-MS/MS测定动物源性食品中205种农药及13种代谢物残留量, refAbstract=null), Reference(id=1183428260483445463, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=40, issue=3, pageStart=324, pageEnd=336, url=null, language=null, rfNumber=[22], rfOrder=36, authorNames=WEN X, TAN SH, LIN QX, journalName=Journal of Analtical Science, refType=null, unstructuredReference=WEN X, TAN SH, LIN QX, et al. Determination of 205 pesticidesand 13 metabolites residuesin animal derived foods by QuEChERS dSPE EMR-Lipid-GC-MS-MS[J]. Journal of Analtical Science, 2024, 40(3): 324-336., articleTitle=Determination of 205 pesticidesand 13 metabolites residuesin animal derived foods by QuEChERS dSPE EMR-Lipid-GC-MS-MS, refAbstract=null), Reference(id=1183428260558942936, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=45, issue=16, pageStart=268, pageEnd=283, url=null, language=null, rfNumber=[23], rfOrder=37, authorNames=余晓琴, 闵宇航, 刘斯琪, journalName=食品科学, refType=null, unstructuredReference=余晓琴, 闵宇航, 刘斯琪, 等. QuEChERS EMR-Lipid净化结合超高效液相色谱串联质谱法快速测定食品中非法添加工业染料[J]. 食品科学, 2024, 45(16): 268-283., articleTitle=QuEChERS EMR-Lipid净化结合超高效液相色谱串联质谱法快速测定食品中非法添加工业染料, refAbstract=null), Reference(id=1183428260634440409, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=45, issue=16, pageStart=268, pageEnd=283, url=null, language=null, rfNumber=[23], rfOrder=38, authorNames=YU XQ, MIN YH, LIU SQ, journalName=Food Science, refType=null, unstructuredReference=YU XQ, MIN YH, LIU SQ, et al. Rapid determination of illegal addition of industrial dyes in foods by QuEChERS using EMR-Lipid sorbent combined with ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Food Science, 2024, 45(16): 268-283., articleTitle=Rapid determination of illegal addition of industrial dyes in foods by QuEChERS using EMR-Lipid sorbent combined with ultra-high performance liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1183428260709937882, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=47, issue=7, pageStart=116, pageEnd=120, url=null, language=null, rfNumber=[24], rfOrder=39, authorNames=马宁, 李洪波, 崔海燕, journalName=饲料研究, refType=null, unstructuredReference=马宁, 李洪波, 崔海燕, 等. Captiva EMR-Lipid固相萃取/超高效液相色谱-串联质谱快速筛查饲料中7种真菌毒素[J]. 饲料研究, 2024, 47(7): 116-120., articleTitle=Captiva EMR-Lipid固相萃取/超高效液相色谱-串联质谱快速筛查饲料中7种真菌毒素, refAbstract=null), Reference(id=1183428260785435355, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=47, issue=7, pageStart=116, pageEnd=120, url=null, language=null, rfNumber=[24], rfOrder=40, authorNames=MA N, LI HB, CUI HY, journalName=Feed Research, refType=null, unstructuredReference=MA N, LI HB, CUI HY, et al. Captiva EMR-Lipid SPE/ultra performance liquid chromatography-tandem mass spectrometry rapid screening seven mycotoxins in feed[J]. Feed Research, 2024, 47(7): 116-120., articleTitle=Captiva EMR-Lipid SPE/ultra performance liquid chromatography-tandem mass spectrometry rapid screening seven mycotoxins in feed, refAbstract=null), Reference(id=1183428260865127132, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=15, issue=19, pageStart=228, pageEnd=234, url=null, language=null, rfNumber=[25], rfOrder=41, authorNames=唐玥, 李少华, 陈达炜, journalName=食品安全质量检测学报, refType=null, unstructuredReference=唐玥, 李少华, 陈达炜, 等. 糖诱导相分离/超高效液相色谱-高分辨质谱法测定牛奶中高氯酸盐含量[J]. 食品安全质量检测学报, 2024, 15(19): 228-234., articleTitle=糖诱导相分离/超高效液相色谱-高分辨质谱法测定牛奶中高氯酸盐含量, refAbstract=null), Reference(id=1183428260928041693, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=15, issue=19, pageStart=228, pageEnd=234, url=null, language=null, rfNumber=[25], rfOrder=42, authorNames=TANG Y, LI SH, CHEN DW, journalName=Journal of Food Safety & Quality, refType=null, unstructuredReference=TANG Y, LI SH, CHEN DW, et al. Determination of perchlorate content in milk by sugar-induced phase separation and ultra performance liquid chromatography-high resolution mass spectrometry[J]. Journal of Food Safety & Quality, 2024, 15(19): 228-234., articleTitle=Determination of perchlorate content in milk by sugar-induced phase separation and ultra performance liquid chromatography-high resolution mass spectrometry, refAbstract=null), Reference(id=1183428260986761950, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=15, issue=20, pageStart=279, pageEnd=287, url=null, language=null, rfNumber=[26], rfOrder=43, authorNames=梁艳婷, 杨奉筠, 贾艳丰, journalName=食品安全质量检测学报, refType=null, unstructuredReference=梁艳婷, 杨奉筠, 贾艳丰, 等. 基于自建数据库的超高效液相色谱-四极杆-飞行时间质谱法定量测定玉米中5种真菌毒素[J]. 食品安全质量检测学报, 2024, 15(20): 279-287., articleTitle=基于自建数据库的超高效液相色谱-四极杆-飞行时间质谱法定量测定玉米中5种真菌毒素, refAbstract=null), Reference(id=1183428261041287903, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=15, issue=20, pageStart=279, pageEnd=287, url=null, language=null, rfNumber=[26], rfOrder=44, authorNames=LIANG YT, YANG FJ, JIA YF, journalName=Journal of Food Safety & Quality, refType=null, unstructuredReference=LIANG YT, YANG FJ, JIA YF, et al. Determination of 5 kinds of mycotoxins in Zea mays by ultra performance liquid chromatography- quadrupole-time-of-flight mass spectrometry based on self-established database[J]. Journal of Food Safety & Quality, 2024, 15(20): 279-287., articleTitle=Determination of 5 kinds of mycotoxins in Zea mays by ultra performance liquid chromatography- quadrupole-time-of-flight mass spectrometry based on self-established database, refAbstract=null), Reference(id=1183428261108396768, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=1, pageEnd=11, url=http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html, language=null, rfNumber=[27], rfOrder=45, authorNames=邱月, 陆嘉莉, 李根容, journalName=分析试验室, refType=null, unstructuredReference=邱月, 陆嘉莉, 李根容, 等. QuEChERS增强型去脂质技术结合超高效液相色谱串联质谱法测定食用植物油中27种光稳定剂[J/OL]. 分析试验室, 1-11. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html, articleTitle=QuEChERS增强型去脂质技术结合超高效液相色谱串联质谱法测定食用植物油中27种光稳定剂, refAbstract=null), Reference(id=1183428261171311329, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=null, volume=null, issue=null, pageStart=1, pageEnd=11, url=http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html, language=null, rfNumber=[27], rfOrder=46, authorNames=QIU Y, LU JL, LI GR, journalName=Chinese Journal of Analysis Laboratory, refType=null, unstructuredReference=QIU Y, LU JL, LI GR, et al. Determination of 27 kinds of light stabilizer in edible plant oil by QuEChERS enhanced matrix removal-lipid technique combined with ultra high-performance liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Analysis Laboratory, 1-11. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html, articleTitle=Determination of 27 kinds of light stabilizer in edible plant oil by QuEChERS enhanced matrix removal-lipid technique combined with ultra high-performance liquid chromatography- tandem mass spectrometry, refAbstract=null), Reference(id=1183428261246808802, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=45, issue=21, pageStart=172, pageEnd=179, url=null, language=null, rfNumber=[28], rfOrder=47, authorNames=李名路, 辛丽娜, 梁飞燕, journalName=食品研究与开发, refType=null, unstructuredReference=李名路, 辛丽娜, 梁飞燕, 等. 固相萃取-超高效液相色谱-串联质谱法测定虾肉中40种精神类药物残留及基质效应[J]. 食品研究与开发, 2024, 45(21): 172-179., articleTitle=固相萃取-超高效液相色谱-串联质谱法测定虾肉中40种精神类药物残留及基质效应, refAbstract=null), Reference(id=1183428261301334755, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2024, volume=45, issue=21, pageStart=172, pageEnd=179, url=null, language=null, rfNumber=[28], rfOrder=48, authorNames=LI ML, XIN LN, LIANG FY, journalName=Food Research and Development, refType=null, unstructuredReference=LI ML, XIN LN, LIANG FY, et al. Determination of 40 Psychotropic drug residues and matrix effects in shrimp meat by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J]. Food Research and Development, 2024, 45(21): 172-179., articleTitle=Determination of 40 Psychotropic drug residues and matrix effects in shrimp meat by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1183428261448135396, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2006, volume=830, issue=2, pageStart=293, pageEnd=300, url=null, language=null, rfNumber=[29], rfOrder=49, authorNames=MATUSZEWSKI BK, journalName=Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences, refType=null, unstructuredReference=MATUSZEWSKI BK. Standard line slopes as a measure of a relative matrix effect in quantitative HPLC-MS bioanalysis[J]. Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences, 2006, 830(2): 293-300., articleTitle=Standard line slopes as a measure of a relative matrix effect in quantitative HPLC-MS bioanalysis, refAbstract=null), Reference(id=1183428261511049957, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2023, volume=41, issue=11, pageStart=986, pageEnd=994, url=null, language=null, rfNumber=[30], rfOrder=50, authorNames=童兰艳, 许博舟, 聂雪梅, journalName=色谱, refType=null, unstructuredReference=童兰艳, 许博舟, 聂雪梅, 等. 液相色谱-四极杆/静电场轨道阱质谱法测定牛奶中22种真菌毒素[J]. 色谱, 2023, 41(11): 986-994., articleTitle=液相色谱-四极杆/静电场轨道阱质谱法测定牛奶中22种真菌毒素, refAbstract=null), Reference(id=1183428261578158822, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2023, volume=41, issue=11, pageStart=986, pageEnd=994, url=null, language=null, rfNumber=[30], rfOrder=51, authorNames=TONG LY, XU BZ, NIE XM, journalName=Chinese Journal of Chromatography, refType=null, unstructuredReference=TONG LY, XU BZ, NIE XM, et al. Determination of 22 mycotoxins in milk by liquid chromatography-quadrupole/ orbitrap mass spectrometry[J]. Chinese Journal of Chromatography, 2023, 41(11): 986-994., articleTitle=Determination of 22 mycotoxins in milk by liquid chromatography-quadrupole/ orbitrap mass spectrometry, refAbstract=null), Reference(id=1183428261670433511, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2017, volume=49, issue=6, pageStart=54, pageEnd=59, url=null, language=null, rfNumber=[31], rfOrder=52, authorNames=郭洋洋, 罗小清, 彭麟, journalName=畜牧与兽医, refType=null, unstructuredReference=郭洋洋, 罗小清, 彭麟, 等. 猪可食性组织中加米霉素残留量的UPLC-MS/MS检测方法研究[J]. 畜牧与兽医, 2017, 49(6): 54-59., articleTitle=猪可食性组织中加米霉素残留量的UPLC-MS/MS检测方法研究, refAbstract=null), Reference(id=1183428261724959464, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, doi=null, pmid=null, pmcid=null, year=2017, volume=49, issue=6, pageStart=54, pageEnd=59, url=null, language=null, rfNumber=[31], rfOrder=53, authorNames=GUO YY, LUO XQ, PENG L, journalName=Animal Husbandry & Veterinary Medicine, refType=null, unstructuredReference=GUO YY, LUO XQ, PENG L, et al. Development of an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of gamithromycin in edible swine tissues[J]. Animal Husbandry & Veterinary Medicine, 2017, 49(6): 54-59., articleTitle=Development of an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of gamithromycin in edible swine tissues, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1183428253957108337, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, xref=null, ext=[AuthorCompanyExt(id=1183428253961302642, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China), AuthorCompanyExt(id=1183428253969691251, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, companyId=1183428253957108337, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=中检科(北京)测试技术有限公司, 北京 100176 )])], figs=[ArticleFig(id=1183428256213643935, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Fig.1, caption=Molecular structural formula of gamithromycin, figureFileSmall=2noeNUzOk65lBgjjL8XXvQ==, figureFileBig=LivvcGURzh0YF0MK4mIwfg==, tableContent=null), ArticleFig(id=1183428256276558496, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=图1, caption=加米霉素的分子结构式, figureFileSmall=2noeNUzOk65lBgjjL8XXvQ==, figureFileBig=LivvcGURzh0YF0MK4mIwfg==, tableContent=null), ArticleFig(id=1183428256343667361, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Fig.2, caption=Effects of different extraction solvents on the recovery rate of gamithromycin, figureFileSmall=/q1VEQawlFO8oAsOrqTbxg==, figureFileBig=Tdi/GApYM0WGIuMd28/xEQ==, tableContent=null), ArticleFig(id=1183428256402387618, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=图2, caption=不同提取溶剂对加米霉素回收率的影响, figureFileSmall=/q1VEQawlFO8oAsOrqTbxg==, figureFileBig=Tdi/GApYM0WGIuMd28/xEQ==, tableContent=null), ArticleFig(id=1183428256461107875, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Fig.3, caption=MRM mode ion scanning spectrum of the standard sample of gamithromycin (5.0 ng/mL), figureFileSmall=yMaSPG2kQHWVxZDHTUjHDA==, figureFileBig=cCtmkBSrKOhQqUnoFoz4oQ==, tableContent=null), ArticleFig(id=1183428256515633828, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=图3, caption=加米霉素(5.0 ng/mL)标准品MRM模式离子扫描图谱, figureFileSmall=yMaSPG2kQHWVxZDHTUjHDA==, figureFileBig=cCtmkBSrKOhQqUnoFoz4oQ==, tableContent=null), ArticleFig(id=1183428256586936997, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Fig.4, caption=LOD with MRM mode example scan map, figureFileSmall=tk8gq1ThklAP1K4iPd72kQ==, figureFileBig=uPK19JiueKWJpqydljV5HQ==, tableContent=null), ArticleFig(id=1183428256662434470, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=图4, caption=LOD添加MRM模式离子扫描图谱, figureFileSmall=tk8gq1ThklAP1K4iPd72kQ==, figureFileBig=uPK19JiueKWJpqydljV5HQ==, tableContent=null), ArticleFig(id=1183428256716960423, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Fig.5, caption=LOQ with MRM mode example scan map, figureFileSmall=4prM+p9ZrvhaIZI6Hf6Lkw==, figureFileBig=zdevHgNfbmAfU6W1ZTz2eA==, tableContent=null), ArticleFig(id=1183428256763097768, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=图5, caption=LOQ添加MRM模式离子扫描图谱, figureFileSmall=4prM+p9ZrvhaIZI6Hf6Lkw==, figureFileBig=zdevHgNfbmAfU6W1ZTz2eA==, tableContent=null), ArticleFig(id=1183428256821818025, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Fig.6, caption=MRM chromatogram of blank sample of raw milk, figureFileSmall=F6V90LHN3UzShYAUn0JLKg==, figureFileBig=3clFcySAOjYixOpT1RyYCQ==, tableContent=null), ArticleFig(id=1183428256876343978, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=图6, caption=生乳空白样品MRM色谱图, figureFileSmall=F6V90LHN3UzShYAUn0JLKg==, figureFileBig=3clFcySAOjYixOpT1RyYCQ==, tableContent=null), ArticleFig(id=1183428256943452843, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Fig.7, caption=MRM chromatogram of raw milk added sample, figureFileSmall=JvbJSS5MqkluK6aEceFiaA==, figureFileBig=P5nUU9cz7JRinUh7Ba9P4A==, tableContent=null), ArticleFig(id=1183428257010561708, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=图7, caption=生乳添加样品MRM色谱图, figureFileSmall=JvbJSS5MqkluK6aEceFiaA==, figureFileBig=P5nUU9cz7JRinUh7Ba9P4A==, tableContent=null), ArticleFig(id=1183428257073476269, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Table 1, caption=

Mobile phase conditions for gradient elution

, figureFileSmall=null, figureFileBig=null, tableContent=
时间
/min		 流速
/(mL/min)		 流动相A
/%		 流动相B
/%
0.00 0.400 85.0 15.0
0.50 0.400 85.0 15.0
2.80 0.400 5.0 95.0
3.50 0.400 5.0 95.0
3.60 0.400 85.0 15.0
5.00 0.400 85.0 15.0
), ArticleFig(id=1183428257132196526, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=表1, caption=

梯度洗脱的流动相条件

, figureFileSmall=null, figureFileBig=null, tableContent=
时间
/min		 流速
/(mL/min)		 流动相A
/%		 流动相B
/%
0.00 0.400 85.0 15.0
0.50 0.400 85.0 15.0
2.80 0.400 5.0 95.0
3.50 0.400 5.0 95.0
3.60 0.400 85.0 15.0
5.00 0.400 85.0 15.0
), ArticleFig(id=1183428257203499695, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Table 2, caption=

Mass spectrometry parameters of gamithromycin

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物 母离子
(m/z)		 子离子
(m/z)		 保留时间
/min		 去簇电压
/V		 碰撞能量
/V
加米霉素 777.6 619.6* 2.35 90 42
157.9 2.35 90 48
), ArticleFig(id=1183428257270608560, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=表2, caption=

加米霉素质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物 母离子
(m/z)		 子离子
(m/z)		 保留时间
/min		 去簇电压
/V		 碰撞能量
/V
加米霉素 777.6 619.6* 2.35 90 42
157.9 2.35 90 48
), ArticleFig(id=1183428257337717425, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=EN, label=Table 3, caption=

Addition amount, recovery rate, and relative standard deviation of gamithromycin in raw milk

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物名称 添加量/(μg/kg) 平均回收率/% RSDs/%
加米霉素 1.0 77.0 4.57
2.0 74.0 3.92
10.0 74.9 4.51
), ArticleFig(id=1183428257392243378, tenantId=1146029695717560320, journalId=1149652044408987649, articleId=1153986643288642061, language=CN, label=表3, caption=

牛乳中加米霉素的添加量、平均回收率和相对标准偏差

, figureFileSmall=null, figureFileBig=null, tableContent=
化合物名称 添加量/(μg/kg) 平均回收率/% RSDs/%
加米霉素 1.0 77.0 4.57
2.0 74.0 3.92
10.0 74.9 4.51
)], attaches=null, journal=Journal(id=1146438185598431260, delFlag=0, nameCn=食品安全质量检测学报, nameEn=Journal of Food Safety & Quality, nameHistory1=null, nameHistory2=null, issn=2095-0381, eissn=null, cn=11-5956/TS, coden=null, periodic=3, language=CN, oaType=0, ccby=CC BY-NC-ND, superviseOffice=null, ownerOffice=null, pubOffice=null, editorOffice=null, officeType=null, aims=null, clcCode=null, officeProv=null, officeCity=null, officeAddr=null, officeZip=null, officeEmail=null, officePhone=null, editDirector=null, officeDirector=null, officeDirectorPhone=null, officeStaffNum=null, officeEmpNum=null, coverPicUrl=4kwA5ri4VfzavOn19fwc2g==, journalPrice=null, startedYear=null, abbrevIsoEn=J Food Saf Qual, journalRemark=null, publicationField=null, createdTime=1751261763241, updatedTime=1754445151803, createdBy=18614031015, updatedBy=13701087609, firstLetterCn=J, firstLetterEn=J, subjectCode=Engineering, subjectName=工程, subjectCodeEn=Engineering, subjectNameEn=null, picCn=4kwA5ri4VfzavOn19fwc2g==, picEn=eHhRQNEus+t1f6yOGnBJ3w==, jcr=null, cjcr=null, exts=[JournalExt(id=1159790285120618579, language=CN, name=食品安全质量检测学报, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=null, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1754445151834, updatedTime=1754445151834, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=http://chinafoodj.ijournals.cn/ch/first_menu.aspx?parent_id=20160111022419868, submissionAuthorUrl=http://chinafoodj.ijournals.cn/ch/author/login.aspx, submissionEditorUrl=http://chinafoodj.ijournals.cn/ch/login.aspx, submissionReviewUrl=http://chinafoodj.ijournals.cn/ch/auditor/login.aspx, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""}), JournalExt(id=1159790285187727444, language=EN, name=Journal of Food Safety & Quality, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=null, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1754445151850, updatedTime=1754445151850, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=http://chinafoodj.ijournals.cn/ch/first_menu.aspx?parent_id=20160111022419868, submissionAuthorUrl=http://chinafoodj.ijournals.cn/ch/author/login.aspx, submissionEditorUrl=http://chinafoodj.ijournals.cn/ch/login.aspx, submissionReviewUrl=http://chinafoodj.ijournals.cn/ch/auditor/login.aspx, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""})], databaseList=null, tenantJournalId=1149652044408987649, websiteList=[Website(id=1151872930754474249, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1149652044408987649, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/spaq/CN, language=CN, createTime=1752557507456, createBy=18614031015, updateTime=1752558523388, updateBy=18614031015, name=食品安全质量检测学报, tplId=1146099689490845704, title=食品安全质量检测学报, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1151887749801407249, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930754474249, code=articleTextType, value=kx, createTime=1752561040592, updateTime=1752561040592, creator=18614031015, updator=18614031015), WebsiteProps(id=1151887749776241422, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930754474249, code=banner, value=null, createTime=1752561040586, updateTime=1752561040586, creator=18614031015, updator=18614031015), WebsiteProps(id=1151887749767852813, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930754474249, code=logo, value=https://castjournals.cast.org.cn/joweb/kjdb/CN/file/pic?fileId=RhDdm4lBDQfNHl8cX0659g==, createTime=1752561040584, updateTime=1752561040584, creator=18614031015, updator=18614031015), WebsiteProps(id=1151887749793018640, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930754474249, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/kjdb/CN/file/pic, createTime=1752561040590, updateTime=1752561040590, creator=18614031015, updator=18614031015), WebsiteProps(id=1151887749784630031, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930754474249, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_cn_619/, createTime=1752561040588, updateTime=1752561040588, creator=18614031015, updator=18614031015)]), Website(id=1151872930855137548, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1149652044408987649, journalNameCn=null, journalNameEn=null, grayFlag=null, tenantId=1146029695717560320, platformId=null, journalGroupId=null, journalGroupNameCn=null, journalGroupNameEn=null, type=1, domain=https://castjournals.cast.org.cn/joweb/spaq/EN, language=EN, createTime=1752557507480, createBy=18614031015, updateTime=1752558528290, updateBy=18614031015, name=食品安全质量检测学报, tplId=1146101810881728533, title=食品安全质量检测学报, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1155904094024884374, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930855137548, code=articleTextType, value=kx, createTime=1753518611675, updateTime=1753518611675, creator=18614031015, updator=18614031015), WebsiteProps(id=1155904094008107155, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930855137548, code=banner, value=null, createTime=1753518611671, updateTime=1753518611671, creator=18614031015, updator=18614031015), WebsiteProps(id=1155904094003912850, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930855137548, code=logo, value=https://castjournals.cast.org.cn/joweb/kjdb/EN/file/pic?fileId=RhDdm4lBDQfNHl8cX0659g==, createTime=1753518611670, updateTime=1753518611670, creator=18614031015, updator=18614031015), WebsiteProps(id=1155904094020690069, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930855137548, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/kjdb/EN/file/pic, createTime=1753518611674, updateTime=1753518611674, creator=18614031015, updator=18614031015), WebsiteProps(id=1155904094016495764, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1151872930855137548, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_en_623/, createTime=1753518611673, updateTime=1753518611673, creator=18614031015, updator=18614031015)])], journalTitle=食品安全质量检测学报, weixinUrl=null, journalUrl=null, iacademicId=null, status=0, seqNo=null, journalTitleEn=Journal of Food Safety & Quality, journalPhotoCn=4kwA5ri4VfzavOn19fwc2g==, journalPhotoEn=eHhRQNEus+t1f6yOGnBJ3w==, journalFirstLetter=J, journalRecommend=null, journalNew=null, journalCollection=null, jcrJf=null, cjcrJf=null, jcrJfStr=null, cjcrJfStr=null, submissionFirstDecision=null, sciSubjectClassification=null, casSubjectClassification=null, citeScore=null, totalCitationFrequency=null, icpCode=null, psCode=null, advertisingLicenseCode=null, copyrightInformation=null, country=null, option=null, provinceCode=null, provinceName=null, collectFlag=false), detailUrlCn=https://castjournals.cast.org.cn/joweb/spaq/CN/10.19812/j.cnki.jfsq11-5956/ts.20241018002, detailUrlEn=https://castjournals.cast.org.cn/joweb/spaq/EN/10.19812/j.cnki.jfsq11-5956/ts.20241018002, pdfUrlCn=https://castjournals.cast.org.cn/joweb/spaq/CN/PDF/10.19812/j.cnki.jfsq11-5956/ts.20241018002, pdfUrlEn=https://castjournals.cast.org.cn/joweb/spaq/EN/PDF/10.19812/j.cnki.jfsq11-5956/ts.20241018002, aliStartDate=null, aliEndDate=null, collectionFlag=false, citedCount=null, citedUrl=null, reference=null)
收藏切换
高效液相色谱-串联质谱法测定生乳中加米霉素残留量
收藏切换
PDF下载
李默 , 赵鑫 , 张虹吉 , 周婷 , 王倩 , 赵修平 , 李克静 *
食品安全质量检测学报 | 食品分析与检测 2025,16(3): 303-308
收起
收藏切换
食品安全质量检测学报 | 食品分析与检测 2025, 16(3): 303-308
高效液相色谱-串联质谱法测定生乳中加米霉素残留量
全屏
李默 , 赵鑫, 张虹吉, 周婷, 王倩, 赵修平, 李克静*
作者信息
  • 中检科(北京)测试技术有限公司, 北京 100176

    • 李默(1991—), 女, 助理研究员, 主要研究方向为农兽药残留及真菌毒素。E-mail:

通讯作者:

* 李克静(1981—), 女, 高级工程师, 主要研究方向为食品安全检测。E-mail:
Determination of residual levels of gamithromycin in raw milk by high performance liquid chromatography-tandem mass spectrometry
Mo LI , Xin ZHAO, Hong-Ji ZHANG, Ting ZHOU, Qian WANG, Xiu-Ping ZHAO, Ke-Jing LI*
Affiliations
  • Zhongjianke (Beijing) Testing Technology Co., Ltd., Beijing 100176, China
出版时间: 2025-02-15 doi: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
文章导航
收藏切换
摘要
收起

目的 建立以基质外标法定量, 通过式净化柱(EMR-Lipid)结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)测定生乳中加米霉素残留量的分析方法。方法 样品经酸性乙腈提取后, 由EMR-Lipid通过式净化柱净化, 通过BEH C18色谱柱进行梯度洗脱, 电喷雾正离子多反应模式进行检测, 基质外标法定量。结果 加米霉素在0.5~20.0 ng/mL质量浓度范围内呈现良好线性关系, 线性相关系数大于0.99; 检出限(limit of detection, LOD)为0.5 μg/kg; 定量限(limit of quantification, LOQ)为1.0 μg/kg; 加米霉素在生乳中表现为基质增强效应, 经基质空白曲线校正后, 加米霉素在不同添加浓度平均回收率为74.0%~77.0%, 测定结果的相对标准偏差(relative standard deviation, RSD)为3.92%~4.57%。结论 该方法准确、灵敏、稳定、简单易操作, 可以用于生乳中加米霉素残留量快速测定及定量分析, 为生乳中加米霉素残留监控提供技术支持。

加米霉素  /  高效液相色谱-串联质谱法  /  EMR-Lipid通过式净化柱  /  生乳

Objective To establish an analytical method for the determination of gamithromycin residues in raw milk based on matrix external standard method combined with through type purification column (EMR-Lipid) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The samples were extracted with acid acetonitrile, purified by the EMR-Lipid through type purification column, gradient eluted through a BEH C18 chromatographic column. Detection was carried out in the electrospray positive ion multiple reaction mode, and quantification was performed using the matrix external standard method. Results Calibration curves were linear in the range of 0.5-20.0 ng/mL with correlation coefficients more than 0.99. The limit of detection (LOD) was 0.5 μg/kg, limit of quantification (LOQ) was 1.0 μg/kg. Gamithromycin showed a matrix enhancement effects in raw milk. After matrix blank curve correction, the average recoveries of gamithromycin at different spiked concentrations ranged from 74.0% to 77.0%, and the relative standard deviations (RSD) of the determination results were from 3.92% to 4.57%. Conclusion This method is accurate, sensitive, stable, simple, and easy to operate, it can be used for the rapid determination and quantitative analysis of gamithromycin residues in raw milk, providing technical support for monitoring the residual amount of gamithromycin in raw milk.

gamithromycin  /  high performance liquid chromatography-tandem mass spectrometry  /  EMR-Lipid through type purification column  /  raw milk
李默, 赵鑫, 张虹吉, 周婷, 王倩, 赵修平, 李克静. 高效液相色谱-串联质谱法测定生乳中加米霉素残留量. 食品安全质量检测学报, 2025 , 16 (3) : 303 -308 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
Mo LI, Xin ZHAO, Hong-Ji ZHANG, Ting ZHOU, Qian WANG, Xiu-Ping ZHAO, Ke-Jing LI. Determination of residual levels of gamithromycin in raw milk by high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2025 , 16 (3) : 303 -308 . DOI: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
正文
收起
0 引言
收起
加米霉素(gamithromycin)是一种新型的半合成大环内酯类兽用抗生素, 由法国梅里亚公司研发, 其结构式如图1所示。该药的杀菌作用是通过抑制敏感菌RNA依赖性蛋白合成来实现的, 常用于兽医临床因巴氏杆菌、支原体、睡眠嗜组织菌等感染所致的牛呼吸系统疾病(bovine respiratory disease, BRD)的治疗[1-3]。是我国批准的用于治疗牛、猪部分呼吸道疾病的二类新兽药[4]。
作为新一代大环类脂类抗菌药的加米霉素, 具备给药吸收快、抗菌活性强、肺部药物浓度高、毒性低以及组织残留少等优点, 拥有广阔的临床应用前景[5-6]。欧洲药品局(European Medicines Agency, EMA)先后在2007年和2016年将加米霉素批准用于靶动物牛和猪[7-9]; 2010年, 加拿大保健产品与食品管理局(Health Products and Food Administration of Canada, HPFB)批准加米霉素用于防止溶血性曼氏杆菌等引起的BRD; 2011年, 美国食品与药品管理局(US Food and Drug Administration, FDA)也批准了该药用于此用途[10-13]。依据我国相关规定, 加米霉素只在猪、牛的肌肉、肝、肾等靶组织中有相关的最大残留限量要求, 并未对生乳及牛奶中加米霉素的残留限量进行规定, 但是欧盟在EU No 470/2009中规定加米霉素在泌乳期禁用。生乳的质量安全一直是社会各界关注的重点, 建立生乳中加米霉素稳定、快速、灵敏的检测方法对保证我国奶源安全及出口乳品的质量, 了解加米霉素的污染情况具有实际意义。
目前, 加米霉素的分析方法主要是高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)[14-17]。样品基质多为猪、牛的肌肉组织。乳制品基质检测, 目前在国内偶见报道。烟利亚[14]建立了利用液相色谱-串联质谱法测定猪肉和牛肉中双氯酚酸、氟尼辛、加米霉素的残留量; 王艳艳等[15]通过液相色谱串联-质谱仪对牛可食性组织中加米霉素残留量进行测定; 虽然陈心怡等[17]建立了液相色谱-串联质谱法测定牛奶中加米霉素的分析方法, 但是该方法使用同位素内标定量, 相较而言成本较高, 不便于推广。近年来, 通过式固相萃取技术作为一种新型的前处理净化方式以成本低, 操作简单, 耗时短等优势被广泛应用于食品检测中[18-24]。本研究以基质空白曲线定量, 通过式净化柱(EMR-Lipid)结合HPLC-MS/MS建立起一种前处理方法简单、成本较低、易于推广的加米霉素的分析方法, 以满足日常生乳中加米霉素的监控需求。
1 材料与方法
收起
1.1 材料与试剂
乙腈(色谱纯, 上海安谱公司); 甲酸(优级纯, 北京百灵威科技有限公司); 乙酸铵(色谱纯, 美国Sigma公司); 加米霉素标准溶液(质量浓度100 μg/mL, 天津阿尔塔First Standard公司)。
1.2 仪器与设备
岛津LC-30A高效液相色谱仪(日本岛津公司); Triple Quad 4500三重四极杆质谱仪(美国AB公司); ACQUITY UPLC BEH C18色谱柱(100 mm×2.1 mm, 1.7 μm, 美国Waters公司); SR-2DS振荡器(日本TAITEC公司); ME203E分析天平(精度10 mg)、ME204E分析天平(精度0.1 mg)[梅特勒托利多科技(中国)有限公司]; X-15R离心机(德国Beckman公司); Milli-Q EQ7008超纯水机(美国Millipore公司); SI Vortex Genie 2漩涡混合器(美国Scientific Industries公司); Captuve EMR-Lipid净化柱(300 mg/3 mL, 美国安捷伦公司); 0.22 μm有机相滤膜(天津津腾实验设备有限公司)。
1.3 试验方法
1.3.1 标准溶液配制
准确吸取适量的加米霉素标准品, 用乙腈稀释混匀, 定容至10 mL, 得到10 μg/mL标准储备溶液, 置于-18 ℃冰箱保存。取适量该溶液, 分别配制0.20 μg/mL和0.02 μg/mL的标准工作溶液。精密吸取标准工作液适量, 用经提取净化后的空白样品溶液稀释配制成0.5~20.0 ng/mL的系列基质校准工作曲线。
1.3.2 样品前处理
称取生乳5 g(精确至0.01 g)置于50 mL离心管中, 加入0.2%甲酸-乙腈溶液定容至15 mL, 振荡20 min, 8000 r/min离心5 min, 上清液转移至另一套离心管中, 待净化。
取3 mL上清液过EMR-Lipid通过式净化柱(无需活化), 上样后立即接收。待样液全部流完之后, 再加入1 mL 0.2%甲酸-乙腈溶液淋洗小柱并合并样液, 抽干小柱。将收集的过柱液体在40 ℃下用氮气吹至近干, 加入0.5 mL 0.05%甲酸-乙酸铵溶液, 用乙腈定容至1 mL, 涡旋混合均匀, 过0.22 μm滤膜, 供HPLC-MS/MS分析。
1.3.3 液相色谱-串联质谱条件
(1)液相色谱条件
色谱柱为ACQUITY UPLC BEH C18 (100 mm×2.1 mm, 1.7 μm, 美国Waters公司); 流动相A: 水(含0.1%甲酸), 流动相B: 乙腈; 流速: 0.4 mL/min; 进样量: 6.00 µL; 柱温: 45 ℃; 洗脱的梯度条件如表1所示。
(2)质谱条件
电离源: 电喷雾正离子模式(electrospray ionization, ESI+); 监测模式: 多反应监测(multiple reaction monitoring, MRM); 气帘气: 35 psi; 雾化气: 氮气, 50 psi; 辅助加热气: 氮气, 55 psi; 碰撞气: 氮气; 离子喷雾电压: 5500 V; 辅助加热器温度: 500 ℃; 加米霉素质谱参数如表2所示。
1.4 数据处理
方法学验证参照GB 5009.295《食品安全国家标准 化学分析方法验证通则》进行分析验证。在方法学考察中, 重复性实验平行测定大于6次, 回收率测定3组7份, 线性测定5个点(不包括零点), 每个点测定3份, 实际样品平行测定3份, 数据采集和分析软件分别为Analyst 1.6版本、Analyst 1.6.3系统软件和Excel 2016, 结果以平均数表示。
2 结果与分析
收起
2.1 前处理条件优化
2.1.1 提取溶剂优化
乙腈、甲醇、甲酸乙腈以及磷酸盐缓冲溶液是常用的加米霉素提取溶剂。由于EMR-Lipid通过式净化柱是利用极性、非极性及离子交换等基团组成的填充剂进行选择性的吸附而达到去除样品干扰物的目的, 若选择磷酸盐缓冲液则会明显干扰净化效果, 故不将其作为本研究的提取溶液。用甲醇进行提取时, 由于乳化现象较严重, 因此也不作为最佳的提取溶剂; 本研究对乙腈、2.0%甲酸-乙腈、1.0%甲酸-乙腈、0.5%甲酸-乙腈、0.2%甲酸-乙腈和0.1%甲酸-乙腈6种提取溶剂的提取效率进行了对比。具体回收率的结果比较见图2。结果表明: 6种提取溶剂中, 乙腈的回收率在5.0%左右, 0.1%甲酸-乙腈的回收率在65%左右, 0.2%、0.5%、1.0%、2.0%甲酸-乙腈的回收率分别为: 82.0%、79.4%、81.6%、79.8%。综合考虑测试成本因素, 最终选用0.2%甲酸-乙腈作为本研究的提取溶剂。
2.1.2 净化方式优化
本研究采用EMR-Lipid通过式净化柱净化, 无需活化, 且上样后直接接收, 净化液直接进行氮吹浓缩、过膜后供仪器分析测试。结果表明: (1)在相应的保留时间处, 空白基质样品对被测物无显著干扰; (2)所得到的加米霉素回收率处于60%~120%的范围之内, 满足GB 5009.295《食品安全国家标准 化学分析方法验证通则》的要求, 同时还能够极大地提高测试效率。故本研究采用EMR-Lipid通过式净化柱进行净化。
2.1.3 基质效应的评估
采用液相色谱-串联质谱法测定时, 基质效应会对分析结果产生影响[25-28]。根据MATUSZEWSKI等[29]的方法, 基质效应=(基质匹配标准曲线斜率-溶剂标准曲线斜率)/溶剂标准曲线斜率×100%。若结果为负数则表示基质抑制效应, 结果为正数表示基质增强效应。当-20%<基质效应<20%之间时为弱基质效应; 如果在-50%<基质效应<20%或20%<基质效应<50%之间, 则为中等基质效应; 基质效应≥50%或基质效应≤50%时为强基质效应[30]。
按1.3的试验方法配制基质匹配标准曲线和溶剂标准曲线。溶剂标准曲线线线性方程: Y=20793.90478X- 1506.77265 (r2=0.99953), 基质匹配曲线线性方程为: Y=29847.58152X-1943.54824 (r2=0.99819)。结果表明加米霉素在生乳基质中的基质效应为43.5%, 表明存在中等基质增强效应。所以, 为抵消基质效应的影响, 选择基质匹配标准曲线来进行定量。
2.2 质谱条件优化
加米霉素含有羧基, 易结合氢离子[31], 本研究通过流动注射进样方式选择并优化MRM参数, 在正离子模式下选择[M+H]+为母离子, 优化碰撞能量以获得响应较高的子离子。把丰度最强的离子对作为定量离子对, 接着对毛细管电压、雾化气流速、锥孔气流速、雾化气温度、源温度、锥孔电压、碰撞能量等质谱条件予以优化, 最终确定的质谱条件如表2所示。按照上述色谱和质谱条件获得的标准溶液图谱详见图3。
2.3 方法学验证
2.3.1 线性范围
按照1.3.1所述采用空白生乳基质标准工作液, 配制成加米霉素质量浓度为0、0.5、1.0、2.0、5.0、10.0、20.0 ng/mL的系列基质匹配标准工作液, 供HPLC-MS/MS检测。采用MRM离子扫描方式, 将定量离子对峰面积作为纵坐标, 把基质标准溶液浓度当作横坐标, 拟合出基质校准标准曲线。考察加米霉素在0.5~20.0 ng/mL的质量浓度范围内线性方程及其相关系数。结果表明, 在0.5~20.0 ng/mL质量浓度范围内呈现良好的线性关系, 线性方程为Y=29847.58152X-1943.54824(相关系数r=0.999)。
2.3.2 检测方法灵敏度
在生乳空白基质样品中添加一定浓度的加米霉素平行测定10次, 当检出率大于50%, 且有检出的信噪比(S/N)均大于等于3时, 将其确定为检出限(limit of detection, LOD), 相关图谱见图4。结果表明10次测定的检出率为100%, 并且有检出的信噪比(S/N)均大于等于3, 该方法下加米霉素的检出限为0.5 μg/kg, 满足GB 5009.295的要求。
在生乳空白基质样品中添加一定浓度的加米霉素平行测定7次, 且信噪比(S/N)均大于等于10为定量限(limit of quantification, LOQ), 图谱见图5。结果表明7次测定的信噪比(S/N)均大于等于10, 该方法下加米霉素的LOQ为1.0 μg/kg, 满足GB 5009.295的要求。
2.3.3 检测方法的精密度和准确度
选取牛乳空白基质样品, 开展添加回收和精密度试验。进行3水平添加试验时, 选取方法LOQ、2倍方法LOQ和10倍方法LOQ, 每个水平平行测定7次, 并且进行重复性验证, 结果详见表3, 添加样品图谱见图6、图7。结果表明加米霉素在不同添加浓度的平均回收率为74.0%~77.0%之间, 测定结果的RSDs为3.92%~4.57%之间。该加标水平下, 精密度良好, 回收率满足GB 5009.295的要求。
2.4 实际样品检测
对200个生乳样品进行加米霉素测定, 检测方法按照本研究所述开展, 均未检测出加米霉素。
3 结论
收起
本研究建立了一种采用HPLC-MS/MS检测生乳中加米霉素的测定方法。该方法以酸性乙腈作为提取溶剂, 经EMR-Lipid通过式净化柱净化后, 进行氮吹浓缩复溶以供HPLC-MS/MS测定。其具有干扰小、提取效率高、分析时间快等优点。通过添加空白样品的回收实验测定, 证实此方法灵敏度好、准确度高、稳定性好且简单易操作, 适用于生乳中加米霉素的定性定量分析。
文献
收起
参考文献 引证文献
排序方式：
[1]
XIAO TS, YANG YQ, ZHANG YX, et al. Efficacy of gamithromycin injection administered intramuscularly against bacterial stwine respiratory disase[J]. Research in Veterinary Science, 2020, 128: 118123.
[2]
European Medicines Agency Veterinary Medicines and Inspections. V-129-en6[EB/OL]. (2016-07-25) [2024-10-18]. https://www.emea.Europa.eu/vetdocs/PDFs/EPAR/V-129-en6.pdf https://www.emea.Europa.eu/vetdocs/PDFs/EPAR/V-129-en6.pdf
[3]
EMA. Committee for medicine products for veterinary use[DB/OL]. [2024-10-18]. http://www.ema.europa.eu/docs/enGB/documentlibrary/MaximumResidueLimits-Summaryofopinion/2014/07/WC500169766.pdf http://www.ema.europa.eu/docs/enGB/documentlibrary/MaximumResidueLimits-Summaryofopinion/2014/07/WC500169766.pdf
[4]
中华人民共和国农业农村部. 中华人民共和国农业农村部公告第15号[Z]. 2018.
Ministry of Agriculture of the PRC. Announcement No. 15 of the Ministry of Agriculture and Rural Affairs of the People's Republic of China[Z]. 2018.
[5]
PAPATSIROS V, TZIKA E, ATHANASIOU L, et al. In vivo effectiveness of injectable antibiotics on the recovery of acute Actinobacillus pleuropneumoniae-infected pigs[J]. Microbial Drug Rssisitance, 2019, 25(4): 603-610.
[6]
BERLIN S, RANDOW T, SCHEUCH E, et al. Pharmacokinetics and pulmonary distribution of gamithromycin after intravenous administration in foals[J]. Journal of Veterinary Pharmacology and Therapeutics, 2017, 40(4): 406-410.
[7]
The European Medicines Agency. Zactran EPAR scientific discussion[EB/OL]. (2018-07-30) [2024-12-15]. http://www.ema.europa.eu/docs/enGB/documentlibrary/EPAR-ScientificDiscussion/veterinary/000129/WC500068716 http://www.ema.europa.eu/docs/enGB/documentlibrary/EPAR-ScientificDiscussion/veterinary/000129/WC500068716
[8]
孙晨明, 高嫣珺, 徐亚亚, 等. UPLC-MS/MS测定牛血浆中加米霉素方法的建立[J]. 中国兽药杂志, 2023, 8(57): 19-24.
SUN CM, GAO YJ, XU YY, et al. Establishment of UPLC-MS/MS method for determination of streptomycin in bovine plasma[J]. Chinese Journal of Veterinary Drug, 2023, 57(8): 19-25.
[9]
FDA. Freedom of information summary original new animal drug application[EB/OL]. (2013-10-24) [2025-1-19]. http://www.fda.gov/downloads/animalveterinary/products/approvedanimaldrugproducts/foiadrugsummaries/ucm277806 http://www.fda.gov/downloads/animalveterinary/products/approvedanimaldrugproducts/foiadrugsummaries/ucm277806
[10]
李先强. 兽用加米霉素研究与应用现状[J]. 动物医学进展, 2018, 39(12): 180-184.
LI XQ. The research and application status of animal grade streptomycin[J]. Advances in Veterinary Medicine, 2018, 39(12): 180-184.
[11]
杨新艳, 侯林, 周德刚. 加米霉素的研究进展[J]. 安徽农业科学, 2016, 44(31): 150-152, 168.
YANG XY, HOU L, ZHOU DG. Research progress of kanamycin[J]. Anhui Agricultural Science, 2016, 44(31): 150-152, 168.
[12]
王忠, 王小莺, 鲍光明, 等. 加米霉素的研究进展[J]. 中国兽医学报, 2015, 35(10): 1708-1712.
WANG Z, WANG XY, BAO GM, et al. Research progress of kanamycin[J]. Chinese Journal of Veterinary Science, 2015, 35(10): 1708-1712.
[13]
李小娜, 梁小菊, 张莹雪, 等. 动物专用抗生素-加米霉素的研究进展[J]. 吉林畜牧兽医, 2019, 9: 92-93.
LI XN, LIANG XJ, ZHANG YX, et al. Research progress on animal specific antibiotic-kanamycin[J]. Jilin Animal Husbandry and Veterinary, 2019, 9: 92-93.
[14]
烟利亚. 液相色谱串联质谱法测定猪肉和牛肉中双氯酚酸、氟尼辛、加米霉素的残留量[J]. 广州化工, 2024, 25(13): 82-86.
YAN LY. Determination of residual levels of diclofenac, flunixin, and kanamycin in pork and beef by liquid chromatography tandem mass spectrometry[J]. Guangzhou Chemical Industry, 2024, 25(13): 82-86.
[15]
王艳艳, 王红霄, 邓菲. 牛可食性组织中加米霉素残留量的液相色谱-串联质谱检测方法的研究[J]. 中国兽医杂志, 2018, 54(9): 99-103.
WANG YY, WANG HX, DENG F. Study on the detection method of residual streptomycin in edible tissues of cattle by liquid chromatography tandem mass spectrometry[J]. Chinese Journal of Veterinary Medicine, 2018, 54(9): 99-103.
[16]
李伟岭, 范小平, 杨芳, 等. 高效液相色谱-串联质谱法检测猪可食性组织中加米霉素残留[J]. 中国兽医杂志, 2022, 58(4): 59-64.
LI WL, FAN XP, YANG F, et al. High performance liquid chromatography tandem mass spectrometry for detecting residues of streptomycin in edible pig tissues[J]. Chinese Journal of Veterinary Medicine, 2022, 58(4): 59-64.
[17]
陈心怡, 李丽苏, 刘佳娜. 等. 同位素内标-液相色谱-串联质谱测定牛奶中加米霉素[J]. 食品工业, 2023, 44(9): 247-252.
CHEN XY, LI LS, LIU JN, et al. Isotope internal standard liquid chromatography tandem mass spectrometry determination of streptomycin in milk[J]. Food Industry, 2023, 44(9): 247-252.
[18]
李丽苏, 岳振峰, 赵凤娟, 等. EMR-Lipid通过式固相萃取结合同位素稀释-高效液相色谱-串联质谱法测定牛奶中磺胺溴二甲嘧啶和磺胺乙氧嗪残留量[J/OL]. 分析试验室, 1-9. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html
LI LS, YUE ZF, ZHAO FJ, et al. Determination of sulfabromodimethazine and sulfaethoxypyridazine residues in milk by EMR-lipid solid phase extraction combined with isotopic dilution-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analysis Laboratory, 1-9. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html http://kns.cnki.net/kcms/detail/11.2017.TF.20240930.1011.006.html
[19]
胡珀, 卜媛媛, 金鹏, 等. QuEChERS EMR-Lipid净化结合同位素稀释-超高效液相色谱-串联质谱法同时测定蜂房及其制剂中10种真菌毒素[J]. 食品与药品, 2024, 26(4): 316-322.
HU B, BU YY, JIN P, et al. Simultaneous determination of ten mycotoxins in vespae nidus and its preparations by QuEChERS EMR-Lipid combined with isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry[J]. Food and Drug, 2024, 26(4): 316-322.
[20]
申磊, 柳溪, 羊银, 等. Captiva EMR-Lipid技术结合液相色谱-串联质谱法测定畜禽肉及内脏中4种抗生素残留[J]. 食品安全质量检测学报, 2024, 15(11): 220-228.
SHEN L, LIU X, YANG Y, et al. Determination of 4 kinds of antibiotics residues in meat and viscera of livestock and poultry by Captiva EMR-Lipid technology combined with liquid chromatography-tandem mass spectrometry[J]. Journal of Food Safety & Quality, 2024, 15(11): 220-228.
[21]
邱巧丽, 潘胜东, 王立, 等. 基于EMR-Lipid分散固相萃取-超高效液相色谱-串联质谱法同时测定牛肉中17种全氟烷基化合物[J]. 色谱, 2024, 42(11): 1032-1041.
QIU QL, PAN SD, WANG L, et al. Simultaneous determination of 17 perfluoroalkyl substances in beef by EMR-Lipid dispersive solid-phase extraction and ultra performance liquid chromatography tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2024, 42(11): 1032-1041.
[22]
温馨, 谭淑铧, 林庆昶, 等. QuEChERS dSPE EMR-Lipid-GC-MS/MS测定动物源性食品中205种农药及13种代谢物残留量[J]. 分析科学学报, 2024, 40(3): 324-336.
WEN X, TAN SH, LIN QX, et al. Determination of 205 pesticidesand 13 metabolites residuesin animal derived foods by QuEChERS dSPE EMR-Lipid-GC-MS-MS[J]. Journal of Analtical Science, 2024, 40(3): 324-336.
[23]
余晓琴, 闵宇航, 刘斯琪, 等. QuEChERS EMR-Lipid净化结合超高效液相色谱串联质谱法快速测定食品中非法添加工业染料[J]. 食品科学, 2024, 45(16): 268-283.
YU XQ, MIN YH, LIU SQ, et al. Rapid determination of illegal addition of industrial dyes in foods by QuEChERS using EMR-Lipid sorbent combined with ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Food Science, 2024, 45(16): 268-283.
[24]
马宁, 李洪波, 崔海燕, 等. Captiva EMR-Lipid固相萃取/超高效液相色谱-串联质谱快速筛查饲料中7种真菌毒素[J]. 饲料研究, 2024, 47(7): 116-120.
MA N, LI HB, CUI HY, et al. Captiva EMR-Lipid SPE/ultra performance liquid chromatography-tandem mass spectrometry rapid screening seven mycotoxins in feed[J]. Feed Research, 2024, 47(7): 116-120.
[25]
唐玥, 李少华, 陈达炜, 等. 糖诱导相分离/超高效液相色谱-高分辨质谱法测定牛奶中高氯酸盐含量[J]. 食品安全质量检测学报, 2024, 15(19): 228-234.
TANG Y, LI SH, CHEN DW, et al. Determination of perchlorate content in milk by sugar-induced phase separation and ultra performance liquid chromatography-high resolution mass spectrometry[J]. Journal of Food Safety & Quality, 2024, 15(19): 228-234.
[26]
梁艳婷, 杨奉筠, 贾艳丰, 等. 基于自建数据库的超高效液相色谱-四极杆-飞行时间质谱法定量测定玉米中5种真菌毒素[J]. 食品安全质量检测学报, 2024, 15(20): 279-287.
LIANG YT, YANG FJ, JIA YF, et al. Determination of 5 kinds of mycotoxins in Zea mays by ultra performance liquid chromatography- quadrupole-time-of-flight mass spectrometry based on self-established database[J]. Journal of Food Safety & Quality, 2024, 15(20): 279-287.
[27]
邱月, 陆嘉莉, 李根容, 等. QuEChERS增强型去脂质技术结合超高效液相色谱串联质谱法测定食用植物油中27种光稳定剂[J/OL]. 分析试验室, 1-11. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html
QIU Y, LU JL, LI GR, et al. Determination of 27 kinds of light stabilizer in edible plant oil by QuEChERS enhanced matrix removal-lipid technique combined with ultra high-performance liquid chromatography- tandem mass spectrometry[J]. Chinese Journal of Analysis Laboratory, 1-11. [2024-10-18]. http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html http://kns.cnki.net/kcms/detail/11.2017.tf.20241031.1412.016.html
[28]
李名路, 辛丽娜, 梁飞燕, 等. 固相萃取-超高效液相色谱-串联质谱法测定虾肉中40种精神类药物残留及基质效应[J]. 食品研究与开发, 2024, 45(21): 172-179.
LI ML, XIN LN, LIANG FY, et al. Determination of 40 Psychotropic drug residues and matrix effects in shrimp meat by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J]. Food Research and Development, 2024, 45(21): 172-179.
[29]
MATUSZEWSKI BK. Standard line slopes as a measure of a relative matrix effect in quantitative HPLC-MS bioanalysis[J]. Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences, 2006, 830(2): 293-300.
[30]
童兰艳, 许博舟, 聂雪梅, 等. 液相色谱-四极杆/静电场轨道阱质谱法测定牛奶中22种真菌毒素[J]. 色谱, 2023, 41(11): 986-994.
TONG LY, XU BZ, NIE XM, et al. Determination of 22 mycotoxins in milk by liquid chromatography-quadrupole/ orbitrap mass spectrometry[J]. Chinese Journal of Chromatography, 2023, 41(11): 986-994.
[31]
郭洋洋, 罗小清, 彭麟, 等. 猪可食性组织中加米霉素残留量的UPLC-MS/MS检测方法研究[J]. 畜牧与兽医, 2017, 49(6): 54-59.
GUO YY, LUO XQ, PENG L, et al. Development of an ultra-performance liquid chromatography-tandem mass spectrometry method for the determination of gamithromycin in edible swine tissues[J]. Animal Husbandry & Veterinary Medicine, 2017, 49(6): 54-59.
2025年第16卷第3期
PDF下载
268
96
引用本文
BibTeX
文章信息
doi: 10.19812/j.cnki.jfsq11-5956/ts.20241018002
  • 接收时间：2024-10-18
  • 首发时间：2025-07-21
  • 出版时间：2025-02-15
补充材料
相关文章
文章信息
作者
出版历史
  • 收稿日期：2024-10-18
基金
作者信息
    中检科(北京)测试技术有限公司, 北京 100176

通讯作者:

* 李克静(1981—), 女, 高级工程师, 主要研究方向为食品安全检测。E-mail:
参考文献
分享链接
https://castjournals.cast.org.cn/joweb/spaq/CN/10.19812/j.cnki.jfsq11-5956/ts.20241018002
分享至
全文二维码

扫描看全文

引用本文
BibTeX
本文的引用情况
2种不同金属材料的力学参数
科
Family		 属数
Number of
genus		 种数
Number of
species		 占总种数比例
Percentage of
total species (%)		 属
Genus		 种数
Number of
species		 占总种数比例
Percentage of total
species (%)
鹅膏菌科Amanitaceae 2 11 5.26 鹅膏菌属 Amanita 10 4.78
小菇科 Mycenaceae 2 12 5.74 丝盖伞属 Inocybe 5 2.39
多孔菌科 Polyporaceae 8 14 6.70 蜡蘑属 Laccaria 5 2.39
红菇科 Russulaceae 3 23 11.00 小皮伞属 Marasmius 6 2.87
小菇属 Mycena 11 5.26
光柄菇属 Pluteus 5 2.39
红菇属 Russula 17 8.13
栓菌属 Trametes 5 2.39
关闭全屏
相关链接
论文
最新文章
热读文章
热点专题
内参
蓝皮书
产业发展报告
传播力报告
期刊分级目录
资讯
学术新闻
行业新闻
学术会议
行业会议
关于
关于我们
联系我们
北京市海淀区学院南路86号
100081
010-62199257
qkjq@cast.org.cn

中国科学技术协会版权所有 京ICP 备10216604号-4 海淀分局备案 1101084647
科技导报社主办 中国科协信息中心技术支持