首页 期刊 论文 学科刊群 资讯 加盟 关于
EN
image
Article(id=1241676524861059483, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241676522256388920, articleNumber=null, orderNo=null, doi=10.20043/j.cnki.MPM.202406227, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=null, receivedDate=1718640000000, receivedDateStr=2024-06-18, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1773968352760, onlineDateStr=2026-03-20, pubDate=1731168000000, pubDateStr=2024-11-10, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1773968352760, onlineIssueDateStr=2026-03-20, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1773968352760, creator=13701087609, updateTime=1773968352760, updator=13701087609, issue=Issue{id=1241676522256388920, tenantId=1146029695717560320, journalId=1227665162245664772, year='2024', volume='51', issue='21', pageStart='3841', pageEnd='4032', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1773968352140, creator=13701087609, updateTime=1773968629818, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1241677686985249701, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241676522256388920, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1241677686985249702, tenantId=1146029695717560320, journalId=1227665162245664772, issueId=1241676522256388920, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=3985, endPage=3991, ext={EN=ArticleExt(id=1241676526983377342, articleId=1241676524861059483, tenantId=1146029695717560320, journalId=1227665162245664772, language=EN, title=QuEChERS-UHPLC-MS/MS method for determining residues of 45 antibiotics in eggs, columnId=1241676526886908346, journalTitle=Modern Preventive Medicine, columnName=Experimental Technology and ApplicationsExperimental Technology and Applications, runingTitle=null, highlight=null, articleAbstract=
Objective

To establish a QuEChERS-UHPLC-MS/MS method for the determination of residues of 45 antibiotics in eggs.

Methods

Samples were extracted using a 90% acetonitrile aqueous solution (containing 0.1% formic acid), and the supernatant was transferred to a QuEChERS tube (150 mg HLB-P + 50 mg PSA) for purification. The purified extract was concentrated to near dryness under nitrogen, and then reconstituted with 10% methanol aqueous solution (containing 0.1% formic acid). Target compounds were separated using a BEH C18 column (2.1×100 mm, 1.7 μm) with a gradient elution of 0.1% formic acid in water and 0.1% formic acid in methanol as the mobile phase. Detection was performed in positive ion multiple reaction monitoring mode, and quantification was achieved using matrix-matched calibration curves.

Results

Over the concentration range of 1.0 to 200 μg/L, all 45 target analytes exhibited good linear relationships in their regression equations. The method’s limit of detection was 1.0 μg/kg, with spiked recoveries ranging from 69.2% to 109.6% and relative standard deviations (RSD) between 1.2% and 15.8%.

Conclusion

This method is simple, rapid, and exhibits high accuracy and precision, making it suitable for the simultaneous detection of 45 antibiotics in eggs.

, correspAuthors=null, 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=Chun-hui HAO, Wei CUI, Yu-lu CHEN, Ling-fei LUO, Yan LI), CN=ArticleExt(id=1241676527641883098, articleId=1241676524861059483, tenantId=1146029695717560320, journalId=1227665162245664772, language=CN, title=QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋中45种抗生素残留量, columnId=1228016572288135432, journalTitle=现代预防医学, columnName=实验技术及其应用, runingTitle=null, highlight=null, articleAbstract=
目的

建立鸡蛋中45种抗生素残留量的QuEChERS-超高效液相色谱-串联质谱测定方法。

方法

样品经90%乙腈水溶液（含0.1%甲酸）提取后，取上清液至QuEChERS管（150 mg HLB-P + 50 mg PSA）净化，净化液氮吹至近干，10%甲醇水（含0.1%甲酸）定容。目标物经BEH C18柱（2.1×100 mm，1.7 μm）分离，以0.1%甲酸水-0.1%甲酸甲醇为流动相进行梯度洗脱，正离子多反应监测模式检测，基质匹配校准曲线法定量。

结果

在1.0～200 μg/L的范围内，45种目标分析物的回归方程均具有良好的线性关系。方法的检出限为1.0 μg/kg，加标回收率为69.2%～109.6%，RSD为1.2%～15.8%。

结论

该方法操作简单、快速，准确度和精密度均较高，适用于鸡蛋中45种抗生素的同时检测。

, correspAuthors=null, authorNote=null, correspAuthorsNote=
李琰，E-mail:
, copyrightStatement=本刊刊出的所有文章不代表中华预防医学会和本刊编委会的观点，除非特别声明。, copyrightOwner=中华预防医学会和四川大学华西公共卫生学院, extLink=null, articleAbsUrl=null, sourceXml=gday4j2CJwP2dVhtA4G6MA==, magXml=SlHAz+UCHdPZvwpF4Uw5DQ==, pdfUrl=null, pdf=aoRwX24PgsxKdNCZlqeUfQ==, pdfFileSize=784454, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=e/9gAYLw+o0L8Or1rKh55g==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=psjPkShDspCl6Lj7EbxwRw==, mapNumber=null, authorCompany=null, fund=null, authors=

郝春慧（1987—），女，硕士，主管技师，研究方向:环境及食品卫生化学检验

, authorsList=郝春慧, 崔伟, 陈雨露, 骆玲飞, 李琰)}, authors=[Author(id=1241821857003929978, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, orderNo=0, 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=1241821857125564805, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821857003929978, language=EN, stringName=Chun-hui HAO, firstName=Chun-hui, middleName=null, lastName=HAO, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1241821857205256586, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821857003929978, language=CN, stringName=郝春慧, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=上海市闵行区疾病预防控制中心理化检验科，上海 201101, bio={"content":"

郝春慧（1987—），女，硕士，主管技师，研究方向:环境及食品卫生化学检验

"}, bioImg=null, bioContent=

郝春慧（1987—），女，硕士，主管技师，研究方向:环境及食品卫生化学检验

, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1241821855401705832, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, xref=null, ext=[AuthorCompanyExt(id=1241821855405900137, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China), AuthorCompanyExt(id=1241821855418483050, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=上海市闵行区疾病预防控制中心理化检验科，上海 201101)])]), Author(id=1241821857343668626, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, 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=1241821857477886367, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821857343668626, language=EN, stringName=Wei CUI, firstName=Wei, middleName=null, lastName=CUI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1241821857586938279, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821857343668626, language=CN, stringName=崔伟, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=上海市闵行区疾病预防控制中心理化检验科，上海 201101, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1241821855401705832, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, xref=null, ext=[AuthorCompanyExt(id=1241821855405900137, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China), AuthorCompanyExt(id=1241821855418483050, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=上海市闵行区疾病预防控制中心理化检验科，上海 201101)])]), Author(id=1241821857737933235, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, 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=1241821857888928193, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821857737933235, language=EN, stringName=Yu-lu CHEN, firstName=Yu-lu, middleName=null, lastName=CHEN, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1241821858023145933, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821857737933235, language=CN, stringName=陈雨露, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=上海市闵行区疾病预防控制中心理化检验科，上海 201101, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1241821855401705832, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, xref=null, ext=[AuthorCompanyExt(id=1241821855405900137, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China), AuthorCompanyExt(id=1241821855418483050, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=上海市闵行区疾病预防控制中心理化检验科，上海 201101)])]), Author(id=1241821858178335198, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, 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=1241821858367078895, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821858178335198, language=EN, stringName=Ling-fei LUO, firstName=Ling-fei, middleName=null, lastName=LUO, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1241821858551628285, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821858178335198, language=CN, stringName=骆玲飞, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=上海市闵行区疾病预防控制中心理化检验科，上海 201101, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1241821855401705832, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, xref=null, ext=[AuthorCompanyExt(id=1241821855405900137, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China), AuthorCompanyExt(id=1241821855418483050, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=上海市闵行区疾病预防控制中心理化检验科，上海 201101)])]), Author(id=1241821858723594758, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, orderNo=4, firstName=null, middleName=null, lastName=null, nameCn=null, orcid=null, stid=null, country=null, authorPic=null, dead=0, email=lypoiuly-83@163.com, emailSecond=null, emailThird=null, correspondingAuthor=0, authorType=1, ext={EN=AuthorExt(id=1241821858862006799, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821858723594758, language=EN, stringName=Yan LI, firstName=Yan, middleName=null, lastName=LI, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1241821859017196060, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, authorId=1241821858723594758, language=CN, stringName=李琰, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=null, address=上海市闵行区疾病预防控制中心理化检验科，上海 201101, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1241821855401705832, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, xref=null, ext=[AuthorCompanyExt(id=1241821855405900137, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China), AuthorCompanyExt(id=1241821855418483050, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=上海市闵行区疾病预防控制中心理化检验科，上海 201101)])])], keywords=[Keyword(id=1241821859243688498, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=EN, orderNo=1, keyword=QuEChERS), Keyword(id=1241821859465986632, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=EN, orderNo=2, keyword=UHPLC-MS/MS), Keyword(id=1241821859616981589, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=EN, orderNo=3, keyword=Antibiotics), Keyword(id=1241821859776365151, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=EN, orderNo=4, keyword=Eggs), Keyword(id=1241821859939943018, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=CN, orderNo=1, keyword=QuEChERS), Keyword(id=1241821863437992568, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=CN, orderNo=2, keyword=超高效液相色谱-串联质谱法), Keyword(id=1241821863580598912, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=CN, orderNo=3, keyword=抗生素), Keyword(id=1241821863723205253, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=CN, orderNo=4, keyword=鸡蛋)], refs=[Reference(id=1241821866487251687, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2015, volume=12, issue=4, pageStart=90, pageEnd=91, 92, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=张萍, journalName=北方药学, refType=null, unstructuredReference=张萍.鸡蛋中抗生素类药物残留的研究进展[J].北方药学，2015，12（4）：90-91, 92., articleTitle=鸡蛋中抗生素类药物残留的研究进展, refAbstract=null), Reference(id=1241821866617275119, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2015, volume=12, issue=4, pageStart=90, pageEnd=91, 92, url=null, language=null, rfNumber=[1], rfOrder=1, authorNames=Zhang P, journalName=Journal of North Pharmacy, refType=null, unstructuredReference=Zhang P. Research progress on antibiotic residues in eggs[J]. Journal of North Pharmacy, 2015, 12(4): 90-91, 92.(In Chinese), articleTitle=Research progress on antibiotic residues in eggs, refAbstract=null), Reference(id=1241821866743104247, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2023, volume=29, issue=9, pageStart=651, pageEnd=655, url=null, language=null, rfNumber=[2], rfOrder=2, authorNames=侯学文, 邢燕, 高慧, journalName=预防医学论坛, refType=null, unstructuredReference=侯学文，邢燕，高慧，等.山东省市售鸡蛋中抗生素残留及暴露风险评估[J].预防医学论坛，2023，29（9）：651-655., articleTitle=山东省市售鸡蛋中抗生素残留及暴露风险评估, refAbstract=null), Reference(id=1241821866864739068, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2023, volume=29, issue=9, pageStart=651, pageEnd=655, url=null, language=null, rfNumber=[2], rfOrder=3, authorNames=Hou XW, Xing Y, Gao H, journalName=Preventive Medicine Tribune, refType=null, unstructuredReference=Hou XW, Xing Y, Gao H, et al. Risk assessment on antibiotic residues and exposure in commercially available eggs in Shandong province[J].Preventive Medicine Tribune, 2023, 29(9): 651-655.(In Chinese), articleTitle=Risk assessment on antibiotic residues and exposure in commercially available eggs in Shandong province, refAbstract=null), Reference(id=1241821866994762500, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2019, volume=46, issue=17, pageStart=3131, pageEnd=3133, url=null, language=null, rfNumber=[3], rfOrder=4, authorNames=刘孟文, 杨欢欢, 赵一鹏, journalName=现代预防医学, refType=null, unstructuredReference=刘孟文，杨欢欢，赵一鹏，等.陕西省329份市售鸡肉和鸡蛋中四环素类抗生素残留调查[J].现代预防医学，2019，46（17）：3131-3133., articleTitle=陕西省329份市售鸡肉和鸡蛋中四环素类抗生素残留调查, refAbstract=null), Reference(id=1241821867124785932, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2019, volume=46, issue=17, pageStart=3131, pageEnd=3133, url=null, language=null, rfNumber=[3], rfOrder=5, authorNames=Liu MW, Yang HH, Zhao YP, journalName=Modern Preventive Medicine, refType=null, unstructuredReference=Liu MW, Yang HH, Zhao YP, et al. Residues of tetracycline antibiotics in 329 chicken and eggs on market, Shaanxi[J]. Modern Preventive Medicine,2019, 46(17): 3131-3133.(In Chinese), articleTitle=Residues of tetracycline antibiotics in 329 chicken and eggs on market, Shaanxi, refAbstract=null), Reference(id=1241821867300946710, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2022, volume=34, issue=2, pageStart=292, pageEnd=296, url=null, language=null, rfNumber=[4], rfOrder=6, authorNames=肖永华, 革丽亚, 粱高道, journalName=中国食品卫生杂志, refType=null, unstructuredReference=肖永华，革丽亚，粱高道，等.湖北省鸡肉和鸡蛋中多组分抗生素残留分析[J].中国食品卫生杂志，2022，34（2）：292-296., articleTitle=湖北省鸡肉和鸡蛋中多组分抗生素残留分析, refAbstract=null), Reference(id=1241821867426775834, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2022, volume=34, issue=2, pageStart=292, pageEnd=296, url=null, language=null, rfNumber=[4], rfOrder=7, authorNames=Xiao YH, Ge LY, Liang GD, journalName=Chinese Journal of Food Hygiene, refType=null, unstructuredReference=Xiao YH, Ge LY, Liang GD, et al. Occurrence of multi-antibiotics in chicken and egg samples in Hubei[J]. Chinese Journal of Food Hygiene,2022, 34(2): 292-296.(In Chinese), articleTitle=Occurrence of multi-antibiotics in chicken and egg samples in Hubei, refAbstract=null), Reference(id=1241821867535827745, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2023, volume=35, issue=7, pageStart=1063, pageEnd=1066, url=null, language=null, rfNumber=[5], rfOrder=8, authorNames=王姝婷, 黄希汇, 刘少颖, journalName=中国食品卫生杂志, refType=null, unstructuredReference=王姝婷，黄希汇，刘少颖，等.市售鸡肉与鸡蛋中四环素类抗生素残留调查与膳食暴露风险评估[J].中国食品卫生杂志，2023，35（7）：1063-1066., articleTitle=市售鸡肉与鸡蛋中四环素类抗生素残留调查与膳食暴露风险评估, refAbstract=null), Reference(id=1241821867623908138, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2023, volume=35, issue=7, pageStart=1063, pageEnd=1066, url=null, language=null, rfNumber=[5], rfOrder=9, authorNames=Wang ST, Huang XH, Liu SY, journalName=Chinese Journal of Food Hygiene, refType=null, unstructuredReference=Wang ST, Huang XH, Liu SY, et al. Investigation and dietary exposure risk assessment of tetracycline antibiotics residues in eggs and chicken sold on the market[J]. Chinese Journal of Food Hygiene, 2023, 35(7): 1063-1066.(In Chinese), articleTitle=Investigation and dietary exposure risk assessment of tetracycline antibiotics residues in eggs and chicken sold on the market, refAbstract=null), Reference(id=1241821867737154353, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2024, volume=40, issue=3, pageStart=382, pageEnd=388, url=null, language=null, rfNumber=[6], rfOrder=10, authorNames=郝春慧, 崔伟, 骆玲飞, journalName=中国公共卫生, refType=null, unstructuredReference=郝春慧，崔伟，骆玲飞，等.水中52种抗生素全自动固相萃取-超高效液相色谱-串联质谱法测定[J].中国公共卫生，2024，40（3）：382-388., articleTitle=水中52种抗生素全自动固相萃取-超高效液相色谱-串联质谱法测定, refAbstract=null), Reference(id=1241821867900732221, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2024, volume=40, issue=3, pageStart=382, pageEnd=388, url=null, language=null, rfNumber=[6], rfOrder=11, authorNames=Hao CH, Cui W, Luo LF, journalName=Chinese Journal of Public Health, refType=null, unstructuredReference=Hao CH, Cui W, Luo LF, et al. Determination of 52 antibiotics in water through a fully automated solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry system[J]. Chinese Journal of Public Health, 2024, 40(3): 382-388.(In Chinese), articleTitle=Determination of 52 antibiotics in water through a fully automated solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry system, refAbstract=null), Reference(id=1241821868022367043, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2017, volume=27, issue=4, pageStart=473, pageEnd=476, url=null, language=null, rfNumber=[7], rfOrder=12, authorNames=王敏娟, 胡佳薇, 田丽, journalName=中国卫生检验杂志, refType=null, unstructuredReference=王敏娟，胡佳薇，田丽，等.超高效液相色谱-串联质谱法同时测定鸡蛋中21种喹诺酮及四环素类抗生素残留[J].中国卫生检验杂志，2017，27（4）：473-476., articleTitle=超高效液相色谱-串联质谱法同时测定鸡蛋中21种喹诺酮及四环素类抗生素残留, refAbstract=null), Reference(id=1241821868181750601, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2017, volume=27, issue=4, pageStart=473, pageEnd=476, url=null, language=null, rfNumber=[7], rfOrder=13, authorNames=Wang MJ, Hu JW, Tian L, journalName=Chinese Journal of Health Laboratory Technology, refType=null, unstructuredReference=Wang MJ, Hu JW, Tian L, et al. Simultaneous determination of quinoline and tetracycline residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Health Laboratory Technology, 2017, 27(4): 473-476.(In Chinese), articleTitle=Simultaneous determination of quinoline and tetracycline residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1241821868341134166, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2018, volume=45, issue=24, pageStart=4482, pageEnd=4486, 4490, url=null, language=null, rfNumber=[8], rfOrder=14, authorNames=李磊, 周贻兵, 张权, journalName=现代预防医学, refType=null, unstructuredReference=李磊，周贻兵，张权，等.QuEChERS净化超高效液相色谱-串联质谱法快速测定鸡蛋中13种喹诺酮类抗生素[J].现代预防医学，2018，45（24）：4482-4486, 4490., articleTitle=QuEChERS净化超高效液相色谱-串联质谱法快速测定鸡蛋中13种喹诺酮类抗生素, refAbstract=null), Reference(id=1241821868487934814, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2018, volume=45, issue=24, pageStart=4482, pageEnd=4486, 4490, url=null, language=null, rfNumber=[8], rfOrder=15, authorNames=Li L, Zhou YB, Zhang Q, journalName=Modern Preventive Medicine, refType=null, unstructuredReference=Li L, Zhou YB, Zhang Q, et al. Rapid determination of 13 quinolones antibiotics in eggs by QuEChERS purification combined with ultra-high-performance liquid chromatography-tandem mass spectrometry[J]. Modern Preventive Medicine, 2018, 45(24): 4482-4486, 4490.(In Chinese), articleTitle=Rapid determination of 13 quinolones antibiotics in eggs by QuEChERS purification combined with ultra-high-performance liquid chromatography-tandem mass spectrometry, refAbstract=null), Reference(id=1241821868622152549, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2018, volume=28, issue=8, pageStart=910, pageEnd=914, 921, url=null, language=null, rfNumber=[9], rfOrder=16, authorNames=廖艳华, 周劭桓, 林文斯, journalName=中国卫生检验杂志, refType=null, unstructuredReference=廖艳华，周劭桓，林文斯，等.超高效液相色谱-串联质谱法测定鸡蛋中11种喹诺酮类抗生素残留的样品前处理方法优化[J].中国卫生检验杂志，2018，28（8）：910-914, 921., articleTitle=超高效液相色谱-串联质谱法测定鸡蛋中11种喹诺酮类抗生素残留的样品前处理方法优化, refAbstract=null), Reference(id=1241821868773147504, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2018, volume=28, issue=8, pageStart=910, pageEnd=914, 921, url=null, language=null, rfNumber=[9], rfOrder=17, authorNames=Liao YH, Zhou SH, Lin WS, journalName=Chinese Journal of Health Laboratory Technology, refType=null, unstructuredReference=Liao YH, Zhou SH, Lin WS, et al. Optimization of sample pretreatment method for determination of 11 quinolone antibiotic residues in eggs by UPLC-MS/MS[J]. Chinese Journal of Health Laboratory Technology, 2018,28(8): 910-914, 921.(In Chinese), articleTitle=Optimization of sample pretreatment method for determination of 11 quinolone antibiotic residues in eggs by UPLC-MS/MS, refAbstract=null), Reference(id=1241821868898976630, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2021, volume=127, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[10], rfOrder=18, authorNames=Paoletti F, Sdogati S, Barola C, journalName=Food Control, refType=null, unstructuredReference=Paoletti F, Sdogati S, Barola C, et al. Development and validation of a multiclass confirmatory method for the determination of over 60 antibiotics in eggs using liquid-chromatography high-resolution mass spectrometry[J]. Food Control, 2021, 127: 108109., articleTitle=Development and validation of a multiclass confirmatory method for the determination of over 60 antibiotics in eggs using liquid-chromatography high-resolution mass spectrometry, refAbstract=null), Reference(id=1241821870450869115, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2018, volume=1532, issue=null, pageStart=20, pageEnd=29, url=null, language=null, rfNumber=[11], rfOrder=19, authorNames=Zhou J, Xu JJ, Cong JM, journalName=Journal of Chromatography a, refType=null, unstructuredReference=Zhou J, Xu JJ, Cong JM, et al. Optimization for quick, easy, cheap,effective, rugged and safe extraction of mycotoxins and veterinary drugs by response surface methodology for application to egg and milk[J]. Journal of Chromatography a, 2018, 1532: 20-29., articleTitle=Optimization for quick, easy, cheap,effective, rugged and safe extraction of mycotoxins and veterinary drugs by response surface methodology for application to egg and milk, refAbstract=null), Reference(id=1241821870618641284, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2024, volume=22, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[12], rfOrder=20, authorNames=Yang Y, Li X, Lin J, journalName=Food Chemistry: X, refType=null, unstructuredReference=Yang Y, Li X, Lin J, et al. A modified QuEChERS-based UPLC-MS/MS method for rapid determination of multiple antibiotics and sedative residues in freshwater fish[J]. Food Chemistry: X, 2024, 22:101268., articleTitle=A modified QuEChERS-based UPLC-MS/MS method for rapid determination of multiple antibiotics and sedative residues in freshwater fish, refAbstract=null), Reference(id=1241821870761247624, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2019, volume=1104, issue=null, pageStart=182, pageEnd=189, url=null, language=null, rfNumber=[13], rfOrder=21, authorNames=Gajda A, Nowacka-Kozak E, Gbylik-Sikorska M, journalName=Journal of Chromatography B, refType=null, unstructuredReference=Gajda A,Nowacka-Kozak E,Gbylik-Sikorska M,et al. Multi-residues UHPLC–MS/MS analysis of 53 antibacterial compounds in poultry feathers as an analytical tool in food safety assurance[J].Journal of Chromatography B, 2019, 1104: 182-189., articleTitle=Multi-residues UHPLC–MS/MS analysis of 53 antibacterial compounds in poultry feathers as an analytical tool in food safety assurance, refAbstract=null), Reference(id=1241821870887076753, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2016, volume=1429, issue=null, pageStart=175, pageEnd=188, url=null, language=null, rfNumber=[14], rfOrder=22, authorNames=Moretti S, Dusi G, Giusepponi D, journalName=Journal of Chromatography a, refType=null, unstructuredReference=Moretti S, Dusi G, Giusepponi D, et al. Screening and confirmatory method for multiclass determination of 62 antibiotics in meat[J].Journal of Chromatography a, 2016, 1429: 175-188., articleTitle=Screening and confirmatory method for multiclass determination of 62 antibiotics in meat, refAbstract=null), Reference(id=1241821871012905879, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2022, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[15], rfOrder=23, authorNames=国家市场监督管理总局, journalName=null, refType=null, unstructuredReference=国家市场监督管理总局.GB 31650.1-2022 食品安全国家标准-食品中41种兽药最大残留限量[S].北京：中国农业出版社，2022., articleTitle=null, refAbstract=null), Reference(id=1241821871163900832, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, doi=null, pmid=null, pmcid=null, year=2022, volume=null, issue=null, pageStart=null, pageEnd=null, url=null, language=null, rfNumber=[15], rfOrder=24, authorNames=State Administration for Market Regulation, journalName=null, refType=null, unstructuredReference=State Administration for Market Regulation. GB 31650.1-2022 National food safety standard - Maximum residue limits for 41 veterinary drugs in foods[S]. Beijing: China Agriculture Press, 2022., articleTitle=null, refAbstract=null)], funds=null, companyList=[AuthorCompany(id=1241821855401705832, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, xref=null, ext=[AuthorCompanyExt(id=1241821855405900137, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China), AuthorCompanyExt(id=1241821855418483050, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, companyId=1241821855401705832, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=上海市闵行区疾病预防控制中心理化检验科，上海 201101)])], figs=[ArticleFig(id=1241821864025195168, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=EN, label=Figure 1, caption=Total ion chromatogram of 45 antibiotics added to eggs at a level of 100 μg/kg, figureFileSmall=/hiyc49ZAjRtOy+4EO4Vwg==, figureFileBig=tpW340ncMTx3DijW/hVY+w==, tableContent=null), ArticleFig(id=1241821864155218602, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=CN, label=图1, caption=鸡蛋中45种抗生素添加水平为100 μg/kg的总离子流图, figureFileSmall=/hiyc49ZAjRtOy+4EO4Vwg==, figureFileBig=tpW340ncMTx3DijW/hVY+w==, tableContent=null), ArticleFig(id=1241821864348156600, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=EN, label=Table 1, caption=

Molecular weight, retention time, and mass spectrometric parameters of 45 antibiotics

, figureFileSmall=null, figureFileBig=null, tableContent=
编号抗生素名称分子量保留时间(min)母离子子离子碰撞电压(V)锥孔电压(V)
1磺胺醋酰(Sulfacetamide)214.241.97215.1155.9*/92.114/2960
2磺胺嘧啶(Sulfadiazine)250.282.78251.0108.0*/91.932/3450
3磺胺噻唑(Sulfathiazole)255.323.32256.191.9*/108.137/3370
4磺胺吡啶(Sulfapyridine)249.293.58250.0184.0*/108.024/3370
5磺胺甲基嘧啶(Sulfamerazine)264.303.87265.1155.8*/92.024/4180
6磺胺对甲氧嘧啶(Sulfameter)280.314.55281.092.0*/108.043/3360
7磺胺甲噻二唑(Sulfamethizole)270.334.71271.1155.7*/91.919/3810
8磺胺二甲基嘧啶(Sulfamethazine)278.334.78279.1186.0*/124.225/2970
9甲氧苄啶(Trimethoprim)290.324.86291.1260.9*/123.134/3390
10磺胺甲氧哒嗪(Sulfamethoxypyridazine)280.305.03281.0156.2*/92.024/3860
11氧氟沙星(Ofloxacin)361.375.13362.1261.0*/344.038/30100
12培氟沙星(Pefloxacin)333.265.14334.1315.9*/233.130/3690
13依诺沙星(Enoxacin)320.325.17321.1303.0*/231.927/47110
14诺氟沙星(Norfloxacin)319.335.32320.2301.9*/233.028/34100
15磺胺氯哒嗪(Sulfachloropyridazine)284.725.32285.1156.0*/91.923/4120
16四环素(Tetracycline)444.355.37445.1409.9*/427.026/1920
17环丙沙星(Ciprofloxacin)331.345.51332.1314.0*/230.828/4790
18磺胺甲基异噁唑(Sulfamethoxazole)253.285.51254.191.9*/107.937/3470
19土霉素(Oxytetracycline)460.625.51461.2425.8*/201.028/5120
20磺胺间甲氧嘧啶(Sulfamonomethoxine)280.305.59281.1125.9*/108.026/3570
21恩诺沙星(Enrofloxacin)359.395.64360.1316.1*/245.027/3790
22洛美沙星(Lomefloxacin)351.365.80352.1265.0*/237.031/46110
23磺胺邻二甲氧嘧啶(Sulfadoxine)310.335.86311.0156.0*/91.925/4160
24奥比沙星(Orbifloxacin)395.385.89396.2294.9*/378.033/28110
25磺胺二甲基异噁唑(Sulfisoxazole)267.305.89268.1112.9*/92.120/4070
26双氟沙星(Difloxacin)399.245.93400.1382.0*/299.030/3990
27沙拉沙星(Sarafloxacin)385.136.09386.1367.9*/342.032/27110
28磺胺苯酰(Sulfabenzamide)276.316.19277.1156.2*/92.017/3670
29磺胺苯吡唑(Sulfaphenazole)314.366.51315.1158.0*/131.137/6680
30克林沙星(Clinafloxacin)365.796.54366.1347.9*/304.827/3090
31司帕沙星(Sparfloxacin)392.406.55393.2291.9*/250.736/43120
32西诺沙星(Cinoxacin)262.226.67263.1245.0*/216.922/3180
33金霉素(Chlortetracycline)478.756.79479.1444.1*/153.929/3680
34磺胺间二甲氧嘧啶(Sulfadimethoxine)310.336.83311.1156.0*/107.926/3780
35恶喹酸(Oxolinic acid)261.237.02262.1244.0*/215.941/4150
36磺胺喹恶啉(Sulfaquinoxaline)300.347.05301.1156.0*/92.023/4180
37多西环素(Doxycycline)444.217.65445.1428.0*/409.927/3410
38萘啶酸(Nalidixic acid)232.247.95233.1187.0*/159.034/4460
39替米考星(Tilmicosin)869.137.98869.6696.4*/174.157/5430
40氟甲喹(Flumequine)261.258.23262.1244.0*/202.026/4570
41磷酸竹桃霉素(Oleandomycin phosphate)687.868.36688.3544.2*/158.023/3530
42泰乐菌素(Tylosin)916.109.14916.5772.3*/174.242/4840
43克拉霉素(Clarithromycin)747.9510.36748.5590.1*/158.028/3540
44阿奇霉素(Azithromycin)748.9810.37749.6591.1*/157.927/3320
45罗红霉素(Roxithromycin)837.0510.57837.6679.3*/158.031/4040
), ArticleFig(id=1241821864457208511, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=CN, label=表1, caption=

45种抗生素的分子量、保留时间和质谱参数

, figureFileSmall=null, figureFileBig=null, tableContent=
编号抗生素名称分子量保留时间(min)母离子子离子碰撞电压(V)锥孔电压(V)
1磺胺醋酰(Sulfacetamide)214.241.97215.1155.9*/92.114/2960
2磺胺嘧啶(Sulfadiazine)250.282.78251.0108.0*/91.932/3450
3磺胺噻唑(Sulfathiazole)255.323.32256.191.9*/108.137/3370
4磺胺吡啶(Sulfapyridine)249.293.58250.0184.0*/108.024/3370
5磺胺甲基嘧啶(Sulfamerazine)264.303.87265.1155.8*/92.024/4180
6磺胺对甲氧嘧啶(Sulfameter)280.314.55281.092.0*/108.043/3360
7磺胺甲噻二唑(Sulfamethizole)270.334.71271.1155.7*/91.919/3810
8磺胺二甲基嘧啶(Sulfamethazine)278.334.78279.1186.0*/124.225/2970
9甲氧苄啶(Trimethoprim)290.324.86291.1260.9*/123.134/3390
10磺胺甲氧哒嗪(Sulfamethoxypyridazine)280.305.03281.0156.2*/92.024/3860
11氧氟沙星(Ofloxacin)361.375.13362.1261.0*/344.038/30100
12培氟沙星(Pefloxacin)333.265.14334.1315.9*/233.130/3690
13依诺沙星(Enoxacin)320.325.17321.1303.0*/231.927/47110
14诺氟沙星(Norfloxacin)319.335.32320.2301.9*/233.028/34100
15磺胺氯哒嗪(Sulfachloropyridazine)284.725.32285.1156.0*/91.923/4120
16四环素(Tetracycline)444.355.37445.1409.9*/427.026/1920
17环丙沙星(Ciprofloxacin)331.345.51332.1314.0*/230.828/4790
18磺胺甲基异噁唑(Sulfamethoxazole)253.285.51254.191.9*/107.937/3470
19土霉素(Oxytetracycline)460.625.51461.2425.8*/201.028/5120
20磺胺间甲氧嘧啶(Sulfamonomethoxine)280.305.59281.1125.9*/108.026/3570
21恩诺沙星(Enrofloxacin)359.395.64360.1316.1*/245.027/3790
22洛美沙星(Lomefloxacin)351.365.80352.1265.0*/237.031/46110
23磺胺邻二甲氧嘧啶(Sulfadoxine)310.335.86311.0156.0*/91.925/4160
24奥比沙星(Orbifloxacin)395.385.89396.2294.9*/378.033/28110
25磺胺二甲基异噁唑(Sulfisoxazole)267.305.89268.1112.9*/92.120/4070
26双氟沙星(Difloxacin)399.245.93400.1382.0*/299.030/3990
27沙拉沙星(Sarafloxacin)385.136.09386.1367.9*/342.032/27110
28磺胺苯酰(Sulfabenzamide)276.316.19277.1156.2*/92.017/3670
29磺胺苯吡唑(Sulfaphenazole)314.366.51315.1158.0*/131.137/6680
30克林沙星(Clinafloxacin)365.796.54366.1347.9*/304.827/3090
31司帕沙星(Sparfloxacin)392.406.55393.2291.9*/250.736/43120
32西诺沙星(Cinoxacin)262.226.67263.1245.0*/216.922/3180
33金霉素(Chlortetracycline)478.756.79479.1444.1*/153.929/3680
34磺胺间二甲氧嘧啶(Sulfadimethoxine)310.336.83311.1156.0*/107.926/3780
35恶喹酸(Oxolinic acid)261.237.02262.1244.0*/215.941/4150
36磺胺喹恶啉(Sulfaquinoxaline)300.347.05301.1156.0*/92.023/4180
37多西环素(Doxycycline)444.217.65445.1428.0*/409.927/3410
38萘啶酸(Nalidixic acid)232.247.95233.1187.0*/159.034/4460
39替米考星(Tilmicosin)869.137.98869.6696.4*/174.157/5430
40氟甲喹(Flumequine)261.258.23262.1244.0*/202.026/4570
41磷酸竹桃霉素(Oleandomycin phosphate)687.868.36688.3544.2*/158.023/3530
42泰乐菌素(Tylosin)916.109.14916.5772.3*/174.242/4840
43克拉霉素(Clarithromycin)747.9510.36748.5590.1*/158.028/3540
44阿奇霉素(Azithromycin)748.9810.37749.6591.1*/157.927/3320
45罗红霉素(Roxithromycin)837.0510.57837.6679.3*/158.031/4040
), ArticleFig(id=1241821865983935177, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=EN, label=Table 2, caption=

Regression equations, correlation coefficients, and spiked recoveries of the method (n=7)

, figureFileSmall=null, figureFileBig=null, tableContent=
编号化合物名称回归方程相关系数(r)加标2 μg/kg加标10 μg/kg加标100 μg/kg
回收率(%)RSD(%)回收率(%)RSD(%)回收率(%)RSD(%)
1磺胺醋酰y=20 045x+17 2810.998 076.915.784.611.783.04.2
2磺胺嘧啶y=3.390×104x -9101.000 076.66.571.08.972.97.9
3磺胺噻唑y=3.634×104 -1 8840.997 579.87.977.67.173.44.4
4磺胺吡啶y=3.760×104x+2 5440.998 973.29.474.49.172.94.5
5磺胺甲基嘧啶y=5.232×104x+13 5230.998 473.710.274.27.473.56.9
6磺胺对甲氧嘧啶y=4.171×104x+1 6180.998 380.18.480.211.578.63.6
7磺胺甲噻二唑y=5.234×104x+20 6460.996 670.09.475.58.573.19.6
8磺胺二甲基嘧啶y=7.910×104x+24 4700.996 576.813.774.16.476.45.3
9甲氧苄啶y=1.098×105x+27 0760.997 997.111.197.513.687.64.9
10磺胺甲氧哒嗪y=8.382×104x+3 4690.998 782.813.081.611.480.85.2
11氧氟沙星y=9.536×104x+7 6310.999 080.86.981.38.982.67.0
12培氟沙星y=8.610×104x+1.176×1050.997 681.313.277.613.189.56.0
13依诺沙星y=1.572×105x+9.210×1040.996 583.810.586.815.588.26.5
14诺氟沙星y=1.067×105x+4.046×1040.999 285.912.085.29.082.05.0
15磺胺氯哒嗪y=8.536×104x+19 5980.999 278.74.075.56.478.44.5
16四环素y=8.546×104x+3 0060.998 769.210.671.62.572.611.6
17环丙沙星y=1.157×105x+2.172×1050.998 971.312.079.512.792.45.5
18磺胺甲基异噁唑y=3.164×104x+1 1320.999 986.210.184.27.483.67.4
19土霉素y=7.029×104x-3.801×1040.999 273.68.073.313.280.83.7
20磺胺间甲氧嘧啶y=4.149×104x +31 7990.999 788.011.580.99.877.81.2
21恩诺沙星y=261 679x - 59 2890.999 282.98.087.714.587.614.5
22洛美沙星y=8.525×104x -20 4620.998 890.68.684.76.689.74.3
23磺胺邻二甲氧嘧啶y=1.385×105x+6.251×1040.999 576.27.887.710.586.96.3
24奥比沙星y=8.457×104x+7.716×1040.996 382.110.289.98.091.94.6
25磺胺二甲基异噁唑y=3.878×104x+3.500×1040.996 985.613.182.46.788.610.2
26双氟沙星y=6.698×104x+2.341×1050.998 285.312.279.15.988.67.1
27沙拉沙星y=7.404×104x+4 8780.995 990.713.381.39.981.58.9
28磺胺苯酰y=4.222×104x+9 7390.997 971.613.372.44.979.07.3
29磺胺苯吡唑y=5.664×104x+1.057×1050.999 5105.78.685.46.685.42.1
30克林沙星y=6.584×104x +12 1150.999 783.36.780.312.481.41.9
31司帕沙星y=6.054×104x-5760.999 290.46.581.28.288.38.2
32西诺沙星y=1.573×105x-3.423×1040.999 294.68.684.89.890.65.6
33金霉素y=5.872×104x-4.344×1040.997 475.011.475.86.875.48.2
34磺胺间二甲氧嘧啶y=1.109×105x+3.188×1040.997 572.713.281.99.382.76.7
35恶喹酸y=7.300×104x-3 7060.996 284.915.880.912.384.63.3
36磺胺喹恶啉y=5.630×104x+9 4460.998 376.411.879.212.183.09.8
37多西环素y=8.792×104x-1.515×1050.998 887.88.381.58.081.54.1
38萘啶酸y=2.419×105x+1.979×1050.996 681.311.5109.610.9104.58.3
39替米考星y=9 340x+1 0210.998 787.69.993.113.094.16.2
40氟甲喹y=2.193×105x+1.299×1060.995 175.74.789.95.193.110.7
41磷酸竹桃霉素y=1.621×105x+8 0830.997 976.57.884.68.890.45.9
42泰乐菌素y=13 014x+7 3480.998 774.98.482.312.385.96.7
43克拉霉素y=1.588×105x+1.461×1050.995 377.410.0101.67.1101.77.6
44阿奇霉素y=6.612×104x+17 5970.997 985.512.793.812.792.82.1
45罗红霉素y=1.749×105x+8.007×1040.998 178.82.291.16.395.74.9
), ArticleFig(id=1241821866143318735, tenantId=1146029695717560320, journalId=1227665162245664772, articleId=1241676524861059483, language=CN, label=表2, caption=

方法的回归方程、相关系数及加标回收率（n=7）

, figureFileSmall=null, figureFileBig=null, tableContent=
编号化合物名称回归方程相关系数(r)加标2 μg/kg加标10 μg/kg加标100 μg/kg
回收率(%)RSD(%)回收率(%)RSD(%)回收率(%)RSD(%)
1磺胺醋酰y=20 045x+17 2810.998 076.915.784.611.783.04.2
2磺胺嘧啶y=3.390×104x -9101.000 076.66.571.08.972.97.9
3磺胺噻唑y=3.634×104 -1 8840.997 579.87.977.67.173.44.4
4磺胺吡啶y=3.760×104x+2 5440.998 973.29.474.49.172.94.5
5磺胺甲基嘧啶y=5.232×104x+13 5230.998 473.710.274.27.473.56.9
6磺胺对甲氧嘧啶y=4.171×104x+1 6180.998 380.18.480.211.578.63.6
7磺胺甲噻二唑y=5.234×104x+20 6460.996 670.09.475.58.573.19.6
8磺胺二甲基嘧啶y=7.910×104x+24 4700.996 576.813.774.16.476.45.3
9甲氧苄啶y=1.098×105x+27 0760.997 997.111.197.513.687.64.9
10磺胺甲氧哒嗪y=8.382×104x+3 4690.998 782.813.081.611.480.85.2
11氧氟沙星y=9.536×104x+7 6310.999 080.86.981.38.982.67.0
12培氟沙星y=8.610×104x+1.176×1050.997 681.313.277.613.189.56.0
13依诺沙星y=1.572×105x+9.210×1040.996 583.810.586.815.588.26.5
14诺氟沙星y=1.067×105x+4.046×1040.999 285.912.085.29.082.05.0
15磺胺氯哒嗪y=8.536×104x+19 5980.999 278.74.075.56.478.44.5
16四环素y=8.546×104x+3 0060.998 769.210.671.62.572.611.6
17环丙沙星y=1.157×105x+2.172×1050.998 971.312.079.512.792.45.5
18磺胺甲基异噁唑y=3.164×104x+1 1320.999 986.210.184.27.483.67.4
19土霉素y=7.029×104x-3.801×1040.999 273.68.073.313.280.83.7
20磺胺间甲氧嘧啶y=4.149×104x +31 7990.999 788.011.580.99.877.81.2
21恩诺沙星y=261 679x - 59 2890.999 282.98.087.714.587.614.5
22洛美沙星y=8.525×104x -20 4620.998 890.68.684.76.689.74.3
23磺胺邻二甲氧嘧啶y=1.385×105x+6.251×1040.999 576.27.887.710.586.96.3
24奥比沙星y=8.457×104x+7.716×1040.996 382.110.289.98.091.94.6
25磺胺二甲基异噁唑y=3.878×104x+3.500×1040.996 985.613.182.46.788.610.2
26双氟沙星y=6.698×104x+2.341×1050.998 285.312.279.15.988.67.1
27沙拉沙星y=7.404×104x+4 8780.995 990.713.381.39.981.58.9
28磺胺苯酰y=4.222×104x+9 7390.997 971.613.372.44.979.07.3
29磺胺苯吡唑y=5.664×104x+1.057×1050.999 5105.78.685.46.685.42.1
30克林沙星y=6.584×104x +12 1150.999 783.36.780.312.481.41.9
31司帕沙星y=6.054×104x-5760.999 290.46.581.28.288.38.2
32西诺沙星y=1.573×105x-3.423×1040.999 294.68.684.89.890.65.6
33金霉素y=5.872×104x-4.344×1040.997 475.011.475.86.875.48.2
34磺胺间二甲氧嘧啶y=1.109×105x+3.188×1040.997 572.713.281.99.382.76.7
35恶喹酸y=7.300×104x-3 7060.996 284.915.880.912.384.63.3
36磺胺喹恶啉y=5.630×104x+9 4460.998 376.411.879.212.183.09.8
37多西环素y=8.792×104x-1.515×1050.998 887.88.381.58.081.54.1
38萘啶酸y=2.419×105x+1.979×1050.996 681.311.5109.610.9104.58.3
39替米考星y=9 340x+1 0210.998 787.69.993.113.094.16.2
40氟甲喹y=2.193×105x+1.299×1060.995 175.74.789.95.193.110.7
41磷酸竹桃霉素y=1.621×105x+8 0830.997 976.57.884.68.890.45.9
42泰乐菌素y=13 014x+7 3480.998 774.98.482.312.385.96.7
43克拉霉素y=1.588×105x+1.461×1050.995 377.410.0101.67.1101.77.6
44阿奇霉素y=6.612×104x+17 5970.997 985.512.793.812.792.82.1
45罗红霉素y=1.749×105x+8.007×1040.998 178.82.291.16.395.74.9
)], attaches=null, journal=Journal(id=1227664546253402114, delFlag=0, nameCn=现代预防医学, nameEn=Modern Preventive Medicine, nameHistory1=null, nameHistory2=null, issn=1003-8507, eissn=null, cn=51-1365/R, coden=null, periodic=3, language=CN, oaType=null, ccby=null, 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=IeiuPXEZi6AA+k0VfvoiOQ==, journalPrice=null, startedYear=null, abbrevIsoEn=Modern Preventive Medicine, journalRemark=null, publicationField=null, createdTime=1770627636734, updatedTime=1770628902248, createdBy=18614031015, updatedBy=13701087609, firstLetterCn=M, firstLetterEn=M, subjectCode=Life Sciences, subjectName=null, subjectCodeEn=Life Sciences, subjectNameEn=null, picCn=IeiuPXEZi6AA+k0VfvoiOQ==, picEn=/9iTl8/ndms4tBz1fL28Pg==, jcr=null, cjcr=null, exts=[JournalExt(id=1227669854342280188, language=CN, name=现代预防医学, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1770628902278, updatedTime=1770628902278, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=http://xdyfyxzz.paperopen.com/#/regist, submissionEditorUrl=http://xdyfyxzz.paperopen.com/#/Login, submissionReviewUrl=http://xdyfyxzz.paperopen.com/#/Login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""}), JournalExt(id=1227669854396806141, language=EN, name=Modern Preventive Medicine, nameHistory1=null, nameHistory2=null, managedBy=, sponsoredBy=, publishedBy=, editorOffice=, officeProv=null, officeCity=null, officeAddr=, officeZip=, editDirector=, officeDirector=null, officePhone=null, coverPicUrl=null, journalRemark=, submitArticleUrl=null, websiteUrl=, createdTime=1770628902291, updatedTime=1770628902291, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=http://xdyfyxzz.paperopen.com/#/regist, submissionEditorUrl=http://xdyfyxzz.paperopen.com/#/Login, submissionReviewUrl=http://xdyfyxzz.paperopen.com/#/Login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""})], databaseList=null, tenantJournalId=1227665162245664772, websiteList=[Website(id=1227687234141352800, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1227665162245664772, 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/xdyfyx/CN, language=CN, createTime=1770633045945, createBy=18614031015, updateTime=1770633090526, updateBy=18614031015, name=现代预防医学-中文, tplId=1146099689490845704, title=现代预防医学, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1227687735088051072, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=articleTextType, value=kx, createTime=1770633165380, updateTime=1770633165380, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735071273853, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=banner, value=null, createTime=1770633165376, updateTime=1770633165376, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735113216899, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=grayFlag, value=0, createTime=1770633165386, updateTime=1770633165386, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735062885244, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=logo, value=https://castjournals.cast.org.cn/joweb/xdyfyx/CN/file/pic?fileId=/XB5plC0xuykmQnycvtyrw==, createTime=1770633165374, updateTime=1770633165374, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735125799813, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=minRunFlag, value=0, createTime=1770633165389, updateTime=1770633165389, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735083856767, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/xdyfyx/CN/file/pic, createTime=1770633165379, updateTime=1770633165379, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735121605508, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=silenceFlag, value=0, createTime=1770633165388, updateTime=1770633165388, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735079662462, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_cn_619/, createTime=1770633165378, updateTime=1770633165378, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735096439681, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=themeColor, value=null, createTime=1770633165382, updateTime=1770633165382, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687735104828290, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234141352800, code=themeStyle, value=null, createTime=1770633165384, updateTime=1770633165384, creator=18614031015, updator=18614031015)]), Website(id=1227687234338485094, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1227665162245664772, 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/xdyfyx/EN, language=EN, createTime=1770633045992, createBy=18614031015, updateTime=1770633115374, updateBy=18614031015, name=现代预防医学-英文, tplId=1146101810881728533, title=Modern Preventive Medicine, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1227687709129507332, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=articleTextType, value=kx, createTime=1770633159191, updateTime=1770633159191, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709108535809, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=banner, value=null, createTime=1770633159186, updateTime=1770633159186, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709167256071, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=grayFlag, value=0, createTime=1770633159200, updateTime=1770633159200, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709095952896, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=logo, value=https://castjournals.cast.org.cn/joweb/xdyfyx/EN/file/pic?fileId=/XB5plC0xuykmQnycvtyrw==, createTime=1770633159183, updateTime=1770633159183, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709179838985, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=minRunFlag, value=0, createTime=1770633159203, updateTime=1770633159203, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709121118723, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/xdyfyx/EN/file/pic, createTime=1770633159189, updateTime=1770633159189, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709171450376, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=silenceFlag, value=0, createTime=1770633159201, updateTime=1770633159201, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709112730114, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_en_623/, createTime=1770633159187, updateTime=1770633159187, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709133701637, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=themeColor, value=null, createTime=1770633159192, updateTime=1770633159192, creator=18614031015, updator=18614031015), WebsiteProps(id=1227687709154673158, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1227687234338485094, code=themeStyle, value=null, createTime=1770633159197, updateTime=1770633159197, creator=18614031015, updator=18614031015)])], journalTitle=现代预防医学, weixinUrl=null, journalUrl=http://xdyfyxzz.paperopen.com/, iacademicId=null, status=1, seqNo=null, journalTitleEn=Modern Preventive Medicine, journalPhotoCn=IeiuPXEZi6AA+k0VfvoiOQ==, journalPhotoEn=/9iTl8/ndms4tBz1fL28Pg==, journalFirstLetter=M, 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=, provinceCode=null, provinceName=null, collectFlag=false), detailUrlCn=https://castjournals.cast.org.cn/joweb/xdyfyx/CN/10.20043/j.cnki.MPM.202406227, detailUrlEn=https://castjournals.cast.org.cn/joweb/xdyfyx/EN/10.20043/j.cnki.MPM.202406227, pdfUrlCn=https://castjournals.cast.org.cn/joweb/xdyfyx/CN/PDF/10.20043/j.cnki.MPM.202406227, pdfUrlEn=https://castjournals.cast.org.cn/joweb/xdyfyx/EN/PDF/10.20043/j.cnki.MPM.202406227, aliStartDate=null, aliEndDate=null, collectionFlag=false, citedCount=null, citedUrl=null, reference=null)
收藏切换
QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋中45种抗生素残留量
收藏切换
PDF下载
郝春慧 , 崔伟 , 陈雨露 , 骆玲飞 , 李琰
现代预防医学 | 实验技术及其应用 2024,51(21): 3985-3991
收起
收藏切换
现代预防医学 | 实验技术及其应用 2024, 51(21): 3985-3991
QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋中45种抗生素残留量
全屏
郝春慧, 崔伟, 陈雨露, 骆玲飞, 李琰
作者信息
  • 上海市闵行区疾病预防控制中心理化检验科，上海 201101

    • 郝春慧（1987—），女，硕士，主管技师，研究方向:环境及食品卫生化学检验

通讯作者:

李琰，E-mail:
QuEChERS-UHPLC-MS/MS method for determining residues of 45 antibiotics in eggs
Chun-hui HAO, Wei CUI, Yu-lu CHEN, Ling-fei LUO, Yan LI
Affiliations
  • Department of Physical and Chemical Testing, Minhang District Center for Disease Control and Prevention, Shanghai 201101,China
出版时间: 2024-11-10 doi: 10.20043/j.cnki.MPM.202406227
文章导航
收藏切换
摘要
收起
目的

建立鸡蛋中45种抗生素残留量的QuEChERS-超高效液相色谱-串联质谱测定方法。

方法

样品经90%乙腈水溶液（含0.1%甲酸）提取后，取上清液至QuEChERS管（150 mg HLB-P + 50 mg PSA）净化，净化液氮吹至近干，10%甲醇水（含0.1%甲酸）定容。目标物经BEH C18柱（2.1×100 mm，1.7 μm）分离，以0.1%甲酸水-0.1%甲酸甲醇为流动相进行梯度洗脱，正离子多反应监测模式检测，基质匹配校准曲线法定量。

结果

在1.0～200 μg/L的范围内，45种目标分析物的回归方程均具有良好的线性关系。方法的检出限为1.0 μg/kg，加标回收率为69.2%～109.6%，RSD为1.2%～15.8%。

结论

该方法操作简单、快速，准确度和精密度均较高，适用于鸡蛋中45种抗生素的同时检测。

QuEChERS  /  超高效液相色谱-串联质谱法  /  抗生素  /  鸡蛋
Objective

To establish a QuEChERS-UHPLC-MS/MS method for the determination of residues of 45 antibiotics in eggs.

Methods

Samples were extracted using a 90% acetonitrile aqueous solution (containing 0.1% formic acid), and the supernatant was transferred to a QuEChERS tube (150 mg HLB-P + 50 mg PSA) for purification. The purified extract was concentrated to near dryness under nitrogen, and then reconstituted with 10% methanol aqueous solution (containing 0.1% formic acid). Target compounds were separated using a BEH C18 column (2.1×100 mm, 1.7 μm) with a gradient elution of 0.1% formic acid in water and 0.1% formic acid in methanol as the mobile phase. Detection was performed in positive ion multiple reaction monitoring mode, and quantification was achieved using matrix-matched calibration curves.

Results

Over the concentration range of 1.0 to 200 μg/L, all 45 target analytes exhibited good linear relationships in their regression equations. The method’s limit of detection was 1.0 μg/kg, with spiked recoveries ranging from 69.2% to 109.6% and relative standard deviations (RSD) between 1.2% and 15.8%.

Conclusion

This method is simple, rapid, and exhibits high accuracy and precision, making it suitable for the simultaneous detection of 45 antibiotics in eggs.

QuEChERS  /  UHPLC-MS/MS  /  Antibiotics  /  Eggs
郝春慧, 崔伟, 陈雨露, 骆玲飞, 李琰. QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋中45种抗生素残留量. 现代预防医学, 2024 , 51 (21) : 3985 -3991 . DOI: 10.20043/j.cnki.MPM.202406227
Chun-hui HAO, Wei CUI, Yu-lu CHEN, Ling-fei LUO, Yan LI. QuEChERS-UHPLC-MS/MS method for determining residues of 45 antibiotics in eggs[J]. Modern Preventive Medicine, 2024 , 51 (21) : 3985 -3991 . DOI: 10.20043/j.cnki.MPM.202406227
正文
收起
鸡蛋因富含蛋白质、微量元素及多种维生素等营养物质，而被称为人类“理想的营养库”[1]。我国鸡蛋产量及食用量均居于世界首位[1]。在实际生产过程中，现代化的高密度养殖使得蛋鸡很容易得病，大部分养殖场为防止鸡生病，会直接在鸡饲料中投放抗生素，或用药过程中不遵守处方和药物使用说明书，或使用未经批准的抗生素，滥用抗生素且不遵守休药期[1-5]。抗生素进入鸡体内，没有代谢掉的就会在其体内沉积，内脏、鸡肉、鸡蛋中都会有抗生素的残留[1-5]。人吃了含有抗生素的鸡蛋，可能会产生过敏反应、慢性毒性、破坏胃肠道菌群平衡等危害[1-6]。长时间食用含有抗生素的鸡蛋，会使人体免疫力降低，形成耐药抗药体质[1-6]。鸡蛋中抗生素残留量通常是微量的，而且可能会同时涉及较多品种的药物[1]。目前，我国对鸡蛋中的抗生素残留量的研究较少，各种标准仍在完善中，有些项目的研究还是空白[1]。因此，鸡蛋中多种类抗生素同时检测方法的开发刻不容缓。
目前，有很多鸡蛋中检出不同种类抗生素超过最大残留限量值的报道[1-9]。国内文献中检测方法大多只针对鸡蛋中某一类或少数几类抗生素[7-9]，国外文献中虽有多类别抗生素同时测定的方法[10-14]，但其检测灵敏度不高或样品前处理较为复杂。本研究拟比较QuEChERS和固相萃取两种前处理方式，采用液相色谱串联质谱仪同时测定鸡蛋中19种磺胺类、16种喹诺酮类、6种大环内酯类和4种四环素类共45种抗生素，为鸡蛋中抗生素的日常监测和突发应急事件的应对提供可靠的技术支持。
1　材料与方法
收起
1.1　主要仪器和试剂
1.1.1　仪器
LC-30AD超高效液相色谱仪（日本SHIMADZU）；QTRAP4500质谱仪（美国AB SCIEX）；Direct-Q 3超纯水仪器（美国Millipore）。
1.1.2　标准品和试剂
抗生素标准物质：19种磺胺类、16种喹诺酮类、8种大环内酯类标准溶液（100 μg/ml，溶剂为甲醇）、4种四环素类固体标准品（每种组分均为100 μg）均购自天津阿尔塔科技有限公司。甲醇（色谱纯，美国Supelco）；乙腈（色谱纯，美国Supelco）；甲酸（色谱纯，德国CNW）。QuEChERS净化管（15 ml，150 mg HLB-P + 50 mg PSA，上海速谱）。
1.2　标准溶液的配制
1.2.1　抗生素的混合标准溶液
4种四环素类固体标准品于使用前用1.00 ml水配制成100 μg/ml标准储备液，连同购买的100 μg/ml标准溶液，均在-20 ℃避光保存。取浓度为100 μg/ml的19种磺胺类、16种喹诺酮类、8种大环内酯类、4种四环素类标准溶液，用10%甲醇水（含0.1%甲酸）稀释成1 000 μg/L的45种抗生素的混合标准使用液，于-20℃避光保存。临用前，用10%甲醇水（含0.1%甲酸）配制成抗生素浓度为1.00、2.00、5.00、10.0、50.0、100和200 μg/L的抗生素混合标准系列。
1.2.2　基质混合标准工作溶液
取8份经提取和净化的空白试样，于40℃水浴氮气吹干，加入1.00 ml各浓度的标准系列溶液复溶，微孔滤膜过滤。基质混合标准系列应现用现配。
1.3　样品前处理
准确称取2.00 g样品于50 ml离心管中，加入10.0 ml 90%乙腈水溶液（含0.1%甲酸）振荡5 min，超声提取5 min，15 000 ×g 4 ℃离心5 min，取上清液待净化。将提取液全部转移至QuEChERS净化管（150 mg HLB-P + 50 mg PSA）中，涡旋混匀1 min，15 000 ×g 4℃离心5 min，取5.00 ml上清液，40℃水浴氮吹至近干，10%甲醇水（含0.1%甲酸）定容至1 ml，微孔滤膜过滤，待测。
1.4　仪器条件
1.4.1　色谱条件
ACQUITY UPLCBEH C18色谱柱（2.1×100 mm，1.7 μm，美国Waters）。流动相由0.1%甲酸水溶液（A）和0.1%甲酸甲醇溶液（B）组成。梯度洗脱程序：0～1.0 min，10% B；1.0～4.0 min，30%B；4.0～6.0 min，50% B；6.0～10.0 min，70% B；10.0～12.0 min，95% B；12.0～14.0 min，95%；14.0～15.0 min，10% B；15.0～18.0 min，10% B。流速为0.35 ml/min；进样体积：10 μl；自动进样器温度为15℃；色谱柱温度为40 ℃。
1.4.2　质谱条件
离子源：电喷雾离子源，正离子模式（ESI+）；扫描模式：多反应监测（MRM）；离子源电压：5 500 V；离子源温度：500 ℃；气帘气：35 psi；碰撞气：Medium；辅助加热气：50 psi。45种抗生素经质谱、色谱优化后的质谱采集参数见表1。
2　结果
收起
2.1　质谱条件的优化
将45种抗生素混合标准溶液用50%乙腈水溶液（含0.1%甲酸）稀释成200 μg/L，以针泵进样形式注入离子源，在ESI+模式下进行母离子扫描。45种待测抗生素的前体离子均以[M+H]+形式存在。在确定的母离子条件下再进行子离子扫描，选取响应值较高的子离子，建立离子对。在MRM模式下分别优化其锥孔电压和碰撞电压，完成质谱条件的建立。混标中同分异构体化合物的质谱参数，可通过配制独立的单标溶液来确认。母离子m/z为281.0的磺胺间甲氧嘧啶、磺胺甲氧哒嗪和磺胺对甲氧嘧啶以及母离子m/z为311.0的磺胺间二甲氧嘧啶和磺胺邻二甲氧嘧啶，母离子碰撞产生的子离子几乎完全一致，无法通过质谱参数来进行区分，只能通过待测物的色谱行为来确认。
2.2　色谱条件的优化
2.2.1　流动相的选择
考察流动相组成分别为0.1%甲酸水（A）+0.1%甲酸乙腈（B）及0.1%甲酸水（A）+0.1%甲酸甲醇（B）时的分离效果。流动相B为0.1%甲酸乙腈时，磺胺甲氧哒嗪与磺胺对甲氧嘧啶在同一时间出峰，无法实现色谱分离。流动相B为0.1%甲酸甲醇时，两组同分异构体（磺胺间甲氧嘧啶、磺胺甲氧哒嗪和磺胺对甲氧嘧啶以及磺胺间二甲氧嘧啶和磺胺邻二甲氧嘧啶）均能实现有效的色谱分离。因此用0.1%甲酸水（A）+0.1%甲酸甲醇（B）作为流动相，梯度洗脱程序下在18 min内可以有效分离45种抗生素。
2.2.2　色谱柱的选择
观察ACQUITY UPLC ®BEH C18色谱柱（2.1×100 mm，1.7 μm，美国Waters）及ACQUITY UPLC ®HSS T3色谱柱（2.1×100 mm，1.8 μm，美国Waters）的分离效果，45种抗生素均能实现有效分离，但大部分待测物在BEH C18柱上的质谱响应值更高，且出峰时间更早，故本实验拟采用BEH C18色谱柱。各抗生素的MRM总离子流图见图1，图中峰编号与表1中化合物编号一致。
2.3　基质效应的评价
采用基质提取后添加法进行基质效应的考察，根据公式：基质效应（ME）=（样品基质提取后加标峰面积-样品提取后基质峰面积）/同等加标浓度的标准溶液峰面积，采用100 μg/kg添加水平进行基质效应评价，45种待测抗生素的ME值在0.42～3.20之间。其中有28种抗生素ME值小于0.8，存在强基质抑制效应；有8种抗生素ME值大于1.2，存在强基质增强效应；仅有9种抗生素ME值在0.8～1.2，为一般基质效应。目前常采用样品稀释、基质匹配校正、同位素内标校正等方法来降低基质效应。由于45种抗生素的同位素内标制作成本高，不易获得，因此采用基质匹配校准曲线法来定量，即用不含抗生素的鸡蛋基质提取物来配制校准曲线。
2.4　前处理条件的优化
2.4.1　提取溶剂的选择
考察提取溶剂乙腈水溶液（含0.1%甲酸）中乙腈比例分别为10%、30%、50%、70%、90%对抗生素添加水平为100 μg/kg时回收率的影响。结果显示，随着提取溶液中乙腈比例的增加，各待测物的回收率有显著的提升，乙腈比例为90%时各待测抗生素的回收效果最好，在54.3%～109.6%之间。因此，采用90%乙腈水溶液（含0.1%甲酸）来提取蛋液，待净化分析。
2.4.2　净化方式的选择
比较QuEChERS（150 mg HLB-P + 50 mg PSA）和固相萃取（HLB-P填料）两种净化方式对抗生素添加水平为100 μg/kg时回收率的影响。QuEChERS净化后的回收率在54.3%～109.6%之间，SPE净化后的回收率在31.6%～109.4%之间。磺胺二甲基异噁唑、金霉素、磺胺间二甲氧嘧啶、磺胺喹恶啉、替米考星、泰乐菌素、克拉霉素、阿奇霉素和罗红霉素共9种抗生素用QuEChERS净化后的回收率比SPE净化高出20%以上，故采用QuEChERS处理方法净化样品。
2.5　方法验证
2.5.1　校准曲线和检出限
本法采用基质匹配校准曲线法，四大类共45种抗生素的线性范围、相关系数见表2。线性范围为1.0～200 μg/L，相关系数均大于0.995。称取11份无抗鸡蛋加标后制成各待测组分浓度为2 μg/kg抗生素加标样，经样品前处理后本法分析。检出限的计算公式为MDL = S×t(n-1,0.01)，其中S表示标准偏差，n值为11，t(n-1,0.01)代表显著性水平为0.01（单侧）且自由度为10时的t值。查询t界值表，单侧t0.01,10=2.76。经计算，45种抗生素的检出限在0.1～0.7范围内，均低于1.0 μg/kg，故用本方法测定45种抗生素的检出限统一为1.0 μg/kg。
2.5.2　精密度和准确度
以无抗鸡蛋为本底，进行加标回收及精密度试验，分别添加低（2 μg/kg）、中（10 μg/kg）、高（100 μg/kg）三个浓度水平，各添加水平平行测定7次，计算平均回收率和相对标准偏差（RSD），结果见表2。四大类共45种抗生素的平均回收率为69.2%～109.6%，相对标准差为1.2%～15.8%。
2.6　实际样本的检测
采用该方法对在上海市某区大型商超和农贸市场采购的36份鸡蛋样品进行检测，共8份样品有不同种类的抗生素检出，检出率为22.2%，涉及的指标为环丙沙星、恩诺沙星、甲氧苄啶和多西环素，检出率分别为11.1%、16.7%、2.8%、11.1%。GB 31650.1—2022《食品安全国家标准食品中41种兽药最大残留限量》规定恩诺沙星、甲氧苄啶、多西环素在禽蛋中的最大残留限量均为10 μg/kg，其中恩诺沙星是以恩诺沙星与环丙沙星之和参与评价[15]。有3份样品抗生素含量超标，超标率为8.3%，其中恩诺沙星超标率为8.3%（含量水平为20.4、57.5和275 μg/kg）、甲氧苄啶超标率为2.8%（含量水平为14.3 μg/kg）。
3　讨论
收起
在质谱条件优化过程中，发现磺胺类化合物因其结构中特异的桥键部分（-SO2-）断裂所致，其典型特征碎片离子为m/z 92、m/z 108和m/z 156[6]。抗生素的稳定性与稀释溶剂关系很大，四环素类抗生素在水溶液中稳定性明显优于甲醇，因此本方法用纯水来配制四环素类标准溶液[6]。在摸索质谱参数时用50%乙腈水溶液稀释抗生素标准物质，用10%甲醇水（含0.1%甲酸）稀释混合标准溶液，可减少甲醇对抗生素稳定性的影响[6]。在流动相中添加0.1%甲酸作为改进剂，可以提高待测物在ESI+模式下的灵敏度，而在水相和有机相中均加入0.1%甲酸，可以避免梯度洗脱时甲酸比例的改变所造成的影响[6]。
在样品前处理条件优化过程中，发现随着提取溶液中乙腈比例的增加，待测抗生素的回收率均有显著的提高，可能与有机溶剂能促进蛋白质分子的聚集和沉淀有关。乙腈可与水互溶，在溶解于水的同时从蛋白质分子周围的水化层中夺走水分子，破坏蛋白质分子的水膜，而发生沉淀现象。QuEChERS比SPE净化效果更好，可能与鸡蛋蛋白质含量高易导致萃取小柱堵塞，从而影响回收率有关[7]。
本研究通过优化仪器参数和前处理条件，建立了QuEChERS-超高效液相色谱-串联质谱法同时测定鸡蛋中45种抗生素的检测方法。方法前处理操作简单、耗材少、重复性高、灵敏度高、准确度好，可满足常规实验室快速大批量测定禽蛋中抗生素的需求。
文献
收起
参考文献 引证文献
排序方式：
[1]
张萍.鸡蛋中抗生素类药物残留的研究进展[J].北方药学，2015，12（4）：90-91, 92.
Zhang P. Research progress on antibiotic residues in eggs[J]. Journal of North Pharmacy, 2015, 12(4): 90-91, 92.(In Chinese)
[2]
侯学文，邢燕，高慧，等.山东省市售鸡蛋中抗生素残留及暴露风险评估[J].预防医学论坛，2023，29（9）：651-655.
Hou XW, Xing Y, Gao H, et al. Risk assessment on antibiotic residues and exposure in commercially available eggs in Shandong province[J].Preventive Medicine Tribune, 2023, 29(9): 651-655.(In Chinese)
[3]
刘孟文，杨欢欢，赵一鹏，等.陕西省329份市售鸡肉和鸡蛋中四环素类抗生素残留调查[J].现代预防医学，2019，46（17）：3131-3133.
Liu MW, Yang HH, Zhao YP, et al. Residues of tetracycline antibiotics in 329 chicken and eggs on market, Shaanxi[J]. Modern Preventive Medicine,2019, 46(17): 3131-3133.(In Chinese)
[4]
肖永华，革丽亚，粱高道，等.湖北省鸡肉和鸡蛋中多组分抗生素残留分析[J].中国食品卫生杂志，2022，34（2）：292-296.
Xiao YH, Ge LY, Liang GD, et al. Occurrence of multi-antibiotics in chicken and egg samples in Hubei[J]. Chinese Journal of Food Hygiene,2022, 34(2): 292-296.(In Chinese)
[5]
王姝婷，黄希汇，刘少颖，等.市售鸡肉与鸡蛋中四环素类抗生素残留调查与膳食暴露风险评估[J].中国食品卫生杂志，2023，35（7）：1063-1066.
Wang ST, Huang XH, Liu SY, et al. Investigation and dietary exposure risk assessment of tetracycline antibiotics residues in eggs and chicken sold on the market[J]. Chinese Journal of Food Hygiene, 2023, 35(7): 1063-1066.(In Chinese)
[6]
郝春慧，崔伟，骆玲飞，等.水中52种抗生素全自动固相萃取-超高效液相色谱-串联质谱法测定[J].中国公共卫生，2024，40（3）：382-388.
Hao CH, Cui W, Luo LF, et al. Determination of 52 antibiotics in water through a fully automated solid-phase extraction-ultra-high performance liquid chromatography-tandem mass spectrometry system[J]. Chinese Journal of Public Health, 2024, 40(3): 382-388.(In Chinese)
[7]
王敏娟，胡佳薇，田丽，等.超高效液相色谱-串联质谱法同时测定鸡蛋中21种喹诺酮及四环素类抗生素残留[J].中国卫生检验杂志，2017，27（4）：473-476.
Wang MJ, Hu JW, Tian L, et al. Simultaneous determination of quinoline and tetracycline residues in eggs by ultra performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Health Laboratory Technology, 2017, 27(4): 473-476.(In Chinese)
[8]
李磊，周贻兵，张权，等.QuEChERS净化超高效液相色谱-串联质谱法快速测定鸡蛋中13种喹诺酮类抗生素[J].现代预防医学，2018，45（24）：4482-4486, 4490.
Li L, Zhou YB, Zhang Q, et al. Rapid determination of 13 quinolones antibiotics in eggs by QuEChERS purification combined with ultra-high-performance liquid chromatography-tandem mass spectrometry[J]. Modern Preventive Medicine, 2018, 45(24): 4482-4486, 4490.(In Chinese)
[9]
廖艳华，周劭桓，林文斯，等.超高效液相色谱-串联质谱法测定鸡蛋中11种喹诺酮类抗生素残留的样品前处理方法优化[J].中国卫生检验杂志，2018，28（8）：910-914, 921.
Liao YH, Zhou SH, Lin WS, et al. Optimization of sample pretreatment method for determination of 11 quinolone antibiotic residues in eggs by UPLC-MS/MS[J]. Chinese Journal of Health Laboratory Technology, 2018,28(8): 910-914, 921.(In Chinese)
[10]
Paoletti F, Sdogati S, Barola C, et al. Development and validation of a multiclass confirmatory method for the determination of over 60 antibiotics in eggs using liquid-chromatography high-resolution mass spectrometry[J]. Food Control, 2021, 127: 108109.
[11]
Zhou J, Xu JJ, Cong JM, et al. Optimization for quick, easy, cheap,effective, rugged and safe extraction of mycotoxins and veterinary drugs by response surface methodology for application to egg and milk[J]. Journal of Chromatography a, 2018, 1532: 20-29.
[12]
Yang Y, Li X, Lin J, et al. A modified QuEChERS-based UPLC-MS/MS method for rapid determination of multiple antibiotics and sedative residues in freshwater fish[J]. Food Chemistry: X, 2024, 22:101268.
[13]
Gajda A,Nowacka-Kozak E,Gbylik-Sikorska M,et al. Multi-residues UHPLC–MS/MS analysis of 53 antibacterial compounds in poultry feathers as an analytical tool in food safety assurance[J].Journal of Chromatography B, 2019, 1104: 182-189.
[14]
Moretti S, Dusi G, Giusepponi D, et al. Screening and confirmatory method for multiclass determination of 62 antibiotics in meat[J].Journal of Chromatography a, 2016, 1429: 175-188.
[15]
国家市场监督管理总局.GB 31650.1-2022 食品安全国家标准-食品中41种兽药最大残留限量[S].北京：中国农业出版社，2022.
State Administration for Market Regulation. GB 31650.1-2022 National food safety standard - Maximum residue limits for 41 veterinary drugs in foods[S]. Beijing: China Agriculture Press, 2022.
2024年第51卷第21期
PDF下载
89
42
引用本文
BibTeX
文章信息
doi: 10.20043/j.cnki.MPM.202406227
  • 接收时间：2024-06-18
  • 首发时间：2026-03-20
  • 出版时间：2024-11-10
补充材料
相关文章
文章信息
作者
出版历史
  • 收稿日期：2024-06-18
基金
作者信息
    上海市闵行区疾病预防控制中心理化检验科，上海 201101

通讯作者:

李琰，E-mail:
参考文献
分享链接
https://castjournals.cast.org.cn/joweb/xdyfyx/CN/10.20043/j.cnki.MPM.202406227
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