首页 期刊 论文 学科刊群 资讯 加盟 关于
EN
image
Article(id=1218290945410388690, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1218290941232861879, articleNumber=1001-2494(2024)15-1438-07, orderNo=null, doi=10.11669/cpj.2024.15.011, pmid=null, cstr=null, oa=null, hot=null, price=null, onlineType=0, articleFormat=0, articleType=null, articleTypeStr=research-article, receivedDate=1703174400000, receivedDateStr=2023-12-22, revisedDate=null, revisedDateStr=null, acceptedDate=null, acceptedDateStr=null, onlineDate=1768392796137, onlineDateStr=2026-01-14, pubDate=1723046400000, pubDateStr=2024-08-08, doiRegisterDate=null, doiRegisterDateStr=null, onlineIssueDate=1768392796137, onlineIssueDateStr=2026-01-14, onlineJustAcceptDate=null, onlineJustAcceptDateStr=null, onlineFirstDate=null, onlineFirstDateStr=null, sourceXml=null, magXml=null, createTime=1768392796137, creator=13701087609, updateTime=1768392796137, updator=13701087609, issue=Issue{id=1218290941232861879, tenantId=1146029695717560320, journalId=1190317699101192196, year='2024', volume='59', issue='15', pageStart='1361', pageEnd='1452', issueExtLink='null', onlineDate='null', pubDate='null', beforeIssueId=null, nextIssueId=null, price=null, status=1, issueComplete=1, articleOrder=1, issueType=-1, specialIssue=null, createTime=1768392795141, creator=13701087609, updateTime=1768394622953, updator=13701087609, preIssue=null, nextIssue=null, ext={EN=IssueExt(id=1218298607682376061, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1218290941232861879, language=EN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=), CN=IssueExt(id=1218298607682376062, tenantId=1146029695717560320, journalId=1190317699101192196, issueId=1218290941232861879, language=CN, specialIssueTitle=, coverIllustrator=null, specialIssueEditor=, specialIssueAbout=)}, issueFiles=null}, startPage=1438, endPage=1444, ext={EN=ArticleExt(id=1218290945645269725, articleId=1218290945410388690, tenantId=1146029695717560320, journalId=1190317699101192196, language=EN, title=Rapid Detection of Eight Aminoglycoside Antibiotics by Liquid Chromatography-Tandem Mass Spectrometry, columnId=null, journalTitle=Chinese Pharmaceutical Journal, columnName=null, runingTitle=null, highlight=null, articleAbstract=

OBJECTIVE To establish a method for simultaneous determination of 8 aminoglycoside antibiotics (AGs) including kanamycin, gentamycin C1, gentamycin C2, gentamycin C1a, tobramycin, neomycin, isepamicin and etimicin by LC-MS/MS with instant library searching. METHODS Eight AGs were separated by Shiseido PC HILIC (2.0 mm×100 mm, 3 μm) column, with 0.5% formic acid aqueous solution-0.1% formic acid acetonitrile solution as mobile phase and 0.4 mL·min-1 of flow rate,and procedure of the gradient elution was performed. The screening method of 8 AGs was established by the scanning mode of multiple reaction monitoring (MRM). Typical mass spectrograms of 8 AGs were collected by collision energy expansion (CES) function and enhanced ion (EPI) scanning mode, and added them to the already established mass spectralibrary of antibiotics searching. RESULTS The established method has the advantages of short analysis time, strong specificity and high sensitivity. The screening and qualitative analysis of 8 AGs can be realized within 10 min. Three batches of the INSA insulin product were detected by this method, and kanamycin that was less than the detection limit of 0.05 ng·mg-1 were not detected in above samples. CONCLUSION In this study, the detection method of 8 AGs established by LC-MS/MS with instant library searching can quickly screen and accurately determine trace AGs.

, correspAuthors=Ying LIU, 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=Xiaolong SUN, Qing YANG, Hongbo WANG, Ying LIU), CN=ArticleExt(id=1218290948409316136, articleId=1218290945410388690, tenantId=1146029695717560320, journalId=1190317699101192196, language=CN, title=基于LC-MS/MS法建立快速检测8种氨基糖苷类抗生素的方法, columnId=1190352405612040510, journalTitle=中国药学杂志, columnName=论著, runingTitle=null, highlight=null, articleAbstract=

目的 应用液质谱联用(LC-MS/MS)检索数据库技术建立卡那霉素、庆大霉素C1、庆大霉素C1a、庆大霉素C2、妥布霉素、新霉素、异帕米星、依替米星8种氨基糖苷类抗生素(aminoglycoside antibiotics,AGs)的快速检测方法。方法 采用Shiseido PC HILIC(2.0 mm×100 mm,3 μm)色谱柱对8种AGs进行分离,体积分数0.5%甲酸水溶液-0.1%甲酸乙腈溶液为流动相,梯度洗脱,流速为0.4 mL·min-1;采用多重反应监测(MRM)扫描建立8种AGs的筛查方法;采用碰撞能量扩展(CES)功能和增强子离子(EPI)扫描模式采集8种AGs的典型质谱图,添加到已经建立的抗生素检索质谱库中。结果 所建立的方法专属性强,灵敏度高,10 min即可实现对8种AGs的初筛和定性分析。应用该方法对3批INSA胰岛素产品中的卡那霉素残留进行了监测,3批样品中均未检测到卡那霉素,其残留量小于检出限0.05 ng·mg-1。结论 本研究应用液质联用检索数据库技术建立的8种AGs的检测方法可以对痕量AGs进行快速筛查和准确定性。

, correspAuthors=刘颖, authorNote=null, correspAuthorsNote=
* 刘颖,女,博士,研究员 研究方向:药物分析与药物质量控制Tel:(010)67872233-8312
, copyrightStatement=null, copyrightOwner=null, extLink=null, articleAbsUrl=null, sourceXml=N4JK7o2PwWfzt+0iAVAMUQ==, magXml=K7gr/AwNKo7uoi1xHS/O1Q==, pdfUrl=null, pdf=N541g+zIJazezD6oz8s/+g==, pdfFileSize=1886602, pdfExtLink=null, richHtmlUrl=null, mobilePdfUrl=null, reviewReport=null, pdfFirstPage=null, abstractGraph=pK/Wlm53Rr7dW+8PZae6SA==, abstractGraphContent=null, abstractVideo=null, citation=null, cebUrl=null, magXmlContent=t/li2uFXXQnY1OH1M1Hqog==, mapNumber=null, authorCompany=null, fund=null, authors=

孙晓龙与杨青为共同第一作者

孙晓龙,男,硕士研究生 研究方向:药物分析与药物质量控制;

杨青,女,硕士 研究方向:药物分析与药物质量控制。

, authorsList=孙晓龙, 杨青, 王洪波, 刘颖)}, authors=[Author(id=1218484891277247149, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, 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=1218484891356938932, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484891277247149, language=EN, stringName=Xiaolong SUN, firstName=Xiaolong, middleName=null, lastName=SUN, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1 National Institutes for Food and Drug Control, Beijing 100050, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1218484891432436407, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484891277247149, language=CN, stringName=孙晓龙, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, address=1 中国食品药品检定研究院, 北京 100050, bio={"content":"

孙晓龙,男,硕士研究生 研究方向:药物分析与药物质量控制;

"}, bioImg=null, bioContent=

孙晓龙,男,硕士研究生 研究方向:药物分析与药物质量控制;

, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1218484891025588889, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, xref=1, ext=[AuthorCompanyExt(id=1218484891033977499, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891025588889, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 National Institutes for Food and Drug Control, Beijing 100050, China), AuthorCompanyExt(id=1218484891042366109, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891025588889, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 中国食品药品检定研究院, 北京 100050)])]), Author(id=1218484891621180095, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, 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=1218484891717649095, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484891621180095, language=EN, stringName=Qing YANG, firstName=Qing, middleName=null, lastName=YANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=2, address=2 Shouyao Holdings (Beijing) Co., Ltd, Beijing 100195, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1218484891788952268, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484891621180095, language=CN, stringName=杨青, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=2, address=2 首药控股(北京)股份有限公司, 北京100195, bio={"content":"

杨青,女,硕士 研究方向:药物分析与药物质量控制。

"}, bioImg=null, bioContent=

杨青,女,硕士 研究方向:药物分析与药物质量控制。

, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1218484891109474978, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, xref=2, ext=[AuthorCompanyExt(id=1218484891117863587, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891109474978, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 Shouyao Holdings (Beijing) Co., Ltd, Beijing 100195, China), AuthorCompanyExt(id=1218484891130446500, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891109474978, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 首药控股(北京)股份有限公司, 北京100195)])]), Author(id=1218484891877032661, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, 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=1218484891965113053, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484891877032661, language=EN, stringName=Hongbo WANG, firstName=Hongbo, middleName=null, lastName=WANG, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=3, address=3 School of Pharmacy, Yantai University, Yantai 264003, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1218484892057387743, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484891877032661, language=CN, stringName=王洪波, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=3, address=3 烟台大学药学院, 山东 烟台 264003, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1218484891189166758, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, xref=3, ext=[AuthorCompanyExt(id=1218484891197555368, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891189166758, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 School of Pharmacy, Yantai University, Yantai 264003, China), AuthorCompanyExt(id=1218484891214332585, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891189166758, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 烟台大学药学院, 山东 烟台 264003)])]), Author(id=1218484892179022566, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, 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=1, authorType=1, ext={EN=AuthorExt(id=1218484892338406128, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484892179022566, language=EN, stringName=Ying LIU, firstName=Ying, middleName=null, lastName=LIU, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, *, address=1 National Institutes for Food and Drug Control, Beijing 100050, China, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null), CN=AuthorExt(id=1218484892468429557, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, authorId=1218484892179022566, language=CN, stringName=刘颖, firstName=null, middleName=null, lastName=null, prefix=null, suffix=null, authorComment=null, nameInitials=null, affiliation=null, department=null, xref=1, *, address=1 中国食品药品检定研究院, 北京 100050, bio=null, bioImg=null, bioContent=null, aboutCorrespAuthor=null)}, companyList=[AuthorCompany(id=1218484891025588889, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, xref=1, ext=[AuthorCompanyExt(id=1218484891033977499, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891025588889, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 National Institutes for Food and Drug Control, Beijing 100050, China), AuthorCompanyExt(id=1218484891042366109, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891025588889, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 中国食品药品检定研究院, 北京 100050)])])], keywords=[Keyword(id=1218484892673950470, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, orderNo=1, keyword=aminoglycoside antibiotics), Keyword(id=1218484892762030856, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, orderNo=2, keyword=liquid chromatography-tandem mass spectrometry (LC-MS/MS)), Keyword(id=1218484892841722637, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, orderNo=3, keyword=hydrophilic interaction chromatography (HILIC)), Keyword(id=1218484892917220113, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, orderNo=4, keyword=instant library searching), Keyword(id=1218484893001106199, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, orderNo=5, keyword=quantitative analysis), Keyword(id=1218484893089186593, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, orderNo=6, keyword=qualitative analysis), Keyword(id=1218484893227598629, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, orderNo=1, keyword=氨基糖苷类抗生素), Keyword(id=1218484893315679019, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, orderNo=2, keyword=液相色谱-串联质谱法), Keyword(id=1218484893399565102, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, orderNo=3, keyword=亲水相互作用色谱), Keyword(id=1218484893491839797, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, orderNo=4, keyword=检索数据库), Keyword(id=1218484893567337274, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, orderNo=5, keyword=定性分析), Keyword(id=1218484893647029054, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, orderNo=6, keyword=定量分析)], refs=[Reference(id=1218484895769346982, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=1944, volume=55, issue=1, pageStart=66, pageEnd=69, url=null, language=null, rfNumber=[1], rfOrder=0, authorNames=SCHATZ A, BUGLE E, WAKSMAN S A, journalName=Proc Soc Exp Biol Med, refType=null, unstructuredReference=SCHATZ A, BUGLE E, WAKSMAN S A. Streptomycin, a substance exhibiting antibiotic activity against gram-positive and gram-negative bacteria[J]. Proc Soc Exp Biol Med, 1944, 55(1): 66-69., articleTitle=Streptomycin, a substance exhibiting antibiotic activity against gram-positive and gram-negative bacteria, refAbstract=null), Reference(id=1218484895865815978, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2019, volume=44, issue=11, pageStart=1275, pageEnd=1282, url=null, language=null, rfNumber=[2], rfOrder=1, authorNames=WU J H, LIU P Y, journalName=中国抗生素杂志, refType=null, unstructuredReference=WU J H, LIU P Y. The past and present of aminoglycoside antibiotics[J]. Chin J Antibiot(中国抗生素杂志), 2019, 44(11):1275-1282., articleTitle=The past and present of aminoglycoside antibiotics, refAbstract=null), Reference(id=1218484895937119151, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2022, volume=30, issue=5, pageStart=441, pageEnd=446, url=null, language=null, rfNumber=[3], rfOrder=2, authorNames=MENG F, ZHOU X H, YUAN Y Z, journalName=药学与临床研究, refType=null, unstructuredReference=MENG F, ZHOU X H, YUAN Y Z. Development of detection technologies for aminoglycoside antibiotics[J]. Pharm Clin Res(药学与临床研究), 2022, 30(5):441-446., articleTitle=Development of detection technologies for aminoglycoside antibiotics, refAbstract=null), Reference(id=1218484896050365365, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2017, volume=38, issue=4, pageStart=179, pageEnd=183, url=null, language=null, rfNumber=[4], rfOrder=3, authorNames=XU C X, GU C L, FANG Y, journalName=国外医药抗生素分册, refType=null, unstructuredReference=XU C X, GU C L, FANG Y, et al. Application of antibiotics and the methods for their determination in biological products[J]. World Notes Antibiot(国外医药抗生素分册), 2017, 38(4):179-183,189., articleTitle=Application of antibiotics and the methods for their determination in biological products, refAbstract=null), Reference(id=1218484896163611579, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2010, volume=38, issue=3, pageStart=28, pageEnd=31, url=null, language=null, rfNumber=[5], rfOrder=4, authorNames=YANG X, ZENG X W, LIU Y, journalName=微生物学免疫学进展, refType=null, unstructuredReference=YANG X, ZENG X W, LIU Y, et al. Detection of the residual content of kanamycin and gentamicin in live attenuated japanese encephalitis vaccine with ELISA method[J]. Prog Microbiol Immunol(微生物学免疫学进展), 2010, 38(3):28-31., articleTitle=Detection of the residual content of kanamycin and gentamicin in live attenuated japanese encephalitis vaccine with ELISA method, refAbstract=null), Reference(id=1218484896230720448, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2022, volume=39, issue=2, pageStart=113, pageEnd=118, url=null, language=null, rfNumber=[6], rfOrder=5, authorNames=YANG Q, TIAN Y, JIANG Z Q, journalName=中国药物评价, refType=null, unstructuredReference=YANG Q, TIAN Y, JIANG Z Q, et al. Application of liquid-mass spectrometry in antibiotic analysis[J]. Chin J Drug Eval(中国药物评价), 2022, 39(2):113-118., articleTitle=Application of liquid-mass spectrometry in antibiotic analysis, refAbstract=null), Reference(id=1218484896314606531, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2018, volume=41, issue=5, pageStart=1138, pageEnd=1148, url=null, language=null, rfNumber=[7], rfOrder=6, authorNames=SONG X, ZHOU T, LI J, journalName=J Sep Sci, refType=null, unstructuredReference=SONG X, ZHOU T, LI J, et al. Determination of macrolide antibiotics residues in pork using molecularly imprinted dispersive solid‐phase extraction coupled with LC-MS/MS[J]. J Sep Sci, 2018, 41(5): 1138-1148., articleTitle=Determination of macrolide antibiotics residues in pork using molecularly imprinted dispersive solid‐phase extraction coupled with LC-MS/MS, refAbstract=null), Reference(id=1218484896406881225, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2020, volume=10, issue=3, pageStart=356, pageEnd=null, url=null, language=null, rfNumber=[8], rfOrder=7, authorNames=DO T C M V, NGUYEN D Q, NGUYEN T D, journalName=Catalysts, refType=null, unstructuredReference=DO T C M V, NGUYEN D Q, NGUYEN T D, et al. Development and validation of a LC-MS/MS method for determination of multi-class antibiotic residues in aquaculture and river waters, and photocatalytic degradation of antibiotics by TiO2 nanomaterials[J]. Catalysts, 2020, 10(3): 356., articleTitle=Development and validation of a LC-MS/MS method for determination of multi-class antibiotic residues in aquaculture and river waters, and photocatalytic degradation of antibiotics by TiO2 nanomaterials, refAbstract=null), Reference(id=1218484896490767307, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2022, volume=11, issue=7, pageStart=845, pageEnd=null, url=null, language=null, rfNumber=[9], rfOrder=8, authorNames=CHAN C L, WAI H K F, WU P, journalName=Antibiotics, refType=null, unstructuredReference=CHAN C L, WAI H K F, WU P, et al. A universal LC-MS/MS method for simultaneous detection of antibiotic residues in animal and environmental samples[J]. Antibiotics, 2022, 11(7): 845. DOI: 10.3390/antibiotics11070845., articleTitle=A universal LC-MS/MS method for simultaneous detection of antibiotic residues in animal and environmental samples, refAbstract=null), Reference(id=1218484896604013520, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2018, volume=558, issue=null, pageStart=28, pageEnd=34, url=null, language=null, rfNumber=[10], rfOrder=9, authorNames=LIU Y, ZHANG J, HU C, journalName=Anal Biochem, refType=null, unstructuredReference=LIU Y, ZHANG J, HU C. Validated LC-MS/MS method for simultaneous analysis of 21 cephalosporins in zebrafish for a drug toxicity study[J]. Anal Biochem, 2018, 558: 28-34., articleTitle=Validated LC-MS/MS method for simultaneous analysis of 21 cephalosporins in zebrafish for a drug toxicity study, refAbstract=null), Reference(id=1218484896679510993, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2021, volume=631, issue=null, pageStart=114299, pageEnd=null, url=null, language=null, rfNumber=[11], rfOrder=10, authorNames=YANG Q, LIU Y, JIANG Z, journalName=Anal Biochem, refType=null, unstructuredReference=YANG Q, LIU Y, JIANG Z, et al. Multi-residue method for the detection of 40 β-lactam-antibiotics in vaccines by LC-MS/MS[J]. Anal Biochem, 2021, 631: 114299. DOI: 10.1016/j.ab.2021.114299., articleTitle=Multi-residue method for the detection of 40 β-lactam-antibiotics in vaccines by LC-MS/MS, refAbstract=null), Reference(id=1218484896767591383, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2017, volume=41, issue=5, pageStart=431, pageEnd=440, url=null, language=null, rfNumber=[12], rfOrder=11, authorNames=LIU Y, UBOH C E, LI X, journalName=J Anal Toxicol, refType=null, unstructuredReference=LIU Y, UBOH C E, LI X, et al. Validated LC-MS-MS method for simultaneous analysis of 17 barbiturates in horse plasma for doping control[J]. J Anal Toxicol, 2017, 41(5): 431-440., articleTitle=Validated LC-MS-MS method for simultaneous analysis of 17 barbiturates in horse plasma for doping control, refAbstract=null), Reference(id=1218484896847283162, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2018, volume=null, issue=null, pageStart=null, pageEnd=null, url=https://www.nist.gov/srd/refprop, language=null, rfNumber=[13], rfOrder=12, authorNames=LEMMON E W, HUBER M L, MCLINDEN M O, journalName=null, refType=null, unstructuredReference=LEMMON E W, HUBER M L, MCLINDEN M O. NIST standard reference database 23: reference fluid thermodynamic and transport properties-REFPROP, version 10.0[EB/OL]. Gaithersburg, MD: National Institute of Standards and Technology (NIST), 2018 (2023-11-04) [2023-12-12]. https://www.nist.gov/srd/refprop., articleTitle=NIST standard reference database 23: reference fluid thermodynamic and transport properties-REFPROP, version 10.0, refAbstract=null), Reference(id=1218484896926974945, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2011, volume=4, issue=1, pageStart=35, pageEnd=44, url=null, language=null, rfNumber=[14], rfOrder=13, authorNames=SAITO T, KINUGASA S, journalName=Synthesiol Eng Ed, refType=null, unstructuredReference=SAITO T, KINUGASA S. Development and release of a spectral database for organic compounds-key to the continual services and success of a large-scale database[J]. Synthesiol Eng Ed, 2011, 4(1): 35-44., articleTitle=Development and release of a spectral database for organic compounds-key to the continual services and success of a large-scale database, refAbstract=null), Reference(id=1218484897044415460, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2018, volume=101, issue=4, pageStart=1156, pageEnd=1182, url=null, language=null, rfNumber=[15], rfOrder=14, authorNames=PANG G F, FAN C L, CHANG Q Y, journalName=J AOAC Int, refType=null, unstructuredReference=PANG G F, FAN C L, CHANG Q Y, et al. Screening of 485 pesticide residues in fruits and vegetables by liquid chromatography-quadrupole-time-of-flight mass spectrometry based on TOF accurate mass database and QTOF spectrum library[J]. J AOAC Int, 2018, 101(4): 1156-1182., articleTitle=Screening of 485 pesticide residues in fruits and vegetables by liquid chromatography-quadrupole-time-of-flight mass spectrometry based on TOF accurate mass database and QTOF spectrum library, refAbstract=null), Reference(id=1218484897161855977, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2011, volume=83, issue=17, pageStart=6834, pageEnd=6841, url=null, language=null, rfNumber=[16], rfOrder=15, authorNames=LIU Y, UBOH C E, SOMA L R, journalName=Anal Chem, refType=null, unstructuredReference=LIU Y, UBOH C E, SOMA L R, et al. Efficient use of retention time for the analysis of 302 drugs in equine plasma by liquid chromatography-MS/MS with scheduled multiple reaction monitoring and instant library searching for doping control[J]. Anal Chem, 2011, 83(17): 6834-6841., articleTitle=Efficient use of retention time for the analysis of 302 drugs in equine plasma by liquid chromatography-MS/MS with scheduled multiple reaction monitoring and instant library searching for doping control, refAbstract=null), Reference(id=1218484897275102189, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2013, volume=41, issue=7, pageStart=979, pageEnd=985, url=null, language=null, rfNumber=[17], rfOrder=16, authorNames=ZHAO-YONG L, JUN-HUI C, XIN L, journalName=Fresenius J Anal Chem, refType=null, unstructuredReference=ZHAO-YONG L, JUN-HUI C, XIN L, et al. Rapid screening and identification of paralytic shellfish poisoning toxins in red tide algae using hydrophilic interaction liquid chromatography-high resolution mass spectrometry with an accurate-mass database[J]. Fresenius J Anal Chem, 2013, 41(7): 979-985., articleTitle=Rapid screening and identification of paralytic shellfish poisoning toxins in red tide algae using hydrophilic interaction liquid chromatography-high resolution mass spectrometry with an accurate-mass database, refAbstract=null), Reference(id=1218484897388348401, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2021, volume=17, issue=3, pageStart=316, pageEnd=345, url=null, language=null, rfNumber=[18], rfOrder=17, authorNames=ERKMEN C, GEBREHIWOT W H, USLU B, journalName=Curr Pharm Anal, refType=null, unstructuredReference=ERKMEN C, GEBREHIWOT W H, USLU B. Hydrophilic interaction liquid chromatography (HILIC): latest applications in the pharmaceutical researches[J]. Curr Pharm Anal, 2021, 17(3): 316-345., articleTitle=Hydrophilic interaction liquid chromatography (HILIC): latest applications in the pharmaceutical researches, refAbstract=null), Reference(id=1218484897480623095, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2017, volume=40, issue=1, pageStart=49, pageEnd=80, url=null, language=null, rfNumber=[19], rfOrder=18, authorNames=ZHANG Q, YANG F Q, GE L, journalName=J Sep Sci, refType=null, unstructuredReference=ZHANG Q, YANG F Q, GE L, et al. Recent applications of hydrophilic interaction liquid chromatography in pharmaceutical analysis[J]. J Sep Sci, 2017, 40(1): 49-80., articleTitle=Recent applications of hydrophilic interaction liquid chromatography in pharmaceutical analysis, refAbstract=null), Reference(id=1218484897560314874, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, doi=null, pmid=null, pmcid=null, year=2017, volume=37, issue=9, pageStart=1693, pageEnd=1700, url=null, language=null, rfNumber=[20], rfOrder=19, authorNames=LIU Y, ZHANG F, CHANG Y, journalName=药物分析杂志, refType=null, unstructuredReference=LIU Y, ZHANG F, CHANG Y, et al. Determination of 17 adulteration of drugs in anti-acne cosmetics by liquid chromatography-tandem mass spectrometry with instant library searching[J]. Chin J Pharm Anal(药物分析杂志), 2017, 37(9):1693-1700., articleTitle=Determination of 17 adulteration of drugs in anti-acne cosmetics by liquid chromatography-tandem mass spectrometry with instant library searching, refAbstract=null)], funds=[Fund(id=1218484895605769116, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, awardId=GJJS-2022-9-1, language=CN, fundingSource=中国食品药品检定研究院关键技术研究基金项目(GJJS-2022-9-1), fundOrder=null, country=null)], companyList=[AuthorCompany(id=1218484891025588889, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, xref=1, ext=[AuthorCompanyExt(id=1218484891033977499, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891025588889, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 National Institutes for Food and Drug Control, Beijing 100050, China), AuthorCompanyExt(id=1218484891042366109, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891025588889, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=1 中国食品药品检定研究院, 北京 100050)]), AuthorCompany(id=1218484891109474978, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, xref=2, ext=[AuthorCompanyExt(id=1218484891117863587, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891109474978, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 Shouyao Holdings (Beijing) Co., Ltd, Beijing 100195, China), AuthorCompanyExt(id=1218484891130446500, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891109474978, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=2 首药控股(北京)股份有限公司, 北京100195)]), AuthorCompany(id=1218484891189166758, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, xref=3, ext=[AuthorCompanyExt(id=1218484891197555368, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891189166758, language=EN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 School of Pharmacy, Yantai University, Yantai 264003, China), AuthorCompanyExt(id=1218484891214332585, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, companyId=1218484891189166758, language=CN, country=null, province=null, city=null, postcode=null, companyName=null, departmentName=null, remark=3 烟台大学药学院, 山东 烟台 264003)])], figs=[ArticleFig(id=1218484893827384141, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Fig.1, caption=MRM chromatograms of eight AGs, figureFileSmall=eVIuDWXQh4HHWCJkNJB3ZQ==, figureFileBig=twB39t8i0LKizSMuXmcneA==, tableContent=null), ArticleFig(id=1218484893907075920, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=图1, caption=8种AGs的多反应检测(MRM)色谱图, figureFileSmall=eVIuDWXQh4HHWCJkNJB3ZQ==, figureFileBig=twB39t8i0LKizSMuXmcneA==, tableContent=null), ArticleFig(id=1218484894003544916, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Fig.2, caption=Extracted chromatograms of the 8 Ags, figureFileSmall=lWFm4B11zGkIzNWcym8bfQ==, figureFileBig=skk5Xpfb6oWmd/bt7850vw==, tableContent=null), ArticleFig(id=1218484894095819610, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=图2, caption=8种AGs的提取色谱图, figureFileSmall=lWFm4B11zGkIzNWcym8bfQ==, figureFileBig=skk5Xpfb6oWmd/bt7850vw==, tableContent=null), ArticleFig(id=1218484894175511391, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Fig.3, caption=Typical mass spectrograph of the 8 AGs, figureFileSmall=eHKUYtcfhSP3VdcfhfpWdA==, figureFileBig=H/TzaSiCo+EbH3SQLHhxAA==, tableContent=null), ArticleFig(id=1218484894309729122, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=图3, caption=8种AGs的典型质谱图, figureFileSmall=eHKUYtcfhSP3VdcfhfpWdA==, figureFileBig=H/TzaSiCo+EbH3SQLHhxAA==, tableContent=null), ArticleFig(id=1218484894443946857, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Fig.4, caption=Identification of kanamycin by library searching

A-EPI spectrum of the unknown compound; B-standard mass spectral data.

, figureFileSmall=cUkNIFBqkLwGSWXdU4Obug==, figureFileBig=e9gHgWFSsF4vO7l2My/KNw==, tableContent=null), ArticleFig(id=1218484894557193072, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=图4, caption=液质联用检索数据库检测卡那霉素的结果

A-未知化合物EPI质谱图谱;B-已知标准图谱。

, figureFileSmall=cUkNIFBqkLwGSWXdU4Obug==, figureFileBig=e9gHgWFSsF4vO7l2My/KNw==, tableContent=null), ArticleFig(id=1218484894670439283, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Tab.1, caption=

HPLC gradient elution procedure for the detection of aminoglycoside antibiotics (AGs)

, figureFileSmall=null, figureFileBig=null, tableContent=
t/min Mobile phase A/% Mobile phase B/%
0.1 30 70
1 95 5
3 99 1
4 99 1
5.1 70 30
6 30 70
10 30 70
), ArticleFig(id=1218484894863377271, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=表1, caption=

高效液相色谱(HPLC)检测氨基糖苷类抗生素(AGs)的梯度洗脱程序

, figureFileSmall=null, figureFileBig=null, tableContent=
t/min Mobile phase A/% Mobile phase B/%
0.1 30 70
1 95 5
3 99 1
4 99 1
5.1 70 30
6 30 70
10 30 70
), ArticleFig(id=1218484894959846266, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Tab.2, caption=

MRM parameters and retention time for each drug for AGs

, figureFileSmall=null, figureFileBig=null, tableContent=
Medicine m/z
(Parent ion)		 m/z
(Daughter ion)		 DP
/V		 CE
/V		 tR
/min
Kanamycin 485 163 21 30 3.11
Gentamicin C1 478 322 161 19 3.23
Gentamicin C1a 450 322 134 18 3.25
Gentamicin C2 464 160 141 28 3.25
Tobramycin 468 324 40 20 3.27
Neomycin 615 161 195 38 3.37
Isepamicin 570 411 133 23 3.00
Etimicin 478 350 160 19 3.23
), ArticleFig(id=1218484895077286782, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=表2, caption=

AGs的MRM最优参数和保留时间

, figureFileSmall=null, figureFileBig=null, tableContent=
Medicine m/z
(Parent ion)		 m/z
(Daughter ion)		 DP
/V		 CE
/V		 tR
/min
Kanamycin 485 163 21 30 3.11
Gentamicin C1 478 322 161 19 3.23
Gentamicin C1a 450 322 134 18 3.25
Gentamicin C2 464 160 141 28 3.25
Tobramycin 468 324 40 20 3.27
Neomycin 615 161 195 38 3.37
Isepamicin 570 411 133 23 3.00
Etimicin 478 350 160 19 3.23
), ArticleFig(id=1218484895173755780, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Tab.3, caption=

Verification of the method for detecting kanamycin in biological product A. n=3,$\bar{x}±s$

, figureFileSmall=null, figureFileBig=null, tableContent=
ρ(Theoretical)
/ng·mL-1		 ρ(Measured)
/ng·mL-1		 RSD/%
Precision Accuracy Recovery Matrix effect
5 5.00±0.04 0.71 100.25 98.14 -8.12
50 50.77±0.38 0.74 101.33 98.14 -6.44
100 99.67±0.12 0.12 99.67 97.14 -10.52
), ArticleFig(id=1218484895253447560, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=表3, caption=

INSA胰岛素中卡那霉素检测方法的验证。n=3,$\bar{x}±s$

, figureFileSmall=null, figureFileBig=null, tableContent=
ρ(Theoretical)
/ng·mL-1		 ρ(Measured)
/ng·mL-1		 RSD/%
Precision Accuracy Recovery Matrix effect
5 5.00±0.04 0.71 100.25 98.14 -8.12
50 50.77±0.38 0.74 101.33 98.14 -6.44
100 99.67±0.12 0.12 99.67 97.14 -10.52
), ArticleFig(id=1218484895324750734, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=EN, label=Tab.4, caption=

Stability of kanamycin in blank matrix stored for 12 h at 4 ℃

, figureFileSmall=null, figureFileBig=null, tableContent=
t/h ρ(Measured)/ng·mL-1
51) 501) 1001)
0 4.96 50.1 98.7
3 4.64 49.5 95.8
6 4.08 41.2 83.9
9 3.87 40.5 81.6
12 3.64 38.1 68.9
), ArticleFig(id=1218484895442191251, tenantId=1146029695717560320, journalId=1190317699101192196, articleId=1218290945410388690, language=CN, label=表4, caption=

4 ℃下卡那霉素在空白基质中12 h的稳定性

, figureFileSmall=null, figureFileBig=null, tableContent=
t/h ρ(Measured)/ng·mL-1
51) 501) 1001)
0 4.96 50.1 98.7
3 4.64 49.5 95.8
6 4.08 41.2 83.9
9 3.87 40.5 81.6
12 3.64 38.1 68.9
)], attaches=null, journal=Journal(id=1190317596361715715, delFlag=0, nameCn=中国药学杂志, nameEn=Chinese Pharmaceutical Journal, nameHistory1=null, nameHistory2=null, issn=1001-2494, eissn=null, cn=11-2162/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=hRN1R6HnoNwYkve/JRn0DA==, journalPrice=null, startedYear=null, abbrevIsoEn=null, journalRemark=null, publicationField=null, createdTime=1761723430007, updatedTime=1761735858241, createdBy=18614031015, updatedBy=13701087609, firstLetterCn=C, firstLetterEn=C, subjectCode=Life Sciences, subjectName=Life Sciences, subjectCodeEn=Life Sciences, subjectNameEn=null, picCn=hRN1R6HnoNwYkve/JRn0DA==, picEn=xSRntM4yOh2wVIE2w+OjYg==, jcr=null, cjcr=null, exts=[JournalExt(id=1190369724262355196, language=CN, name=中国药学杂志, 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=1761735858264, updatedTime=1761735858264, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=https://zgyxzzauthor.manuscriptcloud.com/login, submissionEditorUrl=https://zgyxzzeditor.manuscriptcloud.com/login, submissionReviewUrl=https://zgyxzzauthor.manuscriptcloud.com/login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""}), JournalExt(id=1190369724358824189, language=EN, name=Chinese Pharmaceutical Journal, 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=1761735858287, updatedTime=1761735858287, createdBy=13701087609, updatedBy=13701087609, submissionGuidelinesUrl=, submissionAuthorUrl=https://zgyxzzauthor.manuscriptcloud.com/login, submissionEditorUrl=https://zgyxzzeditor.manuscriptcloud.com/login, submissionReviewUrl=https://zgyxzzauthor.manuscriptcloud.com/login, submissionCeEditorUrl=, submissionAeEditorUrl=, option={"copyright":""})], databaseList=null, tenantJournalId=1190317699101192196, websiteList=[Website(id=1190317834875011552, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1190317699101192196, 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/zgyxzz/CN, language=CN, createTime=1761723486870, createBy=18614031015, updateTime=1761723510130, updateBy=18614031015, name=中国药学杂志-中文, tplId=1146099689490845704, title=中国药学杂志, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1190318144041353703, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=articleTextType, value=kx, createTime=1761723560581, updateTime=1761723560581, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144016187876, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=banner, value=null, createTime=1761723560575, updateTime=1761723560575, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144062325226, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=grayFlag, value=0, createTime=1761723560586, updateTime=1761723560586, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144007799267, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=logo, value=https://castjournals.cast.org.cn/joweb/zgyxzz/CN/file/pic?fileId=puyAm9wIHqZks7K8hj8APQ==, createTime=1761723560573, updateTime=1761723560573, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144074908140, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=minRunFlag, value=0, createTime=1761723560589, updateTime=1761723560589, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144032965094, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/zgyxzz/CN/file/pic, createTime=1761723560579, updateTime=1761723560579, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144070713835, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=silenceFlag, value=0, createTime=1761723560588, updateTime=1761723560588, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144024576485, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_cn_619/, createTime=1761723560577, updateTime=1761723560577, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144049742312, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=themeColor, value=null, createTime=1761723560583, updateTime=1761723560583, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318144053936617, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834875011552, code=themeStyle, value=null, createTime=1761723560584, updateTime=1761723560584, creator=18614031015, updator=18614031015)]), Website(id=1190317834937926113, webName=null, webTitle=null, webDomain=null, webCopyrigh=null, webIpcNo=null, seoTitle=null, seoKeywords=null, seoDescription=null, tenantJournalId=null, journalId=1190317699101192196, 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/zgyxzz/EN, language=EN, createTime=1761723486885, createBy=18614031015, updateTime=1761723527689, updateBy=18614031015, name=中国药学杂志-英文, tplId=1146101810881728533, title=Chinese Pharmaceutical Journal, delFlag=0, indexPage=/home, props=[WebsiteProps(id=1190318170478051825, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=articleTextType, value=kx, createTime=1761723566884, updateTime=1761723566884, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170461274606, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=banner, value=null, createTime=1761723566880, updateTime=1761723566880, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170494829044, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=grayFlag, value=0, createTime=1761723566888, updateTime=1761723566888, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170452885997, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=logo, value=https://castjournals.cast.org.cn/joweb/zgyxzz/EN/file/pic?fileId=puyAm9wIHqZks7K8hj8APQ==, createTime=1761723566878, updateTime=1761723566878, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170507411958, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=minRunFlag, value=0, createTime=1761723566891, updateTime=1761723566891, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170473857520, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=picServerUrl, value=https://castjournals.cast.org.cn/joweb/zgyxzz/EN/file/pic, createTime=1761723566883, updateTime=1761723566883, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170503217653, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=silenceFlag, value=0, createTime=1761723566890, updateTime=1761723566890, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170465468911, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=staticResourcePath, value=https://castjournals.cast.org.cn/joweb/cast_kjdb_en_623/, createTime=1761723566881, updateTime=1761723566881, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170482246130, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=themeColor, value=null, createTime=1761723566885, updateTime=1761723566885, creator=18614031015, updator=18614031015), WebsiteProps(id=1190318170486440435, tenantId=1146029695717560320, journalId=null, journalGroupId=null, siteId=1190317834937926113, code=themeStyle, value=null, createTime=1761723566886, updateTime=1761723566886, creator=18614031015, updator=18614031015)])], journalTitle=中国药学杂志, weixinUrl=null, journalUrl=http://www.zgyxzz.com.cn/, iacademicId=null, status=1, seqNo=null, journalTitleEn=Chinese Pharmaceutical Journal, journalPhotoCn=hRN1R6HnoNwYkve/JRn0DA==, journalPhotoEn=xSRntM4yOh2wVIE2w+OjYg==, journalFirstLetter=C, 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/zgyxzz/CN/10.11669/cpj.2024.15.011, detailUrlEn=https://castjournals.cast.org.cn/joweb/zgyxzz/EN/10.11669/cpj.2024.15.011, pdfUrlCn=https://castjournals.cast.org.cn/joweb/zgyxzz/CN/PDF/10.11669/cpj.2024.15.011, pdfUrlEn=https://castjournals.cast.org.cn/joweb/zgyxzz/EN/PDF/10.11669/cpj.2024.15.011, aliStartDate=null, aliEndDate=null, collectionFlag=false, citedCount=null, citedUrl=null, reference=null)
收藏切换
基于LC-MS/MS法建立快速检测8种氨基糖苷类抗生素的方法
收藏切换
PDF下载
孙晓龙 1 , 杨青 2 , 王洪波 3 , 刘颖 1, *
中国药学杂志 | 论著 2024,59(15): 1438-1444
收起
收藏切换
中国药学杂志 | 论著 2024, 59(15): 1438-1444
基于LC-MS/MS法建立快速检测8种氨基糖苷类抗生素的方法
全屏
孙晓龙1, 杨青2, 王洪波3, 刘颖1, *
作者信息
  • 1 中国食品药品检定研究院, 北京 100050
  • 2 首药控股(北京)股份有限公司, 北京100195
  • 3 烟台大学药学院, 山东 烟台 264003

    • 孙晓龙,男,硕士研究生 研究方向:药物分析与药物质量控制;

    杨青,女,硕士 研究方向:药物分析与药物质量控制。

通讯作者:

* 刘颖,女,博士,研究员 研究方向:药物分析与药物质量控制Tel:(010)67872233-8312
Rapid Detection of Eight Aminoglycoside Antibiotics by Liquid Chromatography-Tandem Mass Spectrometry
Xiaolong SUN1, Qing YANG2, Hongbo WANG3, Ying LIU1, *
Affiliations
  • 1 National Institutes for Food and Drug Control, Beijing 100050, China
  • 2 Shouyao Holdings (Beijing) Co., Ltd, Beijing 100195, China
  • 3 School of Pharmacy, Yantai University, Yantai 264003, China
出版时间: 2024-08-08 doi: 10.11669/cpj.2024.15.011
文章导航
收藏切换
摘要
收起

目的 应用液质谱联用(LC-MS/MS)检索数据库技术建立卡那霉素、庆大霉素C1、庆大霉素C1a、庆大霉素C2、妥布霉素、新霉素、异帕米星、依替米星8种氨基糖苷类抗生素(aminoglycoside antibiotics,AGs)的快速检测方法。方法 采用Shiseido PC HILIC(2.0 mm×100 mm,3 μm)色谱柱对8种AGs进行分离,体积分数0.5%甲酸水溶液-0.1%甲酸乙腈溶液为流动相,梯度洗脱,流速为0.4 mL·min-1;采用多重反应监测(MRM)扫描建立8种AGs的筛查方法;采用碰撞能量扩展(CES)功能和增强子离子(EPI)扫描模式采集8种AGs的典型质谱图,添加到已经建立的抗生素检索质谱库中。结果 所建立的方法专属性强,灵敏度高,10 min即可实现对8种AGs的初筛和定性分析。应用该方法对3批INSA胰岛素产品中的卡那霉素残留进行了监测,3批样品中均未检测到卡那霉素,其残留量小于检出限0.05 ng·mg-1。结论 本研究应用液质联用检索数据库技术建立的8种AGs的检测方法可以对痕量AGs进行快速筛查和准确定性。

氨基糖苷类抗生素  /  液相色谱-串联质谱法  /  亲水相互作用色谱  /  检索数据库  /  定性分析  /  定量分析

OBJECTIVE To establish a method for simultaneous determination of 8 aminoglycoside antibiotics (AGs) including kanamycin, gentamycin C1, gentamycin C2, gentamycin C1a, tobramycin, neomycin, isepamicin and etimicin by LC-MS/MS with instant library searching. METHODS Eight AGs were separated by Shiseido PC HILIC (2.0 mm×100 mm, 3 μm) column, with 0.5% formic acid aqueous solution-0.1% formic acid acetonitrile solution as mobile phase and 0.4 mL·min-1 of flow rate,and procedure of the gradient elution was performed. The screening method of 8 AGs was established by the scanning mode of multiple reaction monitoring (MRM). Typical mass spectrograms of 8 AGs were collected by collision energy expansion (CES) function and enhanced ion (EPI) scanning mode, and added them to the already established mass spectralibrary of antibiotics searching. RESULTS The established method has the advantages of short analysis time, strong specificity and high sensitivity. The screening and qualitative analysis of 8 AGs can be realized within 10 min. Three batches of the INSA insulin product were detected by this method, and kanamycin that was less than the detection limit of 0.05 ng·mg-1 were not detected in above samples. CONCLUSION In this study, the detection method of 8 AGs established by LC-MS/MS with instant library searching can quickly screen and accurately determine trace AGs.

aminoglycoside antibiotics  /  liquid chromatography-tandem mass spectrometry (LC-MS/MS)  /  hydrophilic interaction chromatography (HILIC)  /  instant library searching  /  quantitative analysis  /  qualitative analysis
孙晓龙, 杨青, 王洪波, 刘颖. 基于LC-MS/MS法建立快速检测8种氨基糖苷类抗生素的方法. 中国药学杂志, 2024 , 59 (15) : 1438 -1444 . DOI: 10.11669/cpj.2024.15.011
Xiaolong SUN, Qing YANG, Hongbo WANG, Ying LIU. Rapid Detection of Eight Aminoglycoside Antibiotics by Liquid Chromatography-Tandem Mass Spectrometry[J]. Chinese Pharmaceutical Journal, 2024 , 59 (15) : 1438 -1444 . DOI: 10.11669/cpj.2024.15.011
正文
收起
氨基糖苷类抗生素(aminoglycoside antibiotics,AGs)是在20 世纪40 年代被发现的,AGs家族起源于Schatz和Waksman发现的从天然产物中分离得到的链霉素[1]。链霉素诞生后,大多数AGs在与链霉素密切相关的次级代谢物的混合物中被发现,通过对天然来源的AGs进行结构修饰又得到了一系列半合成衍生物[2]。AGs是通过氧桥和氨基醇相连的苷类抗生素,其结构中含有许多氨基和羟基,大多数为强极性化合物,在临床中用于治疗细菌感染性疾病。
目前,国内外药典中主要采用薄层色谱(thin-layer chromatography,TLC)法和高效液相色谱(high pressure liquid chromatography,HPLC)法进行AGs药品的质量控制,HPLC法常用的检测器有紫外(ultraviolet,UV)检测器、蒸发光散射检测器(evaporative light-scattering detector, ELSD)、脉冲安培检测器(pulse amperometric detector,PAD)[3],值得注意的是使用HPLC-UV法时需采用衍生化方法为AGs引入生色团,以利于检测。由于AGs良好的抗菌作用,它也被用于其他领域,如在疫苗等生物制品的生产中常会加入少量AGs防止细菌感染[4-5],但是要对其添加量进行严格控制,并进行检测。由于传统HPLC法的灵敏度限制,无法对痕量AGs进行准确定性和定量分析。液质联用(LC-MS/MS)分析技术具有灵敏度高、检测限低、专属性强的特点,已成为痕量抗生素检测常用的分析手段[6-8],它可同时分析多种药物[9-12]。质谱数据库是筛查、检索和定性分析未知化合物的有力工具,目前被广泛应用的有美国国家标准与技术研究院(NIST)库[13]和日本有机物光谱数据库(SDBS)[14]。因此,LC-MS/MS检索数据库技术,已被应用于农药残留、药物滥用和毒物分析领域[15-17]。该技术可对未知化合物同时进行定性筛查,缩短分析时间,减少对照品的使用。
本研究采用亲水相互作用色谱(hydrophilic interaction chromatography, HILIC)模式与质谱联用建立了庆大霉素、新霉素、卡那霉素三大家族及其半合成衍生物中具有代表性的共8种AGs的LC-MS/MS质谱检索数据,填补了本实验室建立的包含124种抗生素的LC-MS/MS检索数据库中AGs的空缺,且所建立的方法具有可扩展性,在后续应用过程中可根据需要添加其他AGs,为非法添加和残留AGs的检测提供有力的技术支撑。
1 仪器与试药
收起
AB Sciex 6500 Qtrap质谱仪(美国AB Sciex公司);20AT高效液相色谱仪(日本Shimadzu公司);CP225D电子天平(瑞士Mettler-Toledo公司);TP 600超声波清洗仪(天鹏电子新技术有限公司);Milli-Q Reference超纯水制备仪(美国Merck Millipore公司)。
甲醇(批号:203512)、乙腈(批号:204433)和甲酸(批号:202674)(质谱纯,美国Fisher公司);氨水(批号:STBJ2608,分析纯,美国Sigma公司);卡那霉素(批号:130307-201417,含量:67.9%)、庆大霉素(批号:130326-201716,每毫克相当于637庆大霉素单位,含量:C1 15.9%,C1a 15.2%,C2 16.9%)、妥布霉素(批号:130527-200402,含量:91.4%)、新霉素(批号:130309-201512,每毫克相当于652单位)、异帕米星(批号:130594-201401,含量:70.9%)、依替米星(批号:130365-200702,每毫克相当于567单位)对照品和标准物质(中国食品药品检定研究院);INSA胰岛素的空白对照及其样品均由某生物医药公司研发生产。
2 方法与结果
收起
2.1 LC-MS/MS方法
2.1.1 色谱方法的建立
AGs是通过氧桥和氨基醇相连的苷类抗生素,其结构中含有许多氨基和羟基,大多数为强极性化合物,在普通反相C18色谱柱几乎不保留。而在HILIC模式下,该类化合物具有更好的保留[18-19],因此本研究选择HILIC色谱柱对8种AGs进行检测。本实验采用8种AGs的混合标准溶液进行液相条件的优化,初步采用乙腈-水为流动相进行优化,通过调节流动相比例、流速、柱温和柱长考察各色谱峰的保留时间、峰形和灵敏度,最终采用Shiseido PC HILIC(2.0 mm×100 mm, 3 μm)色谱柱分离8种AGs。为了进一步提高检测的灵敏度和改善峰形,在水相分别加入了体积分数0.1%、0.3%、0.5%和0.7%甲酸,结果发现随着甲酸浓度的增加,各目标抗生素的峰形不断尖锐,但浓度太高时灵敏度反而降低。因此,最终选择体积分数0.5%甲酸水溶液为流动相A,体积分数0.1%甲酸乙腈溶液为流动相B。
综上,液相分离采用Shiseido PC HILIC(2.1 mm×100 mm,3 μm)色谱柱,流动相:体积分数0.5%甲酸水溶液为流动相A;体积分数0.1%甲酸乙腈溶液为流动相B,按照表1进行梯度洗脱,流速0.4 mL·min-1,柱温40 ℃,进样量10 μL。
2.1.2 质谱方法
质谱测定采用电喷雾(ESI)电离源,在正离子模式下进行多反应监测(MRM)扫描。电喷雾电压为5.5 kV,离子化温度为500 ℃,雾化气、辅助气和气帘气压力分别为275.8、275.8、172.4 kPa,碰撞气电压为6 V,进口电压10 V,出口电压11 V。增强子离子扫描(EPI)模式下,扫描速度为10 000 ·s-1,碰撞能量为35 eV,碰撞能量扩展(CES)为15 eV。在信息关联采集中,MRM响应值大于1 000 CPS即触发EPI扫描。
2.2 对照品溶液的制备
分别准确称取适量的卡那霉素、庆大霉素(包含庆大霉素C1、庆大霉素C1a、庆大霉素C2)、妥布霉素、新霉素、异帕米星、依替米星对照品,用水溶解并稀释,得到浓度约为1 mg·mL-1的6种对照品储备液。
分别精密量取6种储备液一定量,采用体积分数0.1%甲酸甲醇-水(体积比1:1)稀释,制成浓度为1 μg·mL-1或100 ng·mL-1的工作溶液。
精密量取每种储备液0.1 mL混合,置于10 mL量瓶中,加水定容到刻度,进一步用水稀释制成浓度为100 ng·mL-1的AGs混合标准溶液。
2.3 高通量筛查方法的建立
MRM扫描是质谱检测常用的分析方法,具有特异性强、灵敏度高、准确性高、重现性好和线性动态范围宽的优点。通常1次扫描可以检测上百种化合物,达到高通量的筛查目的。首先要确定待测化合物的特异性母离子,然后将选定的母离子进行碰撞诱导(collision-induced),最后选择特异性子离子进行质谱信号的采集,并对每个待测化合物的试验参数进行手动优化,以确定最佳的去簇电压(declustering potential, DP)、碰撞能(collision energy,CE)和碰撞室出口电压(collision cell exit potential, CXP)参数值。表2列出了8种待测化合物的离子通道和MRM最佳参数值。按照“2.1”项下优化的液相和质谱方法,将“2.2”中的8种AGs混合标准溶液注入液质联用仪进行分析,得到8种AGs的色谱图(图1)和保留时间(表2)。8种化合物的离子通道不同,所以不需要在色谱上完全分开,就可以准确定性和定量。图2为分别提取的8种AGs的色谱图。
2.4 质谱检索数据库的建立
6500Qtrap系统是将串联四级杆和离子阱结合在一起的质谱系统,其Q3能够实现四级杆扫描和离子阱扫描的快速转换,从而同时获得MRM和EPI数据。本研究的目的是获得8种AGs的典型EPI质谱图,保存到实验室已经建立的抗生素质谱检索数据库中。实验中应用碰撞能量扩展功能(CES),在1次扫描中完成在3个不同碰撞能量下EPI质谱图的采集,最终给出3张谱图的平均谱图,这样经过1次扫描就能够同时得到待测化合物从高质量数到低质量数的典型质谱图[20]。
取“2.2”项下每种抗生素工作溶液10 μL,逐个注入液质联用仪,采集每种抗生素的典型质谱图(图3),将每种抗生素的名称、分子式和标准化图谱存储在计算机Library(Analyst version 1.6.2)中,完成8种AGs液质联用检索数据库的建立。
2.5 方法的应用
2.5.1 初筛和定性
在实际应用过程中,首先应用所建立的8种AGs的MRM高通量筛选方法筛选样品中可能含有的AGs。进而执行EPI扫描,EPI扫描和MRM筛选之间通过结合信息关联采集(information association collection,IDA)连接,即当MRM筛选的化合物信号强度达到IDA所设定的阈值时,EPI扫描会被触发,从而获得化合物的质谱图[20]。最后将得到的质谱图在所建的质谱库中进行检索,完成化合物的定性。本研究按照上述分析流程对某生物医药公司生产的3批INSA胰岛素产品进行检测,该产品在生产时为控制微生物使用了卡那霉素,并在生产的最后阶段进行了抗生素的清除。检测结果表明,所建立的数据库能够准确筛查并确认INSA胰岛素中的卡那霉素(图4),且该INSA胰岛素中卡那霉素的残留低于定量限。
2.5.2 定量测定
应用所建立的MRM高通量方法中卡那霉素的检测方法可以对INSA胰岛素产品中的卡那霉素进行定量测定,定量方法如下。
样品前处理:精密称取INSA胰岛素20 mg,向其中加入氨水进行蛋白质沉淀,涡旋15 s,在10 000 r·min-1、4 ℃条件下,离心30 min。取上清液注入液质联用仪分析。
方法学验证:①检出限、定量限、线性范围,在INSA胰岛素的空白基质中配制卡那霉素浓度为0.5、0.1、0.05 ng·mL-1的样品,按照样品前处理方法进行前处理,然后注入液质联用仪分析,以信噪比(S/N)为3:1判定检出限(LOD),以信噪比(S/N)为10:1判定定量限(LOQ)。在空白基质中配制浓度为2.5、5、10、25、50、100、200 ng·mL-1标准样品,按上述前处理方法处理后进样分析,以相关系数r衡量线性相关性。结果表明:卡那霉素的LOD为0.05 ng·mg-1,LOQ为0.1 ng·mg-1,卡那霉素在2.5~200 ng·mg-1范围内,回归方程为Y=5.96×103X-3.17×103(r=0.999 9)。②精密度与准确度,在INSA胰岛素的空白基质中加入2 mL质量浓度为5、50、100 ng·mL-1的标准溶液,每种浓度平行配制3份。按照样品前处理方法进行前处理,然后注入液质联用仪分析。结果表明,3种不同浓度的卡那霉素标准溶液(5、50、100 ng·mL-1)在INSA胰岛素空白基质中的精密度相对标准偏差(RSD)小于1%,准确度范围在99%~102%,见表3。③回收率,将INSA胰岛素的空白基质先按照样品前处理方法进行前处理,然后精密量取1 mL空白提取液,向其中加入10 μL的3种不同浓度的卡那霉素标准溶液,制得卡那霉素质量浓度分别为5、50、100 ng·mL-1的对照溶液,每种浓度平行配制3份,作为对照溶液;按照“②”配制方法,制得质量浓度为5、50、100 ng·mL-1加标样品溶液。比较对照溶液和样品溶液的峰面积的比值,计算3种不同浓度下卡那霉素回收率,结果表明,卡那霉素回收率范围在97%~99%,见表3。④基质效应,按照“②”的方法配制3种不同浓度的加标样品溶液,每种浓度各3份;将不含INSA胰岛素的卡那霉素标准溶液(5、50、100 ng·mL-1)按照样品前处理的方法进行处理,制得对照溶液。比较样品溶液与对照溶液在液质联用的响应,计算不同浓度下卡那霉素的基质效应。结果表明,基质效应在-20%~20%,见表3,可忽略不计,认为INSA胰岛素中的基质对卡那霉素没有明显的增强或是抑制效应。⑤ 稳定性,将加标溶液(5、50、100 ng·mL-1)放置4 ℃,分别检测3种不同浓度的样品在0、3、6、9、12 h的稳定性,结果显示:卡那霉素极不稳定,在放置3 h时,样品就开始轻微地降解;当放置6 h时,样品的降解率就已经达到近20%,见表4。因此,卡那霉素的使用过程应临用新制。
样品测定:采用上述已验证的方法测定INSA胰岛素中的卡那霉素,结果显示,该生物医药公司的3批 INSA胰岛素中卡那霉素残留量小于检出限0.05 ng·mg-1。
3 讨论
收起
本实验采用HILIC色谱柱增强AGs在色谱柱上的保留行为,应用LC-MS/MS检索数据技术建立了能够同时检测8种AGs的定性方法。本研究所建立的方法检测时间短,专属性强且灵敏度高,在10 min内即可实现8种AGs的筛查和定性分析,避免假阳性结果。与传统的检测方法相比,该法可同时检测多种AGs,而且可以根据不同的需要添加其他AGs到该质谱检索数据库中。本研究针对AGs建立的液质联用检索数据库可用于生物制品、动物性食物、环境样品和等其他样品中痕量AGs的检测,为其质量与安全提供了保障,同时也为政策的制定和监管提供有效的技术支撑。
基金
收起
  • 中国食品药品检定研究院关键技术研究基金项目(GJJS-2022-9-1)
文献
收起
参考文献 引证文献
排序方式：
[1]
SCHATZ A, BUGLE E, WAKSMAN S A. Streptomycin, a substance exhibiting antibiotic activity against gram-positive and gram-negative bacteria[J]. Proc Soc Exp Biol Med, 1944, 55(1): 66-69.
[2]
WU J H, LIU P Y. The past and present of aminoglycoside antibiotics[J]. Chin J Antibiot(中国抗生素杂志), 2019, 44(11):1275-1282.
[3]
MENG F, ZHOU X H, YUAN Y Z. Development of detection technologies for aminoglycoside antibiotics[J]. Pharm Clin Res(药学与临床研究), 2022, 30(5):441-446.
[4]
XU C X, GU C L, FANG Y, et al. Application of antibiotics and the methods for their determination in biological products[J]. World Notes Antibiot(国外医药抗生素分册), 2017, 38(4):179-183,189.
[5]
YANG X, ZENG X W, LIU Y, et al. Detection of the residual content of kanamycin and gentamicin in live attenuated japanese encephalitis vaccine with ELISA method[J]. Prog Microbiol Immunol(微生物学免疫学进展), 2010, 38(3):28-31.
[6]
YANG Q, TIAN Y, JIANG Z Q, et al. Application of liquid-mass spectrometry in antibiotic analysis[J]. Chin J Drug Eval(中国药物评价), 2022, 39(2):113-118.
[7]
SONG X, ZHOU T, LI J, et al. Determination of macrolide antibiotics residues in pork using molecularly imprinted dispersive solid‐phase extraction coupled with LC-MS/MS[J]. J Sep Sci, 2018, 41(5): 1138-1148.
[8]
DO T C M V, NGUYEN D Q, NGUYEN T D, et al. Development and validation of a LC-MS/MS method for determination of multi-class antibiotic residues in aquaculture and river waters, and photocatalytic degradation of antibiotics by TiO2 nanomaterials[J]. Catalysts, 2020, 10(3): 356.
[9]
CHAN C L, WAI H K F, WU P, et al. A universal LC-MS/MS method for simultaneous detection of antibiotic residues in animal and environmental samples[J]. Antibiotics, 2022, 11(7): 845. DOI: 10.3390/antibiotics11070845.
[10]
LIU Y, ZHANG J, HU C. Validated LC-MS/MS method for simultaneous analysis of 21 cephalosporins in zebrafish for a drug toxicity study[J]. Anal Biochem, 2018, 558: 28-34.
[11]
YANG Q, LIU Y, JIANG Z, et al. Multi-residue method for the detection of 40 β-lactam-antibiotics in vaccines by LC-MS/MS[J]. Anal Biochem, 2021, 631: 114299. DOI: 10.1016/j.ab.2021.114299.
[12]
LIU Y, UBOH C E, LI X, et al. Validated LC-MS-MS method for simultaneous analysis of 17 barbiturates in horse plasma for doping control[J]. J Anal Toxicol, 2017, 41(5): 431-440.
[13]
LEMMON E W, HUBER M L, MCLINDEN M O. NIST standard reference database 23: reference fluid thermodynamic and transport properties-REFPROP, version 10.0[EB/OL]. Gaithersburg, MD: National Institute of Standards and Technology (NIST), 2018 (2023-11-04) [2023-12-12]. https://www.nist.gov/srd/refprop. https://www.nist.gov/srd/refprop
[14]
SAITO T, KINUGASA S. Development and release of a spectral database for organic compounds-key to the continual services and success of a large-scale database[J]. Synthesiol Eng Ed, 2011, 4(1): 35-44.
[15]
PANG G F, FAN C L, CHANG Q Y, et al. Screening of 485 pesticide residues in fruits and vegetables by liquid chromatography-quadrupole-time-of-flight mass spectrometry based on TOF accurate mass database and QTOF spectrum library[J]. J AOAC Int, 2018, 101(4): 1156-1182.
[16]
LIU Y, UBOH C E, SOMA L R, et al. Efficient use of retention time for the analysis of 302 drugs in equine plasma by liquid chromatography-MS/MS with scheduled multiple reaction monitoring and instant library searching for doping control[J]. Anal Chem, 2011, 83(17): 6834-6841.
[17]
ZHAO-YONG L, JUN-HUI C, XIN L, et al. Rapid screening and identification of paralytic shellfish poisoning toxins in red tide algae using hydrophilic interaction liquid chromatography-high resolution mass spectrometry with an accurate-mass database[J]. Fresenius J Anal Chem, 2013, 41(7): 979-985.
[18]
ERKMEN C, GEBREHIWOT W H, USLU B. Hydrophilic interaction liquid chromatography (HILIC): latest applications in the pharmaceutical researches[J]. Curr Pharm Anal, 2021, 17(3): 316-345.
[19]
ZHANG Q, YANG F Q, GE L, et al. Recent applications of hydrophilic interaction liquid chromatography in pharmaceutical analysis[J]. J Sep Sci, 2017, 40(1): 49-80.
[20]
LIU Y, ZHANG F, CHANG Y, et al. Determination of 17 adulteration of drugs in anti-acne cosmetics by liquid chromatography-tandem mass spectrometry with instant library searching[J]. Chin J Pharm Anal(药物分析杂志), 2017, 37(9):1693-1700.
2024年第59卷第15期
PDF下载
133
66
引用本文
BibTeX
文章信息
doi: 10.11669/cpj.2024.15.011
  • 接收时间：2023-12-22
  • 首发时间：2026-01-14
  • 出版时间：2024-08-08
补充材料
相关文章
文章信息
作者
出版历史
  • 收稿日期：2023-12-22
基金
中国食品药品检定研究院关键技术研究基金项目(GJJS-2022-9-1)
作者信息
    1 中国食品药品检定研究院, 北京 100050
    2 首药控股(北京)股份有限公司, 北京100195
    3 烟台大学药学院, 山东 烟台 264003

通讯作者:

* 刘颖,女,博士,研究员 研究方向:药物分析与药物质量控制Tel:(010)67872233-8312
参考文献
分享链接
https://castjournals.cast.org.cn/joweb/zgyxzz/CN/10.11669/cpj.2024.15.011
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