分析测试学报2025，Vol.44Issue(3)：479-485,7.DOI:10.12452/j.fxcsxb.240628178
液相色谱-串联质谱法手性拆分和测定水产品中奥沙西泮和替马西泮对映体
Enantiomeric Separation and Determination of the Enantiomers of Oxazepam and Temazepam in Aquaculture Products by Liquid Chromatography-Tandem Mass Spectrometry
摘要
Abstract
An analytical method was proposed for the enantiomeric separation and residual determi-nation of the enantiomers of oxazepam and temazepam in aquaculture products by liquid chromatogra-phy-tandem mass spectrometry(LC-MS/MS).Samples were extracted twice with acetonitrile and the centrifuged extractions were blew to dryness under nitrogen gas at 40℃.Then,the dried residues were dissolved with 2 mL 50%acetonitrile-water solution,followed by dispersive solid phase extrac-tion(dSPE)cleanup protocol prior to be injected into LC-MS/MS.The chromatographic separation of the targeted enantiomers of oxazepam and temazepam were conducted on an EnantioPAK® Y1-R col-umn(5 µm,150 mm×4.6 mm)under isocratic elution procedure,utilizing acetonitrile and 0.1%formic acid-5 mmol/L ammonium acetate solution as mobile phases.The targeted enantiomers were determined with internal standard method,operating in positive electrospray ionization scanning mode(ESI+)and multiple reaction monitoring(MRM)mode.Excellent linearity for four targeted enan-tiomers were prepared in the concentration ranges of 0.5-50 µg/L,with correlation coefficients(r2)not less than 0.999 0.The limits of detection(LODs)and the limits of quantitation(LOQs)in aqua-culture product samples were 0.2 µg/kg and 0.5 µg/kg,respectively.The average recoveries of tar-geted enantiomers fortified in five negative sample matrixes at three spiked concentration levels ranged from 82.6%to 107%,with relative standard deviations(RSDs,n=6)not more than 9.2%.The newly developed method is sensitive and reliable,and is suitable for the residue analysis of the enantiomers of oxazepam and temazepam in various aquaculture product matrixes.关键词
液相色谱-串联质谱法/对映体/手性拆分/分散固相萃取/水产品Key words
liquid chromatography-tandem mass spectrometry(LC-MS/MS)/enantiomers/enan-tiomeric separation/dispersive solid phase extraction(dSPE)/aquaculture product分类
化学化工引用本文复制引用
王旭峰,王强,侯超苹,杨金兰,黎智广,张英侠,李惠青,黄珂..液相色谱-串联质谱法手性拆分和测定水产品中奥沙西泮和替马西泮对映体[J].分析测试学报,2025,44(3):479-485,7.基金项目
海南省自然科学基金面上项目(322MS152) （322MS152）
中国水产科学研究院南海水产研究所中央级公益性科研院所基本科研业务费专项资金(2023TS05,2021SD20) （2023TS05,2021SD20）
农业国家标准和行业标准制修订项目(NYB-23110) （NYB-23110）
