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

作　　者：王旭峰[1,2,4] 王强 侯超苹[1] 杨金兰 黎智广 张英侠 李惠青[1] 黄珂 WANG Xu-feng;WANG Qiang;HOU Chao-ping;YANG Jin-lan;LI Zhi-guang;ZHANG Ying-xia;LI Hui-qing;HUANG Ke(Fishery Environment and Aquatic Products Quality Testing Center of the Ministry of Agriculture and Rural Affaires(Guangzhou),South China Sea Fisheries Research Institute,Chinese Academy of Fishery Sciences,Guangzhou 510300,China;Sanya Tropical Fisheries Research Institute,Sanya 572025,China;Guangzhou Academy of Agricultural and Rural Sciences,Guangzhou 510300,China;Guangdong Provincial Key Laboratory of Fishery Ecology and Environment,Guangzhou 510300,China)

机构地区：[1]中国水产科学研究院南海水产研究所,农业农村部渔业环境及水产品质量检验测试中心(广州),广东广州510300 [2]三亚热带水产研究院,海南三亚572025 [3]广州市农业农村科学院,广东广州510300 [4]广东省渔业生态环境重点实验室,广东广州510300

出　　处：《分析测试学报》2025年第3期479-485,共7页Journal of Instrumental Analysis

基　　金：海南省自然科学基金面上项目(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);农业国家标准和行业标准制修订项目(NYB-23110)。

摘　　要：建立了液相色谱-串联质谱(LC-MS/MS)手性拆分和测定水产品中奥沙西泮和替马西泮对映体残留量的分析方法。样品经乙腈提取2次,40℃条件下氮气浓缩至近干,残渣加入2 mL 50%乙腈-水溶液溶解,采用分散固相萃取净化,LC-MS/MS测定。使用EnantioPAK■Y1-R(5μm,150 mm×4.6 mm)手性色谱柱,乙腈和0.1%甲酸-5 mmol/L乙酸铵溶液作为流动相,采用等度洗脱方式实现奥沙西泮和替马西泮手性对映体的拆分。目标对映体采用电喷雾正离子(ESI^(+))模式电离,多反应监测(MRM)模式下,内标法测定。目标对映体在0.5~50μg/L质量浓度范围内线性关系良好,相关系数(r^(2))均不低于0.9990。水产品中对映体的检出限和定量下限分别为0.2μg/kg和0.5μg/kg。在5种空白基质中添加低、中、高浓度水平的目标对映体,样品平均加标回收率为82.6%~107%,相对标准偏差(RSD,n=6)为1.6%~9.2%。该方法灵敏可靠、适用性强,可用于不同水产品中奥沙西泮和替马西泮对映体的分析。An analytical method was proposed for the enantiomeric separation and residual determination of the enantiomers of oxazepam and temazepam in aquaculture products by liquid chromatography-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 extraction(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 column(5μm,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 enantiomers were prepared in the concentration ranges of 0.5-50μg/L,with correlation coefficients(r^(2))not less than 0.9990.The limits of detection(LODs)and the limits of quantitation(LOQs)in aquaculture product samples were 0.2μg/kg and 0.5μg/kg,respectively.The average recoveries of targeted 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 

分 类 号：O657.7[理学—分析化学] TS207.3[理学—化学]