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分散固相萃取结合UPLC-MS/MS测定柑桔中青霉素G及其代谢物残留
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周杰,赵静,董超,张耀海,赵其阳,焦必宁 中国农业科学院/西南大学柑桔研究所农业农村部柑桔产品质量安全风险评估实验室(重庆)农业农村部柑桔及苗木质量监督检验测试中心 
基金项目:国家现代农业(柑桔)产业技术体系建设专项(CARS-26);国家柑桔及热带作物产品质量安全风险评估专项(GJFP2018004);2017年农业行业标准制订项目(181721301092371115);中央高校基本科研业务费专项资金(SWU116078)
中文摘要:建立了分散固相萃取结合超高效液相色谱-串联质谱(DSPE/UPLC-MS/MS)快速检测柑桔中青霉素G及其代谢物青霉二酸和去羧青霉噻唑酸的分析方法。样品经80%乙腈提取,十八烷基键合硅胶吸附剂(C18)净化。目标残留物经Acquity UPLCHSS T3色谱柱分离,以乙腈-01%甲酸溶液为流动相进行梯度洗脱,采用正离子多反应监测模式(MRM)检测,基质匹配标准曲线法定量。结果表明,3种目标分析物可在5 min内实现有效快速分离;在5~2 000 μg/L质量浓度范围内线性关系良好(r2≥0.998 1),方法检出限(LOD)为0.5~1 μg/kg,定量下限(LOQ)为5~10 μg/kg。在3个不同加标水平下,柑桔果肉、果皮和全果中的平均回收率为76.7%~107%,相对标准偏差(RSD)为1.3%~9.6%。该方法快速、简便、灵敏、准确,适用于柑桔中青霉素G及其两种代谢物残留的测定。
中文关键词:分散固相萃取  青霉素G  代谢物  超高效液相色谱-串联质谱(UPLC-MS/MS)  柑桔
 
Determination of Penicillin G and Its Metabolite Residues in Citrus by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid-phase Extraction
Abstract:A rapid method was developed for the determination of penicillin G and its two metabolites(penillic acid and penilloic acid) residues in citrus by dispersive solid phase extraction/ultra high performance liquid chromatography-tandem mass spectrometry(DSPE/UPLC-MS/MS).The citrus samples were extracted with 80% acetonitrile,then purified with C18.The analytes were separated on an Acquity UPLCHSS T3 column with acetonitrile and 01% formic acid solution as mobile phases by gradient elution,and finally detected by tandem mass spectrometry in positive ESI mode(ESI+).Identification and quantitation were performed by UPLC-MS/MS under multi reaction monitoring(MRM) mode and matrix matched standard curve method,respectively.Results showed that three analytes could realize an effective and rapid separation within 5 min.There were good linear relationships for the analytes in the concentration range of 5-2 000 μg/L with their correlation coefficients(r2) not less than 0.998 1.The limits of detection(LOD) and limits of quantitation(LOQ) of the method were in the ranges of 0.5-1 μg/kg and 5-10 μg/kg,respectively.The spiked recoveries for penicillin G and its metabolites in blank citrus samples were in the range of 76.7%-107%,with relative standard deviations(RSD) of 1.3%-9.6%.The method is rapid,simple,sensitive and accurate,and is suitable for the determination of penicillin G and its two metabolite residues in citrus.
Key Words:dispersive solid phase extraction  penicillin G  metabolites  ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)  citrus
引用本文:周杰,赵静,董超,张耀海,赵其阳,焦必宁.分散固相萃取结合UPLC-MS/MS测定柑桔中青霉素G及其代谢物残留[J].分析测试学报,2019,(4):442-448.
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