UHPLC-MS/MS Determination of Residual Amounts of Benzimidazoles and Its Metabolites in Dairy Products
摘 要
乳制品样品中加入水、乙腈、氯化钠提取,采用乙腈饱和的正己烷脱脂净化。采用超高效液相色谱-串联质谱法测定样品溶液中苯并咪唑类药物及其代谢物的残留量。以Atlantis T3色谱柱为固定相,以不同体积比的0.1%(体积分数,下同)甲酸乙腈溶液和0.1%甲酸溶液的混合液为流动相进行梯度洗脱,串联质谱分析中采用电喷雾离子源(正离子扫描)和可编辑多反应监测模式。采用同位素内标法定量,苯并咪唑类药物及其代谢物的线性范围均为0.02~5.0 μg·L-1,检出限(3S/N)为0.010~1.0 μg·kg-1,测定下限(10S/N)为0.025~4.0 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为81.4%~108%,测定值的相对标准偏差(n=6)为0.40%~9.3%。
Abstract
The dairy product sample was extracted with water, acetonitrile and NaCl. n-Hexane saturated with acetonitrile was used for de-fat and purification. UHPLC-MS/MS was applied to the determination of residual amounts of benzimidazoles and its metabolites in the sample solution. Atlantis T3 chromatographic column was used as stationary phase, and the mixture of 0.1% (φ, the same below) formic acid acetonitrile solution and 0.1% formic acid solution mixed in different ratios was used as mobile phase in gradient elution. ESI+ and scheduled multi-reactions monitor mode were adopted in MS/MS.Isotope was used as internal standard. Linearity ranges of benzimidazoles and its metabolites were found in the same range of 0.02-5.0 μg·L-1, with detection limits (3S/N) in the range of 0.010-1.0 μg·kg-1 and lower limits of determination (10S/N) in the range of 0.025-4.0 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 81.4%-108%, with RSDs (n=6) of determined values in the range of 0.40%-9.3%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202005013
所属栏目 专题报道(药物分析)
基金项目 广东省科技计划项目(2015A030401074)
收稿日期 2019/10/22
修改稿日期
网络出版日期
作者单位点击查看
备注陈思敏,助理工程师,学士,研究方向为食品安全检测,345871930@qq.com
引用该论文: CHEN Simin,WU Yingxuan,LAN Cao,ZOU You,XIE Minling. UHPLC-MS/MS Determination of Residual Amounts of Benzimidazoles and Its Metabolites in Dairy Products[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(5): 553~564
陈思敏,吴映璇,蓝草,邹游,谢敏玲. 超高效液相色谱-串联质谱法测定乳制品中苯并咪唑类药物及其代谢物的残留量[J]. 理化检验-化学分册, 2020, 56(5): 553~564
共有人对该论文发表了看法,其中:
人认为该论文很差
人认为该论文较差
人认为该论文一般
人认为该论文较好
人认为该论文很好
参考文献
【1】刘琪,朱馨乐,孙雷,等.高效液相色谱-串联质谱法检测猪肝中苯并咪唑类药物及其代谢物的残留量[J].中国兽药杂志, 2010,44(2):1-6.
【2】郭强,常孝勇.动物组织中苯并咪唑类药物检测的LC-MS/MS法研究[J].河南农业科学, 2012,41(2):152-156.
【3】汤娟,吴斌,景苏,等.高效液相色谱-串联质谱测定奶粉中3种苯并咪唑类药物残留[J].质谱学报, 2012,33(1):13-17.
【4】严寒,曾艳兵,罗林广.高效液相色谱法测定动物源性食品中苯并咪唑类药物残留的研究[J].黑龙江畜牧兽医, 2012(19):68-71.
【5】贾涛.液相色谱-串联质谱法检测牛奶中苯并咪唑类药物[J].中国乳业, 2015(9):54-59.
【6】张仟春,杨燕群,苏姚,等.固相微萃取/高效液相色谱联用分析食品中痕量苯并咪唑[J].分析测试学报, 2017,36(6):718-724.
【7】翟纹静,徐振东,陈娟.鸡肉中16种苯并咪唑及其代谢物残留量快速检测方法的研究[J].中国家禽, 2018,40(18):40-44.
【8】DOMÍNGUEZ-ÁLVAREZ J, MATEOS-VIVAS M, GARCÍA-GÓMEZ D, et al. Capillary electrophoresis coupled to mass spectrometry for the determination of anthelmintic benzimidazoles in eggs using a QuEChERS with preconcentration as sample treatment[J]. Journal of Chromatography A, 2013,1278:166-174.
【9】HOU X L, CHEN G, ZHU L, et al. Development and validation of an ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk[J]. Journal of Chromatography B, 2014,962:20-29.
【10】WANG Y Y, LI X W, ZHANG Z W, et al. Simultaneous determination of nitroimidazoles, benzimidazoles, and chloramphenicol components in bovine milk by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Food Chemistry, 2016,192:280-287.
【11】TEJADA-CASADO C, MORENO-GONZÁLEZ D, LARA F J, et al. Determination of benzimidazoles in meat samples by capillary zone electrophoresis tandem mass spectrometry following dispersive liquid-liquid microextraction[J]. Journal of Chromatography A, 2017,1490:212-219.
【2】郭强,常孝勇.动物组织中苯并咪唑类药物检测的LC-MS/MS法研究[J].河南农业科学, 2012,41(2):152-156.
【3】汤娟,吴斌,景苏,等.高效液相色谱-串联质谱测定奶粉中3种苯并咪唑类药物残留[J].质谱学报, 2012,33(1):13-17.
【4】严寒,曾艳兵,罗林广.高效液相色谱法测定动物源性食品中苯并咪唑类药物残留的研究[J].黑龙江畜牧兽医, 2012(19):68-71.
【5】贾涛.液相色谱-串联质谱法检测牛奶中苯并咪唑类药物[J].中国乳业, 2015(9):54-59.
【6】张仟春,杨燕群,苏姚,等.固相微萃取/高效液相色谱联用分析食品中痕量苯并咪唑[J].分析测试学报, 2017,36(6):718-724.
【7】翟纹静,徐振东,陈娟.鸡肉中16种苯并咪唑及其代谢物残留量快速检测方法的研究[J].中国家禽, 2018,40(18):40-44.
【8】DOMÍNGUEZ-ÁLVAREZ J, MATEOS-VIVAS M, GARCÍA-GÓMEZ D, et al. Capillary electrophoresis coupled to mass spectrometry for the determination of anthelmintic benzimidazoles in eggs using a QuEChERS with preconcentration as sample treatment[J]. Journal of Chromatography A, 2013,1278:166-174.
【9】HOU X L, CHEN G, ZHU L, et al. Development and validation of an ultra high performance liquid chromatography tandem mass spectrometry method for simultaneous determination of sulfonamides, quinolones and benzimidazoles in bovine milk[J]. Journal of Chromatography B, 2014,962:20-29.
【10】WANG Y Y, LI X W, ZHANG Z W, et al. Simultaneous determination of nitroimidazoles, benzimidazoles, and chloramphenicol components in bovine milk by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Food Chemistry, 2016,192:280-287.
【11】TEJADA-CASADO C, MORENO-GONZÁLEZ D, LARA F J, et al. Determination of benzimidazoles in meat samples by capillary zone electrophoresis tandem mass spectrometry following dispersive liquid-liquid microextraction[J]. Journal of Chromatography A, 2017,1490:212-219.
相关信息