固相萃取-超高效液相色谱-串联质谱同时测定乳制品中的苯并咪唑类药物及其代谢物残留量
Simultaneous Determination of Benzimidazoles and Their Metabolites Residues in Dairy Products by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
乔勇升 1王萍 1黄银波 1冯寅洁 1蔡霞 1张占林 1陈伟1
作者信息
- 1. 泰州市食品检验院,江苏省市场监管重点实验室(特医食品风险识别及关键分析技术),江苏泰州 225300
- 折叠
摘要
建立了乳制品中苯并咪唑类药物及其代谢物固相萃取-超高效液相色谱-串联质谱的分析方法.样品经含0.2％甲酸的乙腈提取后离心,上清液使用固相萃取柱进行净化,UPLC HSS T3色谱柱分离,电喷雾正离子模式下多反应监测(Multiple Reaction Monitoring,MRM)测定.结果显示,在1.0～50 pg/L范围内的线性相关系数r≥0.995(除三氯苯达唑为 0.9578),方法检出限(Limit of Detection,LOD)(S/N=3)为 0.002 mg/kg(除阿苯达唑-2-氦基砜、噻苯达唑和噻苯咪唑-5-羟基为0.003 mg/kg),方法定量限(Limit of Quantitation,LOQ)(S/N=10)为0.005 mg/kg(除阿苯达唑-2-氨基砜、噻苯达唑和噻苯咪唑-5-羟基为0.010 mg/kg).在0.005、0.01、0.05 mg/kg三个加标水平下回收率在62.5％～117.6％之间,相对标准偏差RSD在1.92％～12.17％之间.该方法操作简单、灵敏度高,适用于乳制品中苯并咪唑类药物及其代谢物的定量分析.
Abstract
A method for the simultaneous determination of benzimidazoles and their metabolites in dairy products was established using ultra high performance liquid chromatography-tandem mass spectrometry(MS).After extracting the samples with acetonitrile containing 0.2％formic acid,the extracts were centrifuged and purified by solid phase extraction column,and then separated by UPLC HSS T3 chromatographic column,determined in multi reaction monitoring(MRM)method with a positive ESI mode.The results showed that the linear correlation coefficient(r)within the range of 1.0～50 pg/L was greater than 0.995(except for triclabendazole,which was 0.9578).The method had a limit of detection(LOD)(S/N=3)of 0.002 mg/kg(except for albendazole-2-aminosulfone,thiabendazole,and thiabendazole-5-hydroxy,which were 0.003 mg/kg).The limit of quantitation(LOQ)(S/N=10)was 0.005 mg/kg(except for albendazole-2-aminosulfone,thiabendazole,and thiabendazole-5-hydroxy,which were 0.010 mg/kg).The recoveries at three spiked levels of 0.005,0.01 and 0.05 mg/kg ranged from 62.5％to 117.6％,with relative standard deviations(RSD)between 1.92％and 12.17％.The method is simple to operate,highly sensitive,and suitable for the quantitative analysis of benzimidazoles and their metabolites in dairy products.
关键词
固相萃取/超高效液相色谱-串联质谱/苯并咪唑类药物及其代谢物/乳制品/残留量测定Key words
solid phase extraction/ultra-performance liquid chromatography-tandem mass spectrometry/benzimidazoles and their metabolites/dairy products/determination of residue引用本文复制引用
基金项目
江苏省市场监督管理局科技项目(KJ21125052)
出版年
2024
国家科技期刊平台
NSTL
万方数据