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

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 T_(3)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1.0~50μg/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-氨基砜、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。

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 T_(3)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 1.0~50μg/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.