Captiva EMR-Lipid技术结合UPLC-MS/MS快速测定牛羊产品中甲苯咪唑及其代谢物的残留量  

Rapid Determination of Mebendazole and Its Metabolites in Cattle and Sheep Products by Captiva EMR-Lipid Technology Combined with UPLC-MS/MS

作　　者：叶佳明 钟世欢 叶磊海 吴余欣 王京 YE Jiaming;ZHONG Shihuan;YE Leihai;WU Yuxin;WANG Jing(Zhejiang Gongzheng Testing Center,Inc,Hangzhou 310009,China;Zhejiang Key Laboratory of Food Safety,Hangzhou 310009,China)

机构地区：[1]浙江公正检验中心有限公司,浙江杭州310009 [2]浙江省食品安全重点实验室,浙江杭州310009

出　　处：《食品工业科技》2024年第3期277-283,共7页Science and Technology of Food Industry

摘　　要：建立了牛羊产品中甲苯咪唑及其代谢物羟基甲苯咪唑、氨基甲苯咪唑的通过式净化-超高效液相色谱-串联质谱测定的分析方法。样品经0.2%氨化乙腈溶液振荡提取,冷冻离心后,经Captiva EMR-Lipid小柱净化,直接进样分析。以安捷伦SB-C_(18)色谱柱(2.1 mm×100 mm,1.8μm)进行分离,以0.1%甲酸水和乙腈为流动相进行梯度洗脱,电喷雾正离子(ESI^(+))模式电离、多反应监测(MRM)模式进行检测,采用基质匹配标准工作曲线,内标法定量。结果表明,甲苯咪唑及其代谢物在0.2~50 ng/mL范围内线性良好,相关系数均大于0.999,甲苯咪唑及其代谢物的检出限(S/N>3)为0.3μg/kg,三水平的加标回收率在80.5%~108.0%之间,RSD为1.1%~5.8%。该方法操作简便、结果准确,克服了目前方法前处理繁琐、检测周期长等不足,适用于牛羊产品中甲苯咪唑及其代谢物残留量的快速检测。A method for detecting mebendazole and its metabolites in cattle and sheep products was established by EMRLipid-ultra-performance liquid chromatography-tandem mass spectrometry.The samples were first extracted by oscillation with 0.2%ammoniated acetonitrile solution,then freeze centrifugation,purified by Captiva EMR-Lipid column and directly analyzed by LC-MS/MS.The 3 kinds of mebendazole drugs were separated by SB-C_(18) column(2.1 mm×100 mm,1.8μm)and gradiently eluted with acetonitrile and 0.1%formic acid water solution as mobile phase.The detection of mebendazole drugs was performed by tandem mass spectrometry in electrospray ionization under multiple reactions monitoring(MRM)mode.Matrix matching standard working curve and internal standard method were used for quantification.The calibration curves for target compounds were linear over the range of 0.2~50 ng/mL with correlation coefficients larger than 0.999.The detection limits(S/N>3)of 3 kinds of mebendazole drugs were 0.3μg/kg.The recoveries of the 3 kinds of mebendazole drugs at three added levels were between 80.5%and 108.0%.The relative standard deviations were 1.1%~5.8%.The method overcame the current shortcomings of cumbersome preprocessing and long detection cycle,and it was simple in operation and accurate in results.The method was applicable to the rapid detection of mebendazole and its metabolites residues in cattle and sheep products.

关 键 词：甲苯咪唑 氨基甲苯咪唑 羟基甲苯咪唑 液相色谱-串联质谱法 固相萃取 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程]