摘要
目的建立快速测定动物源性食品中喹乙醇代谢物(MQCA)的超高效液相色谱-串联质谱方法。方法样品采用蛋白酶酶解,乙酸乙酯提取,PAX固相萃取柱净化后进行UPLC-MS/MS分析。采用C18色谱柱分离,0.2%甲酸水-乙腈为流动相进行梯度洗脱;采用电喷雾-正离子多反应监测模式(MRM)检测,同位素内标法定量。结果超高效液相色谱串联质谱法测定动物源性食品中MQCA的方法平均回收率为88.5%~96.3%,相对标准偏差(RSD)为2.35%~6.25%(n=6)。MQCA的质量浓度为2.0~100.0 ng/ml时,线性关系良好(r>0.999),方法检出限为0.3μg/kg,定量限为1.2μg/kg。结论该方法在动物源性样品中具有较好的重现性与稳定性,能满足动物源性食品中喹乙醇代谢物MQCA残留分析的要求。
Objective To establish a method for the determination of 3-methyl-quinoxaline-2-carboxylic acid(MQCA)residuing in animal-derived food by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods After enzymatic hydrolysis,the samples were extracted with ethyl acetate,purified by PAX column and analyzed by UPLC-MS/MS.The separation was carried out on a C18 column with gradient elution using a mobile phase made up of0.2%formic acid water solution and acetonitrile.The electrospray positive ion multiple reaction monitoring(MRM)mode was used for detection,and isotope internal standard method was used for quantitation.Results The recovery rate of MQCA in animal-derived food by UPLC-MS/MS ranged from 88.5%to 96.3%.The relative standard deviation(RSD)ranged from 2.35%to 6.25%(n=6).When the mass concentration of MQCA was 2.0 to 100.0 ng/mL,the linear relationship was good(r>0.999).The detection limit and the quantitation limit was 0.3 and 1.2μg/kg,respectively.Conclusion The method has good reproducibility and stability in animal samples,and can meet the requirements of residue analysis of MQCA in animal-derived food.
作者
秦忠雪
任琳
何安琪
曾红燕
QIN Zhongxue;REN Lin;HE Anqi;ZENG Hongyan(Sichuan Center for Disease Control and Prevention,Chengdu 610041,Sichuan Province,China;West China School of Public Health/West China Fourth Hospital,Sichuan University,Chengdu 610041,Sichuan Province,China)
出处
《预防医学情报杂志》
CAS
2021年第12期1716-1721,共6页
Journal of Preventive Medicine Information
