QuEChERS-超高效液相色谱-串联质谱法快速测定部分动物源性食品中6种除草剂残留  

Rapid Determination of Residues of Six Herbicides in Partly Animal‐derived Foods by QuEChERS Ultra High‐performance Liquid Chromatography‐Tandem Mass Spectrometry

作　　者：肖泳 曾小明 李政 袁列江 邓航 王淑霞 潘照 XIAO Yong;ZENG Xiaoming;LI Zheng;YUAN Liejiang;DENG Hang;WANG Shuxia;PAN Zhao(Hunan Province Produce Commodity Quality Testing&Research Institute,Changsha 410007,Hunan,)

机构地区：[1]湖南省产商品质量检验研究院,湖南长沙410007

出　　处：《食品研究与开发》2024年第11期178-184,共7页Food Research and Development

基　　金：湖南省自然科学基金科市联合项目(2022JJ90031);湖南省市场监督管理局科技计划项目(2022KJJH51)。

摘　　要：为建立Qu ECh ERS-超高效液相色谱-串联质谱法快速测定部分动物源性食品中6种常见除草剂残留的检测方法,将畜禽肉及内脏、蛋类、生乳等样品经体积分数为10%的甲酸乙腈溶液提取,C_(18)粉和无水硫酸镁净化,采用Hypersil GOLD^(TM)C_(18)色谱柱分离,以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱,基质匹配标准曲线外标法定量。结果表明,苯嘧磺草胺、灭草松、噻草酮、唑啉草酯在0.2~20.0μg/L、氯丙嘧啶酸和氯氨吡啶酸在1.0~50.0μg/L线性关系良好,相关系数(R^(2))均大于0.995,方法的定量限均为1.0μg/kg;以牛肉、鸡蛋、猪肝、牛奶为基质,6种除草剂在1.0、5.0、20.0μg/kg 3个加标水平下的回收率为72.8%~98.5%,相对标准偏差为1.13%~6.28%。This study established an detection method for the rapid determination of residues of six common herbicides in animal-derived foods using QuEChERS-ultra high-performance liquid chromatography-tandem mass spectrometry.Samples such as meat and offal of livestock and poultry,eggs,and raw milk were extracted with a 10%formic acid acetonitrile solution by volume.The extracts were purified with C_(18) powder and anhy-drous magnesium sulfate,separated using a Hypersil GOLD^(TM) C_(18) chromatographic column,and eluted with a gradient of methanol and 0.1%formic acid aqueous solution as the mobile phase.Quantification was performed using the matrix-matched standard curve external standard method.The results showed that the linear relation-ships of saflufenacil,bentazone,cycloxydim,and pinoxaden were good in the range of 0.2μg/L to 20.0μg/L,and aminopyralid and aminocyclopyrachlor in the range of 1.0μg/L to 50.0μg/L,with correlation coefficients(R^(2))all greater than 0.995.The limit of quantification(LOQ)of the method was 1.0μg/kg.For beef,chicken eggs,pork liver,and cow milk as matrices,the recovery rates of the six herbicides at three spiked levels(1.0,5.0μg/kg,and 20.0μg/kg)were 72.8%to 98.5%,with relative standard deviations of 1.13%to 6.28%.

关 键 词：动物源性食品 除草剂 超高效液相色谱-串联质谱 QUECHERS 快速测定 

分 类 号：O657.63[理学—分析化学] TS207.3[理学—化学]