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食品研究与开发:2024,45(11):178-184
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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
(湖南省产商品质量检验研究院,湖南长沙 410007)
Rapid Determination of Residues of Six Herbicides in Partly Animal-derived Foods by QuEChERSUltra High-performance Liquid Chromatography-Tandem Mass Spectrometry
(Hunan Province Produce Commodity Quality Testing&Research Institute,Changsha 410007,Hunan,China)
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投稿时间:2024-01-22    
中文摘要: 为建立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,C18 粉和无水硫酸镁净化,采用Hypersil GOLDTM C18 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0.2~20.0 μg/L、氯丙嘧啶酸和氯氨吡啶酸在1.0~50.0 μg/L线性关系良好,相关系数(R2)均大于0.995,方法的定量限均为1.0 μg/kg;以牛肉、鸡蛋、猪肝、牛奶为基质,6 种除草剂在1.0、5.0、20.0 μg/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%。
Abstract: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 C18 powder and anhydrous magnesium sulfate,separated using a Hypersil GOLDTM C18 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 relationships of saflufenacil,bentazone,cycloxydim,and pinoxaden were good in the range of 0.2 μg/L to 20.0 μg/L,and aminopyralid and aminocyclopyrachlor in the range of 1.0 μg/L to 50.0 μg/L,with correlation coefficients(R2)all greater than 0.995.The limit of quantification(LOQ)of the method was 1.0 μg/kg.For beef,chicken eggs,pork liver,and cow milk as matrices,the recovery rates of the six herbicides at three spiked levels(1.0,5.0 μg/kg,and 20.0 μg/kg)were 72.8% to 98.5%,with relative standard deviations of 1.13% to 6.28%.
文章编号:202411022     中图分类号:    文献标志码:
基金项目: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)
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