高效液相色谱-串联质谱法测定鸡蛋中18种拟除虫菊酯类农药残留  

Determination of 18 pyrethroid pesticide residues in eggs by high performance liquid chromatography tandem mass spectrometry

作　　者：唐俗 卓程梆 朱雨田[1] 徐述龙 杜业刚[1] 罗淙岚 TANG Su;ZHUO Cheng-bang;ZHU Yu-tian;XU Shu-long;DU Ye-gang;LUO Cong-lan(Shenzhen Academy of Metrology and Quality Inspection,Shenzhen 518131,Guangdong,China;College of Food Science,South China Agricultural University,Guangzhou 510642,Guangdong,China)

机构地区：[1]深圳市计量质量检测研究院,广东深圳518131 [2]华南农业大学食品学院,广东广州510642

出　　处：《粮食与油脂》2025年第1期157-162,共6页Cereals & Oils

基　　金：国家重点研发计划(2022YFF0607900);国家市场监管总局科技计划项目(2023MK143)。

摘　　要：基于高效液相色谱-串联质谱法(LC-MS/MS)建立同时测定鸡蛋中18种拟除虫菊酯类农药残留的方法。样品经10 mL乙腈提取,弗罗里硅土固相萃取柱净化,以5 mmol/L乙酸铵溶液(A)-甲醇(B)作为流动相进行梯度洗脱,在离子源温度450℃时,采用多反应监测模式(MRM)进行定性定量分析。结果表明:18种拟除虫菊酯类农药在质量浓度5.00~200.00μg/L范围内,线性关系良好(r>0.995),检出限为5.00μg/kg,在20.0~100μg/kg加标水平下,回收率为79.2%~107%,相对标准偏差为0.707%~8.91%(n=3)。A method for simultaneous determination of 18 pyrethroid pesticide residues in eggs based on liquid chromatography tandem mass spectrometry(LC-MS/MS)was established.The sample was extrac-ted with 10 mL of acetonitrile and purified by a Florisil solid phase extraction column.A gradient elution was performed using 5 mmol/L ammonium acetate solution(A)-methanol(B)as the mobile phase.Qualitative and quantitative analysis was performed using multiple reaction monitoring mode(MRM)at ion source temperature of 450 C.The results showed that 18 pyrethroid pesticides had good linear rela-tionship(r>0.995)in the mass concentration range of 5.00-200.00μg/L.The limit of detection was 5.00μg/kg.At the spiked level of 20.0-100μg/kg,the recovery rate was 79.2%-107%,and the relative standard deviation was 0.707%-8.91%(n=3).

关 键 词：拟除虫菊酯 鸡蛋 高效液相色谱-串联质谱法(LC-MS/MS) 

分 类 号：TS207.53[轻工技术与工程—食品科学]