同位素稀释-高效液相色谱-线性离子阱质谱法测定总膳食乳类样品中8种三嗪类农药

doi:10.16431/j.cnki.1671-7236.2018.10.035

《中国畜牧兽医》 ›› 2018, Vol. 45 ›› Issue (10): 2960-2968.doi: 10.16431/j.cnki.1671-7236.2018.10.035

同位素稀释-高效液相色谱-线性离子阱质谱法测定总膳食乳类样品中8种三嗪类农药

李鹏^1,2, 杨欣^1,2, 苗虹^1,2, 李敬光^1,2, 赵云峰^1,2, 吴永宁^1,2

1. 国家食品安全风险评估中心, 北京 100021;
2. 卫生部食品安全风险评估重点实验室, 北京 100021

修回日期:2018-05-15 出版日期:2018-10-20 发布日期:2018-10-20
通讯作者: 吴永宁 E-mail:wuyongning@cfsa.net.cn
作者简介:李鹏(1985-),男,山东威海人,博士,研究方向:动物性食品卫生学,E-mail:lipeng_cau@163.com
基金资助:
973国家计划"食品加工过程安全性评价及危害物风险评估"（2012CB720804）；食品污染监测与风险评估技术合作研究（2011DF31770）

Simultaneous Determination of 8 Triazine Pesticides in Milk and Dairy Products from Total Diet by Isotope Dilution-High Performance Liquid Chromatography-Linear Ion Trap Mass Spectrometry

LI Peng^1,2, YANG Xin^1,2, MIAO Hong^1,2, LI Jingguang^1,2, ZHAO Yunfeng^1,2, WU Yongning^1,2

1. China National Center For Food Safety Risk Assessment, Beijing 100021, China;
2. Key Laboratory of Food Safety Risk Assessment, Ministry of Health, Beijing 100021, China

Revised:2018-05-15 Online:2018-10-20 Published:2018-10-20

摘要/Abstract

摘要：

本试验旨在建立用同位素稀释-高效液相色谱-串联线性离子阱质谱法（HPLC-LIT-MS）同时测定总膳食乳类样品中8种三嗪类农药的检测方法。在中国144个采样点采集总膳食乳类样品，在待测样品中加入氘代同位素内标，用乙腈经超声提取，凝胶渗透色谱（GPC）净化。以乙腈和含10 mmol/L甲酸铵和0.1%甲酸的水溶液为流动相，目标化合物经CAPCELL PAK CR 1：20色谱柱分离，采用电喷雾电离，选择反应监测（SRM）正离子模式监测二级子离子。以一一对应的氘代同位素为内标物，内标法定量，计算样品中三嗪类农药的含量。总膳食乳类样品中8种三嗪类农药的平均添加回收率为83.9%~103.3%；相对标准偏差为2.5%~9.1%；检出限（LODs）为0.003~0.300 μg/kg。结果表明，该方法精密度和准确度均满足总膳食乳类样品中8种三嗪类农药的膳食暴露评估要求。

关键词: 三嗪类农药; 总膳食乳类样品; 同位素稀释-高效液相色谱-串联线性离子阱质谱法(HPLC-LIT-MS); 凝胶渗透色谱

Abstract:

A method of the determination for 8 triazine pesticides in milk and dairy products from total diet was developed by isotope dilution-high performance liquid chromatography-linear ion trap mass spectrometry (HPLC-LIT-MS).Milk and dairy products from total diet were collected from 144 locations in China.Samples were ultrasonically extracted with acetonitrile,and then passed through gel permeation chromatography (GPC) to clear-up.The LC separation was performed on a CAPCELL PAK CR 1:20 column using acetonitrile and 10 mmol/L formic acid/0.1% formic aqueous solution as mobile phase.The ionization of the analytes was performed by electrospray mode.Selective reaction monitoring (SRM) was used for the monitoring of MS² transitions for each compound.The one-to-one internal standards were used for quantation.The average recoveries were in the range of 83.9% to 103.3%.The relative standard deviations were 2.5% to 9.1%.The limits of detection (LODs) were 0.003 to 0.300 μg/kg.In conclusion,the method was suitable for dietary exposure assessment of 8 triazine pesticides in milk and dairy products from total diet.

Key words: triazine pesticides; milk and dairy products from total diet; HPLC-LIT-MS; gel permeation chromatography

中图分类号:

TS207.5⁺3

李鹏, 杨欣, 苗虹, 李敬光, 赵云峰, 吴永宁. 同位素稀释-高效液相色谱-线性离子阱质谱法测定总膳食乳类样品中8种三嗪类农药[J]. 《中国畜牧兽医》, 2018, 45(10): 2960-2968.

LI Peng, YANG Xin, MIAO Hong, LI Jingguang, ZHAO Yunfeng, WU Yongning. Simultaneous Determination of 8 Triazine Pesticides in Milk and Dairy Products from Total Diet by Isotope Dilution-High Performance Liquid Chromatography-Linear Ion Trap Mass Spectrometry[J]. , 2018, 45(10): 2960-2968.

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同位素稀释-高效液相色谱-线性离子阱质谱法测定总膳食乳类样品中8种三嗪类农药

Simultaneous Determination of 8 Triazine Pesticides in Milk and Dairy Products from Total Diet by Isotope Dilution-High Performance Liquid Chromatography-Linear Ion Trap Mass Spectrometry

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