QuEChERS-高效液相色谱-串联质谱法测定春笋中4种农药残留
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(1.浙江省食品药品检验研究院,浙江 杭州 310052;2.浙江工业大学,浙江 杭州 310014)

作者简介:

周霞 女 主管药师 研究方向为食品分析和药物分析 E-mail:cpuzhouxia@163.com通信作者:┣┣(中)通信作者┫┫罗金文 男 主任药师 研究方向为食品分析和药物分析 E-mail:luojw31@163.com

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浙江省科技计划项目(2017C37013)


Determination of 4 pesticide residues in bamboo shoots by QuEChERS-high performance liquid chromatography-tandem mass spectrometry
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(1.Zhejiang Institution of Food and Drug Control,Zhejiang Hangzhou 310052,China;2.Zhejiang University of Technology,Zhejiang Hangzhou 310014,China)

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    摘要:

    目的 建立检测春笋中吡虫啉、茚虫威、辛硫磷和克百威4种农药的QuEChERS-高效液相色谱-串联质谱法。方法 前处理采用QuEChERS方法,乙腈为提取液,N-丙基乙二胺(PSA)为净化剂,结合液相色谱-质谱联用技术,正离子多反应监测(MRM)模式进行检测,外标法定量。结果 吡虫啉、茚虫威、辛硫磷和克百威4种农药在0.5~20.0 ng/ml范围呈良好的线性关系,相关系数(r2)均大于0.991,在4~40 μg/kg加标范围内,4种农药的回收率为72.4%~92.8%,精密度为1.5%~9.2%,方法的检出限为0.4 μg/kg,定量限为1.2 μg/kg。结论 建立了适用于检测春笋中吡虫啉、茚虫威、辛硫磷和克百威4种农药的QuEChERS-高效液相色谱-串联质谱法,该方法准确、灵敏、高效、简便。

    Abstract:

    Objective A simple and rapid QuEChERS-high performance chromatography-tandem mass spectrometric method was developed for the determination of 4 pesticides, imidacloprid, indoxacarb, phoxim and carbofuran, in bamboo shoots. Methods The residues were extracted from the bamboo shoots with acetonitrile and cleaned up with N-propyl ethylenediamine (PSA), then detected by liquid chromatography-tandem mass spectrometry under multiple reaction monitroring mode (MRM), and quantified by matrix-match calibration curves. Results The recoveries in samples were between 72.4%-92.8% at three spiked levels from 4 to 40 μg/kg, with relative standard deviations of 1.5%-9.2%(n=3). The limits of detection (LOD) of four pesticides were 0.4 μg/kg, while limits of quantification (LOQ) were 1.2 μg/kg. The linear ranges were 0.5-20.0 ng/ml and the correlation coefficients (r2) were above 0.991. Conclusion The method of QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry was accurate, sensitive, simple and convenient for the determination of the 4 pesticide residues, imidacloprid, indoxacarb, phoxim and carbofuran, in bamboo shoots.

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周霞,陈万勤,陈晶燕,朱雅青,朱炳祺,罗金文. QuEChERS-高效液相色谱-串联质谱法测定春笋中4种农药残留[J].中国食品卫生杂志,2018,30(5):486-490.

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  • 收稿日期:2018-05-04
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  • 在线发布日期: 2018-09-29
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