全自动固相萃取-气相色谱-三重四级杆质谱法检测蔬菜中23种农药残留
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(广州市疾病预防控制中心,广东 广州 510440)

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刘苗 女 理化检验技师 研究方向为食品安全风险监测E-mail:liumiao3368918@163.com

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Determination of 23 pesticide residues in vegetables by automatic solid phase extraction and gas chromatography coupled with triple quadrupole tandem mass spectrometry
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(Guangzhou Center for Disease Prevention and Control,Guangdong Guangzhou 510440,China)

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    摘要:

    建立蔬菜中有机磷类、拟除虫菊酯类共23种农药残留的分析方法。方法 样品加丙酮-二氯甲烷(1∶1,V/V)混合溶剂提取后经全自动固相萃取仪净化,采用气相色谱-三重四级杆串联质谱的多反应监测模式进行检测,内标法定量。结果 23种农药在0.05~0.80 mg/L范围内线性良好,相关系数均大于0.993 3;加标回收率在75.0%~105.5%之间;方法的检出限为0.02~0.70 mg/kg。在少量蔬菜样品中发现氯氰菊酯和氯氟氰菊酯超标。结论 该方法适用于蔬菜中多种农药残留的快速筛查测定。

    Abstract:

    A method was developed for the determination of 23 pesticides residues in vegetables, including organophosphorus and pyrethroid pesticides.Methods The pesticides in samples were extracted with acetone/dichloromethane(1∶1, V/V) and cleaned up by automatic solid-phase extraction. The collected solution was analyzed by triple quadrupole gas chromatography-tandem mass spectrometry using multiple reaction monitoring (MRM) with internal standard. Results It showed good linearity with the correlation coefficients above 0.993 3 in the range of 0.05-0.80 mg/L, the recoveries were in the range of 75.0%-105.5%, and the limits of detection(LOD) were 0.02-0.70 mg/kg. The residues of cypermethrin and cyhalothrin exceeded the standard in a few vegetable samples.Conclusion The method could be applied to the routine analysis for various pesticides in vegetable samples.

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刘苗,甘平胜,朱惠扬,李晓晶,杨荣,彭荣飞.全自动固相萃取-气相色谱-三重四级杆质谱法检测蔬菜中23种农药残留[J].中国食品卫生杂志,2016,28(4):471-476.

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  • 收稿日期:2015-11-02
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  • 在线发布日期: 2016-08-18
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