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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 被引量:15

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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摘要 目的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。 Objective 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.
出处 《中国食品卫生杂志》 2016年第4期471-476,共6页 Chinese Journal of Food Hygiene
关键词 全自动固相萃取 气相色谱-三重四级杆串联质谱 农药残留 蔬菜 食品污染物 食品安全 Automatic solid-phase extraction gas chromatography coupled with triple quadrupole mass spectrometry pesticide residues vegetable food contaminant food safety
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