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分散固相萃取-气相色谱-串联质谱法测定蔬菜中多种农药残留 被引量:5

Quantification of pesticide residues in vegetables by gas chromatography with tandem mass spectrometry after dispersive-solid phase extraction
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摘要 目的:建立蔬菜中49种农药残留量的分散固相萃取-气相色谱-串联质谱(QuEChERS-GC-MS/MS)快速分析方法。方法:样品用乙酸乙酯匀浆提取后,经分散固相萃取法净化,采用气相色谱-串联质谱法用选择反应监测模式SRM进行测定,内标法定量。结果:在0.01 mg/L~10.0 mg/L范围内各农药线性相关系数均大于0.99,分别在菜心、青瓜和土豆中添加浓度水平为0.01 mg/kg和0.02 mg/kg的混标,平均回收率为70.8%~122.5%,方法的相对标准偏差为0.7%~7.8%(n=6)。所有农药的方法定量限均小于10μg/kg。结论:该法前处理简单快速、灵敏、准确,具有良好的回收率和稳定性,较好的解决了样品本底成分复杂的基质干扰,适用于蔬菜中多种农药残留的测定。 Objective: A quick method was developed for the determination of 49 pesticide residues in vegetables by gas chromatography with tandem mass spectrometry ( GC - MS/MS) after dispersive solid - phase extraction. Methods: The target compounds were extracted from the samples with ethyl acetate and the extracted solution was cleaned up using dispersive solid - phase extraction. The collected solution was analyzed by GC - MS/MS. The tar- get pesticides were confirmed by using timed SRM with two transitions of each targets and quantified by internal standard method. Results: In the linear range (0.01 mg/L -10.0 mg/L) of each pesticide, the correlation coeffi- cient was higher than 0.99. The average recoveries (spiked at the levels of 0.01 mg/kg,0.02 mg/kg) were from 70.8 % - 122.5 %. The relative standard deviations were from 0.7% - 7.8 % ( n = 6), and all limits of quantifica- tion(LOQs) were less than 10 μg/kg. Conclusion: The method is quick, sensitive, accurate, reproducible and suitable for the analysis of pesticide residues in vegetables.
出处 《中国卫生检验杂志》 北大核心 2013年第2期272-277,共6页 Chinese Journal of Health Laboratory Technology
基金 广东检验检疫局科技计划(2009GDK28) 中山市科技计划-农业科技攻关计划(20103A190)
关键词 分散固相萃取 气相色谱-串联质谱 农药残留 蔬菜 Dispersive - solid phase extraction Gas chromatography - tandem mass spectrometry ( GC - MS/MS) Pesticide residues Vegetables
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