应用QuEChERS技术与气相色谱-串联质谱法同时检测榛子中70种农药残留
Simultaneous determination of 70 pesticide residues in hazelnuts by QuEChERS combined with gas chromatography-tandem mass spectrometry
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摘要: 使用乙腈(含1%乙酸)提取样品中的农药,经N-丙基乙二胺(PSA)粉及碳十八粉混合净化,再经气相色谱-三重四级杆串联质谱分析.建立榛子中70种农药残留同时检测的QuEChERS-气相色谱-串联质谱分析方法.方法结果表明,70种农药在线性范围内(5-100 μg·L-1)相关系数均大于0.9915.方法检出限范围为0.001-1.466 μg·kg-1,方法定量限范围为0.003-4.888 μg·kg-1.当加标水平为75 μg·kg-1时,其回收率在70.00%-94.73%之间,相对标准偏差(RSD)在0.29%-11.80%之间.本方法具有操作简单、快速、灵敏的特点,适用于榛子中农药多残留的检测.Abstract: To establish a QuEChERS-gas chromatography-tandem mass spectrometric method for simultaneous determination of 70 pesticide residues in hazelnuts. The target pesticides in the hazelnut were extracted with acetonitrile and purified with N,N-diisopropylamino ethylamine primary secondary amine (PSA) and C18, then analyzed by gas chromatography-tandem mass spectrometry. The result implied that all the linear relationships were good with the correlation coefficients all greater than 0.9915. The limits of detection of the method were 0.001-1.466 μg·kg-1, the limits of quantification were 0.003-4.888 μg·kg-1. When the 70 kinds of pesticide residues adding standard level was 75 μg·kg-1, the recovery rates and the relative standard deviation (RSD) of the method were from 70.00%-94.73% and 0.29%-11.80%, respectively. The method is convenient, quick, sensitive, and it is suitable to the analysis of multi pesticide residues in hazelnuts.
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Key words:
- hazelnuts /
- QuEChERS /
- GC-MS/MS /
- pesticide residue
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[1] CHERTA L, BELTRAN J, LÍPEZ F, et al. Application of fast gas chromatography-mass spectrometry in combination with the quechers method for the determination of pesticide residues in fruits and vegetables[J]. Food Analytical Methods, 2013, 6(4):1170-1187. [2] 李萍萍, 程景, 乐渊. 气相色谱-三重四极杆串联质谱法测定含硫蔬菜中46种农药残留量[J]. 分析测试学报, 2015, 34(4):421-427. LI P P,CHENG J,YUE Y.Determination of 46 pesticide residues in sulfur-containing vegetables using solid-phase extraction and gas chromatography-triple quadrupole mass spectrometry[J]. JournalofInstrumentalAnalysis,2015,34(4):421-427(in Chinese).
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