固相萃取－液相色谱－电喷雾串联质谱法测定鲜枣中14种农药残留

Determination of 14 Pesticide Residues in Fresh Jujube Using Liquid Chromatography Coupled with Electrospray Ionization Tandem Mass Spectrometry

DOI：10.3969/j.issn.1673-1689.2015.07.010

中文关键词: 固相萃取 鲜枣 液相色谱－串联质谱法 农药残留

英文关键词: solid phase extraction, fresh jujube, Liquid chromatography tandem mass spectrometry (LC-MS/MS), pesticides residues

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中文摘要:

选择强疏水性硅胶基质tC18柱为固相萃取净化柱，以电喷雾(ESI)为离子源，正离子多级反应离子监测(MRM)模式，建立了固相萃取－液相色谱－串联质谱法(HPLC-MS/MS)测定鲜枣中14种农药(包括有机磷杀虫剂、杀菌剂，有机杂环类杀虫剂和新型烟碱类杀虫剂)残留的分析方法。研究比较了不同提取溶剂的提取效果和不同固相萃取小柱的净化效果，同时优化了色谱分离条件和质谱条件。14种农药在10~500 μg/L(或1~50 μg/L)范围内线性相关，相关系数为0.996 3~0.999 9，方法的定量限为0.10~9.50 μg/kg。14种农药在鲜枣中3个水平添加质量浓度的的回收率在67.4%～116.8%，RSD为0.8%~14.8%之间。该方法操作简便，灵敏度、准确度和精密度均符合农药多残留检测技术要求，适用于鲜枣中14种农药多残留的检测。

英文摘要:

This study developed a method to identify 14 pesticides residues(including organic phosphorus insecticides，fungicides，organic heterocyclic pesticides and novel nicotine insecticide) in fresh jujube by solid-phase extraction and liquid chromatography coupled with electrospray ionization tandem(HPLC-MS/MS)，in which a strong hydrophobic silica bonded tC18 column was selected as the solid-phase extraction，electrospray ionization(ESI) was used as the ion source and positive ion multiple reaction monitoring(MRM) was set as the detection mode. The effects of different extraction solvents and solid-phase extraction columns were compared for the determination of 14 pesticides residues，and at the meanwhile the separation and detection conditions for the multiresidue analysis by chromatography and mass spectrometry were also optimized. A good linear relationship could be achieved for the detection of 14 pesticides in fresh jujube in the range of 10~500 μg/L (or 1~50 μg/L)，with the correlation coefficients of 0.996 3~0.999 9，the quantitation limits of 0.10~9.50 μg/kg，the recoveries of 67.4%~116.8% for 14 pesticides of three different concentrations，and RSD of 0.8%~14.8%. The optimized method，which is applicable to determine 14 pesticide residues in fresh jujube，meets the requirements of the multiresidue analysis with simple operation，good sensitivity，and high accuracy.

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