QuEChERS-气相色谱-串联质谱法测定蔬菜水果中48种农药及其代谢物残留量

Determination of 48 kinds of pesticide and its metabolite residues in vegetables and fruits by QuEChERS-gas chromatography- tandem mass spectrometry

中文关键词:  蔬菜  水果  农药残留  分散固相萃取  气相色谱-串联质谱法

英文关键词:vegetables  fruits  pesticide residues  dispersive solid phase extraction  gas chromatography-tandem mass spectrometry

中文摘要:

      目的 建立QuEChERS-气相色谱-串联质谱法(gas chromatography-tandem mass spectrometry, GC-MS/MS)检测蔬菜水果中48种农药及其代谢物残留的分析方法。方法 试样经乙腈提取、氯化钠盐析、无水硫酸镁脱水、柠檬酸钠和柠檬酸二钠作为缓冲保护剂、陶瓷均质子利于萃取过程的均匀性, 净化剂 (900 mg硫酸镁及150 mg PSA)涡旋净化后离心, 上清液滤膜过滤后GC-MS/MS测定。采用基质匹配线性-内标法定量。结果 方法的加标回收率在65.5%~114.2%之间, 精密度在2.2%~24.0%之间, 线性范围为5~ 500 μg/kg(r2＞0.99), 定量限为0.6~1.3 μg/kg。结论 该方法快速、准确、灵敏, 适合测定蔬菜水果中48种农药及代谢物残留量。

英文摘要:

      Objective To establish a method for the determination of 48 kinds of pesticide and its metabolite residues in vegetables and fruits by QuEChERS-gas chromatography-tandem mass spectrometry (GC-MS/MS). Methods The sample was extracted by acetonitrile, salted out by sodium chloride, dehydrated by anhydrous magnesium sulfate, using sodium citrate and disodium citrate as buffer protectants and ceramic homoproton was beneficial to the homogeneity of the extraction process. The sample was centrifuged after vortex purification with purification agents (900 mg magnesium sulfate and 150 mg PSA), and the supernatant was filtered by membrane filtration and determined by GC-MS/MS. Matrix matching linear internal standard method was used for quantitative analysis. Results The recoveries were 65.5%?114.2%, the precision was 2.2%?24.0%, the linear range was 5?500 μg/kg (r2>0.99), and the limit of quantification was 0.6?1.3 μg/kg. Conclusion The proposed method is fast, accurate and sensitive, which is suitable for detecting 48 kinds of pesticides and its metabolite residues in vegetables and fruits.