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QuEChERS-冷冻诱导液液萃取/液相色谱-高分辨质谱法测定蔬菜水果中77种农药残留
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作者单位
毕 军,任 君,赵云峰,陈达炜 1. 国家食品安全风险评估中心/卫生部食品安全风险评估重点实验室北京 1000212. 盘锦检验检测中心 辽宁 盘锦 1240003. 乌海市检验检测中心内蒙古 乌海 016000 
基金项目:国家重点研发计划(2018YFC1602402);国家自然科学基金项目(21607035)
中文摘要:基于QuEChERS-冷冻诱导液液萃取(CI-LLE)技术,建立了蔬菜水果中77种农药残留的超高效液相色谱-高分辨质谱检测方法。样品经常规QuEChERS方法提取、盐析和净化后,进一步以40%乙腈-水溶液对77种农药进行CI-LLE富集和净化。仪器分析以水-甲醇(两相中均含0.1%甲酸和4 mmol/L甲酸铵)为流动相进行梯度洗脱,C18色谱柱(2.6 μm,2.1 mm × 150 mm)分离,高分辨质谱以时间分段全扫描模式采集,内标法定量。结果显示,77种农药在一定浓度范围内呈良好的线性关系(r2 > 0.99);方法检出限为0.02~0.20 μg/kg,定量下限为0.05~0.50 μg/kg。空白样品在4个不同加标水平的回收率为70.8%~119%,相对标准偏差(RSD)为0.70%~15%。该方法操作简单,重现性好,能降低基质效应对农残检测的影响,具有较高的灵敏度、准确度和精密度,符合农药多残留检测技术的要求,已应用于实际样品中农药残留的定性和定量分析。
中文关键词:农药残留  冷冻诱导液液萃取  高分辨质谱  蔬菜  水果  QuEChERS
 
Determination of 77 Pesticide Residues in Vegetables and Fruits by Liquid Chromatography-High Resolution Mass Spectrometry Coupled with QuEChERS and Cold Induced Liquid-Liquid Extraction
Abstract:Based on QuEChERS and cold induced liquid-liquid extraction(CI-LLE) technique, an analytical method for the determination of 77 pesticide residues in vegetables and fruits was developed by ultra-high performance liquid chromatography-high resolution mass spectrometry. The samples were extracted, salted out, and cleaned up by traditional QuEChERS method, and further enriched and cleaned up by CI-LLE technique using 40% acetonitrile-water solution. The chromatographic separation of pesticides was performed on a C18 column(2.1 mm × 150 mm, 2.6 μm) using water-methanol (containing 0.1% formic acid and 4 mmol/L ammonium formate for each) as mobile phases by gradient elution. The pesticides were analyzed by the high resolution mass spectrometry in full scan mode by time sediment, and quantified by internal standard method. Results showed that 77 pesticides had good linearity in the certain concentration ranges with relative coefficients(r2) larger than 0.99. The limits of detection and limits of quantitation were in the ranges of 0.02-0.20 μg/kg and 0.05-0.50 μg/kg, respectively. At four different spiked levels, the recoveries for pesticides in vegetables and fruits ranged from 70.8% to 119%, with relative standard deviations(RSDs) of 0.70%-15%. The method is simple and reproducible, and could be used to reduce matrix effect on the detection of pesticide residues with high sensitivity, accuracy, and precision. Therefore, it could meet the requirements for multi-residue detection of pesticides, and be applied to the qualitative and quantitative determination of pesticides in real samples.
Key Words:pesticide residues  cold induced liquid-liquid extraction  high resolution mass spectrometry  vegetables  fruits  QuEChERS
引用本文:毕 军,任 君,赵云峰,陈达炜.QuEChERS-冷冻诱导液液萃取/液相色谱-高分辨质谱法测定蔬菜水果中77种农药残留[J].分析测试学报,2021,40(9):1318-1327.
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