QuEChERS-液相色谱-串联质谱法测定黄瓜和苹果中7种农药残留量及其风险评估

Determination of 7 kinds of pesticide residues in Cucumis sativus L. and Malus pumila Mill. by QuEChERS-liquid chromatography-tandem mass spectrometry and risk assessment

中文关键词:  QuEChERS  液相色谱-串联质谱法  果蔬  农药残留  风险评估

英文关键词:QuEChERS  liquid chromatography-tandem mass spectrometry  fruits and vegetables  pesticide residues  risk assessment

中文摘要:

      目的 建立QuEChERS前处理结合液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)同时测定黄瓜和苹果中7种农药残留的方法及其风险评估。方法 对果蔬样品进行均质, 采用乙腈作为提取溶剂, 氯化钠和无水乙酸钠作为盐析试剂, 取其上清液通过N-丙基乙二胺(primary secondary amines, PSA)、石墨化炭黑(graphitized carbon black, GCB)和无水硫酸镁试剂进行净化, 使用Agilent Poroshell 120 EC-C18色谱柱, 以梯度洗脱的方式在11 min内对7种不同类别的农药进行检测分析。通过计算估计每日摄入量(estimate dietary intake, EDI)和危害商(hazard quotient, HQ)来评估食用黄瓜和苹果可能存在的潜在健康风险。结果 7种农药在5~500 μg/L范围内具有良好的线性关系, 相关系数均＞0.99。其检出限为0.5~1.0 μg/kg, 定量限为2.0~4.0 μg/kg。在低、中、高3个不同加标水平下的平均回收率为71.0%~118.8%, 相对标准偏差为3.1%~12.7%。同时根据每日允许摄入量(acceptable daily intake, ADI)评估的单个农药的HQ值远远小于1, 其风险在可接受的范围内。结论 该方法具有较高的准确度、精密度和灵敏度, 适用于同时测定果蔬中多类别农药的残留。此外, 本研究中风险评估结果表明黄瓜和苹果中农药残留对人们健康风险在可接受的范围内。

英文摘要:

      Objective To establish a method for the simultaneous determination and risk assessment of multi-class pesticide residues in Cucumis sativus L. and Malus pumila Mill. using QuEChERS-liquid chromatography-tandem mass spectrometry. Methods Fruit and vegetable samples were homogenized using acetonitrile as extraction solvent, sodium chloride and anhydrous sodium acetate as salting-out agent, and the supernatant was taken and purified by primary secondary amines (PSA), graphitized carbon black (GCB) and anhydrous magnesium sulfate reagent, and 7 kinds of pesticides were analyzed in 11 min using an Agilent Poroshell 120 EC-C18 column with gradient elution. The potential health risks associated with the consumption of Cucumis sativus L. and Malus pumila Mill. were assessed by calculating the estimated daily intake the estimated dietary intake (EDI) and hazard quotient (HQ). Results The 7 kinds of pesticides exhibited satisfactory linearity within the range of 5?500 μg/L, with correlation coefficients more than 0.99. The limits of detection were 0.5?1.0 μg/kg and the limits of quantification were 2.0?4.0 μg/kg. The average recoveries ranged from 71.0% to 118.8% at three different spiked levels, with the relative standard deviations ranging from 3.1% to 12.7%. Concurrently, the HQ values of individual pesticides evaluated from the acceptable daily intake (ADI) were found to be less than 1, and their risks were within acceptable limits. Conclusion The method exhibits high accuracy, precision, and sensitivity, and is suitable for the simultaneous determination of multi-class pesticide residues in fruit and vegetable samples. Furthermore, the risk assessment results of this study demonstrated that the health risk to individuals from pesticide residues in Cucumis sativus L. and Malus pumila Mill. is within acceptable limits.