基于QuEChERSEMR-Lipid技术结合气相色谱-串联质谱测定陈皮中153种农药残留

Determination of 153 pesticide residues in Pericarpium Citri Reticulatae by GC-MS/MS with QuEChERS EMR-Lipid approach

[背景]陈皮作为常用中药材,存在不容忽视的农药残留问题。目前陈皮中多农药残留的检测方法很少。[目的]基于新型除脂净化技术Qu ECh ERS EMR-Lipid建立陈皮中153种农药残留的气相色谱-串联质谱(GC-MS/MS)快速检测和准确定量方法。[方法]样品先用酸化乙腈提取,经过Qu ECh ERS EMR-Lipid前处理技术净化浓缩,以VF-1701MS石英毛细柱(30 m×0.25 mm×0.25μm)为分离柱,电子轰击电离源,采用气相色谱-串联质谱法测定,以基质匹配校准曲线内标法进行定量。[结果]153种农药在0.05~5 mg·kg^(-1)范围内均有良好的线性关系(r>0.997),在0.05、0.20、0.80 mg·kg^(-1)加标浓度下的平均回收率为71.3%~126.9%,相对标准偏差为1.1%~13.0%,方法的检出限为0.000 1~0.014 8 mg·kg^(-1),定量限为0.000 3~0.048 9 mg·kg^(-1)。[结论]基于Qu ECh ERS EMR-Lipid建立的GC-MS/MS方法适用于陈皮中多农药残留的快速测定及准确定量。本方法也可为基质类似中药的农药残留检测方法提供借鉴。

[Background]As a common traditional Chinese medicinal material,Pericarpium Citri Reticulatae(PCR) has pesticide residue problems that cannot be ignored.At present,there are few methods for testing hundreds of pesticide residues in PCR.[Objective]This study aims to establish a method for simultaneous determination of 153 kinds of pesticide residues in PCR by gas chromatography-tandem mass spectrometry (GC-MS/MS)combined with a novel lipid removal approach,Quick,Easy,Cheap,Effective,Rugged,and Safe(Qu ECh ERS) enhanced matrix removal (EMR)-Lipid.[Methods]The samples were extracted with acidified acetonitrile through Qu ECh ERS EMR-Lipid approach.GC-MS/MS analysis was performed on a VF-1701MS (30 m×0.25 mm×0.25μm)capillary column with electron impact source.Internal standard method for the matrix-matched calibration curve was used for quantification.[Results]The calibration curves for selected 153 pesticides exhibited good linearity (r>0.997)in the range of 0.05-5 mg·kg^(-1).The average recovery rates at 0.05,0.20,and 0.80 mg·kg^(-1) spiked levels were in the range of 71.3%-126.9%,and the relative standard deviations were in the range of 1.1%-13.0%.The limits of detection and the limits of quantification were 0.000 1-0.014 8 mg·kg^(-1)and 0.000 3-0.048 9 mg·kg^(-1),respectively.[Conclusion]The GC-MS/MS with Qu ECh ERS EMR-Lipid approach is suitable for rapid and accurate detection of multiple pesticide residues in PCR.The method can also provide a reference for the determination of pesticide residues in traditional Chinese medical plants with similar matrix.