陆颖, 徐骞, 付强强, 刘桐, 蔡恩茂, 王文静. 基于QuEChERS EMR-Lipid技术结合气相色谱-串联质谱测定陈皮中153种农药残留[J]. 环境与职业医学, 2021, 38(7): 789-793. DOI: 10.13213/j.cnki.jeom.2021.21035
引用本文: 陆颖, 徐骞, 付强强, 刘桐, 蔡恩茂, 王文静. 基于QuEChERS EMR-Lipid技术结合气相色谱-串联质谱测定陈皮中153种农药残留[J]. 环境与职业医学, 2021, 38(7): 789-793. DOI: 10.13213/j.cnki.jeom.2021.21035
LU Ying, XU Qian, FU Qiangqiang, LIU Tong, CAI Enmao, WANG Wenjing. Determination of 153 pesticide residues in Pericarpium Citri Reticulatae by GC-MS/MS with QuEChERS EMR-Lipid approach[J]. Journal of Environmental and Occupational Medicine, 2021, 38(7): 789-793. DOI: 10.13213/j.cnki.jeom.2021.21035
Citation: LU Ying, XU Qian, FU Qiangqiang, LIU Tong, CAI Enmao, WANG Wenjing. Determination of 153 pesticide residues in Pericarpium Citri Reticulatae by GC-MS/MS with QuEChERS EMR-Lipid approach[J]. Journal of Environmental and Occupational Medicine, 2021, 38(7): 789-793. DOI: 10.13213/j.cnki.jeom.2021.21035

基于QuEChERS EMR-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

  • 摘要: 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QuEChERS 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QuEChERS EMR-Lipid前处理技术净化浓缩,以VF-1701MS石英毛细柱(30 m×0.25 mm×0.25 μm)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 1~0.0148mg·kg-1,定量限为0.0003~0.0489 mg·kg-1

    结论

    基于QuEChERS 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。

     

    Abstract: 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 (QuEChERS) enhanced matrix removal (EMR)-Lipid.

    Methods

    The samples were extracted with acidified acetonitrile through QuEChERS EMRLipid approach. GC-MS/MS analysis was performed on a VF-1701MS (30 m×0.25 mm×0.25 μm) 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 3-0.0489mg·kg-1, respectively.

    Conclusion

    The GC-MS/MS with QuEChERS 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.

     

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