凝胶渗透色谱-气相色谱-串联质谱法测定黄芪中20种禁用农药残留量

doi:10.14088/j.cnki.issn0439-8114.2025.10.026

摘要/Abstract

摘要： 基于凝胶渗透色谱-气相色谱-串联质谱（GPC-GC-MS/MS）技术,建立一种同时测定黄芪[Astragalus membranaceus (Fisch.) Bunge]中20种禁用农药残留的分析方法。结果表明,GPC的净化效果优于Florisil、N-Al₂O₃和C18,能有效去除脂质和色素等干扰物,显著降低基线噪声,提高目标物响应强度,改善检测灵敏度。该方法在0.01~0.50 μg/mL浓度范围内线性关系良好（R²>0.990 0）,检出限（LOD）为0.001~0.003 mg/kg,定量限（LOQ）为0.003~0.010 mg/kg。有机氯类农药回收率普遍高于有机磷类农药,2类农药的相对标准偏差（RSD）在中加标浓度（0.10 mg/kg）时最低,而在低加标浓度（0.01 mg/kg）和高加标浓度（0.50 mg/kg）时均有所升高,反映出基质效应和潜在干扰在不同浓度水平呈现差异化影响。该方法灵敏度良好,其LOD与LOQ均满足农药残留检测要求,不仅符合2020年版《中国药典》的相关规定,也适用于黄芪出口贸易中的农药残留筛查。该方法明显提高了农药的回收率,可有效去除脂溶性色素等基质干扰物,降低基质效应,适用于黄芪及其他高复杂性基质中药材的农药残留监测。

关键词: 凝胶渗透色谱, 气相色谱-串联质谱法, 黄芪[Astragalus membranaceus (Fisch.) Bunge], 禁用农药, 残留量

Abstract: Based on gel permeation chromatography-gas chromatography-tandem mass spectrometry (GPC-GC-MS/MS), an analytical method was established for the simultaneous determination of 20 banned pesticide residues in Astragalus membranaceus (Fisch.) Bunge. The results showed that the purification effect of GPC was superior to Florisil, N-Al₂O₃ and C18. GPC effectively removed interfering substances such as lipids and pigments, significantly reduced baseline noise, enhanced the response intensity of target compounds, and improved detection sensitivity. The method demonstrated good linearity in the concentration range of 0.01-0.50 μg/mL (R²>0.990 0), with limits of detection (LOD) of 0.001-0.003 mg/kg and limits of quantification (LOQ) of 0.003-0.010 mg/kg. The recovery rates of organochlorine pesticides were generally higher than those of organophosphorus pesticides. The relative standard deviations (RSD) of both types of pesticides were the lowest at the medium spiked concentration (0.10 mg/kg), but increased at both low (0.01 mg/kg) and high (0.50 mg/kg) spiked concentrations, reflecting differentiated impacts of matrix effects and potential interferences at different concentration levels. The method exhibited satisfactory sensitivity, with both LOD and LOQ meeting the requirements for pesticide residues detection. It not only complied with the relevant regulations of the 2020 edition of the Chinese Pharmacopoeia, but was also suitable for pesticide residues screening in the export trade of Astragalus membranaceus (Fisch.) Bunge. This method significantly improved pesticides recovery rates, effectively removed matrix interferences such as fat-soluble pigments, reduced matrix effects, and was applicable for pesticide residues monitoring in Astragalus membranaceus (Fisch.) Bunge and other traditional Chinese medicines with highly complex matrices.

Key words: gel permeation chromatography, gas chromatography-tandem mass spectrometry, Astragalus membranaceus (Fisch.) Bunge, banned pesticides, residues

中图分类号:

R284.1

钱叶会. 凝胶渗透色谱-气相色谱-串联质谱法测定黄芪中20种禁用农药残留量[J]. 湖北农业科学, 2025, 64(10): 171-178.

QIAN Ye-hui. Determination of 20 banned pesticide residues in Astragalus membranaceus (Fisch.) Bunge by gel permeation chromatography-gas chromatography-tandem mass spectrometry[J]. HUBEI AGRICULTURAL SCIENCES, 2025, 64(10): 171-178.

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