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基于晶体生长法的磁性石墨化炭黑结合高分辨质谱法用于筛选党参和当归中 300 种农药残留。

Magnetic graphitized carbon black based on crystal growth method combined with high-resolution mass spectrometry for screening of 300 pesticide residues in Radix Codonopsis and Angelica sinensis.

机构信息

Chinese Academy of Inspection and Quarantine, Beijing, PR China; Key Laboratory of Pesticide and Veterinary Drug Monitoring for State Market Regulation/Lanzhou Institute for Food and Drug control, Gansu, PR China.

Chinese Academy of Inspection and Quarantine, Beijing, PR China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2023 Jul 15;1226:123788. doi: 10.1016/j.jchromb.2023.123788. Epub 2023 Jun 10.

Abstract

In this study, a high-throughput method for analyzing 300 pesticide residues in Radix Codonopsis and Angelica sinensis was established by liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-Q-TOF/MS) using iron tetroxide loaded graphitized carbon black magnetic nanomaterial (GCB/FeO) as the purification material. It was optimized that saturated salt water and 1 % acetate acetonitrile were used as the extraction solution, then the supernatant was purified with 2 g anhydrous CaCl and 300 mg GCB/FeO. As a result, 300 pesticides in Radix Codonopsis and 260 in Angelica sinensis achieved satisfactory results. The limits of quantification of 91 % and 84 % of the pesticides in Radix Codonopsis and Angelica sinensis reached 10 μg/kg, respectively. The matrix-matched standard curves ranging from 10 to 200 μg/kg were established with correlation coefficients (R) above 0.99. The pesticides meeting SANTE/12682/2021 accounted for 91.3 %, 98.3 %, 100.0 % and 83.8 %, 97.3, 100.0 % of the total pesticides added in Radix Codonopsis and Angelica sinensis respectively, which were spiked at 10, 20,100 μg/kg. The technique was applied to screen 20 batches of Radix Codonopsis and Angelica sinensis. Five pesticides were detected, three of which were prohibited according to the Chinese Pharmacopoeia (2020 Edition). The experimental results showed that GCB/FeO coupled with anhydrous CaCl exhibited good adsorption performance and could be used for sample pretreatment of various pesticide residues in Radix Codonopsis and Angelica sinensis. Compared with the reported methods for determining pesticides in traditional Chinese medicine (TCM), the proposed method has the advantage of less time-consuming in the clean-up procedure. Furthermore, as a case study on root TCM, this approach may serve as a reference for other TCM.

摘要

本研究建立了一种基于铁四氧化三负载石墨化碳黑磁性纳米材料(GCB/FeO)的高效液相色谱-四极杆飞行时间质谱(LC-Q-TOF/MS)高通量分析党参和当归中 300 种农药残留的方法。优化了饱和盐水和 1%乙酸乙腈作为提取溶液,然后用 2 g 无水氯化钙和 300 mg GCB/FeO 对上清液进行纯化。结果,党参中 300 种农药和当归中 260 种农药均取得了满意的效果。党参和当归中 91%和 84%的农药定量限均达到 10μg/kg。建立了基质匹配标准曲线,浓度范围为 10-200μg/kg,相关系数(R)均大于 0.99。党参和当归中添加的总农药分别有 91.3%、98.3%、100.0%和 83.8%、97.3%、100.0%符合 SANTE/12682/2021 要求,党参和当归分别在 10、20、100μg/kg 添加水平下添加农药,回收率为 80.2%-114.1%。该技术应用于 20 批党参和当归的筛选,检测到 5 种农药,其中 3 种根据《中国药典》(2020 年版)规定为禁用。实验结果表明,GCB/FeO 与无水氯化钙结合具有良好的吸附性能,可用于党参和当归中各种农药残留的样品预处理。与传统中药(TCM)中农药残留检测的报道方法相比,该方法在净化步骤中耗时更少。此外,作为中药根的案例研究,该方法可为其他中药提供参考。

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