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高效液相色谱-串联质谱法结合改良 QuEChERS 法同时测定荔枝和龙眼中七种农药及其代谢物残留

Simultaneous Determination of Seven Pesticides and Metabolite Residues in Litchi and Longan through High-Performance Liquid Chromatography-Tandem Mass Spectrometry with Modified QuEChERS.

机构信息

Institute of Plant Protection, Guangdong Academy of Agricultural Sciences, Key Laboratory of Green Prevention and Control on Fruits and Vegetables in South China Ministry of Agriculture and Rural Affairs, Guangdong Provincial Key Laboratory of High Technology for Plant Protection, Guangzhou 510640, China.

Guangdong Engineering Research Center for Insect Behavior Regulation, South China Agricultural University, Guangzhou 510642, China.

出版信息

Molecules. 2022 Sep 5;27(17):5737. doi: 10.3390/molecules27175737.

DOI:10.3390/molecules27175737
PMID:36080501
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC9457611/
Abstract

This study established a QuEChERS high-performance liquid chromatography/tandem triple-quadrupole mass spectrometry method for determining azoxystrobin, pyraclostrobin, picoxystrobin, difenoconazole, chlorantraniliprole, imidacloprid, and cyantraniliprole and its metabolite (IN-J9Z38) in litchi and longan, and applied this method to the real samples. The residues in samples were extracted with acetonitrile and purified with nano-ZrO2, C18, and PSA. The samples were then detected with multireactive ion monitoring and electrospray ionization in the positive ion mode and quantified using the external matrix-matched standard method. The results showed good linearities for the eight analytes in the range of 1−100 μg/L, with correlation coefficients (r2) of >0.99. The limit of quantification was 1−10 μg/kg, and the limit of detection was 0.3−3 μg/kg. Average recovery from litchi and longan was 81−99%, with the relative standard deviation of 3.5−8.4% at fortified concentrations of 1, 10, and 100 μg/kg. The developed method is simple, rapid, efficient, and sensitive. It allowed the rapid screening, monitoring, and confirming of the aforementioned seven pesticides and a metabolite in litchi and longan.

摘要

本研究建立了 QuEChERS 高效液相色谱/串联三重四极杆质谱法,用于测定荔枝和龙眼中的嘧菌酯、吡唑醚菌酯、肟菌酯、烯唑醇、氯虫苯甲酰胺、噻虫啉和氰氟虫腙及其代谢物(IN-J9Z38),并将该方法应用于实际样品。样品中的残留物质用乙腈提取,并用纳米-ZrO2、C18 和 PSA 进行纯化。然后,采用多反应监测和电喷雾电离在正离子模式下进行检测,并采用外标基质匹配法定量。结果表明,八种分析物在 1-100 μg/L 范围内具有良好的线性关系,相关系数(r2)均大于 0.99。定量限为 1-10 μg/kg,检测限为 0.3-3 μg/kg。荔枝和龙眼中平均回收率为 81-99%,在 1、10 和 100 μg/kg 的加标浓度下,相对标准偏差为 3.5-8.4%。该方法简单、快速、高效、灵敏,可用于荔枝和龙眼中上述七种农药及其代谢物的快速筛选、监测和确证。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/30a97173d895/molecules-27-05737-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/1fc914af25dc/molecules-27-05737-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/2cea29d0ee11/molecules-27-05737-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/8d9d6d1ac2e6/molecules-27-05737-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/30a97173d895/molecules-27-05737-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/1fc914af25dc/molecules-27-05737-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/2cea29d0ee11/molecules-27-05737-g002.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/8d9d6d1ac2e6/molecules-27-05737-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3503/9457611/30a97173d895/molecules-27-05737-g004.jpg

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