采用改进的QuEChERS方法结合超高效液相色谱-四极杆飞行时间质谱法测定辣椒中的12种新烟碱类农药。

Determination of twelve neonicotinoid pesticides in chili using an improved QuEChERS method with UPLC-Q-TOF/MS.

作者信息

Zhang Wenhua, Zhou Chunjie, Zhou Fenglan, Zalán Zsolt, Shi Hui, Kan Jianquan, Cai Tian, Chen Kewei

机构信息

College of Food Science, Southwest University, No. 2 Tiansheng Road, Beibei, Chongqing 400715, PR China; China-Hungary Cooperative Centre for Food Science, Chongqing 400715, PR China; Laboratory of Quality & Safety Risk Assessment for Agro-products on Storage and Preservation (Chongqing), Ministry of Agriculture and Rural Affairs of the People's Republic of China, Chongqing 400715, PR China; Chongqing Key Laboratory of Specialty Food Co-built by Sichuan and Chongqing, Chongqing 400715, PR China.

Key Laboratory of Condiment Supervision Technology for State Market Regulation, Chongqing Institute for Food and Drug Control, No. 1, Chunlan 2(nd) Road, Yubei District, Chongqing 401121, PR China.

出版信息

Food Chem. 2024 Sep 15;452:139463. doi: 10.1016/j.foodchem.2024.139463. Epub 2024 Apr 24.

DOI:10.1016/j.foodchem.2024.139463

PMID:38718451

Abstract

In this study, a QuEChERS method based on citrate was developed and utilized for the analysis of twelve neonicotinoid pesticides in fresh red chilies, fresh green chilies, and dried chilies, coupled with ultra-high performance liquid chromatography quadrupole time of flight mass spectrometry (UPLC-Q-TOF/MS). In the sample preparation, acetonitrile containing 1% formic acid was used as the extraction solvent. Anhydrous sodium sulfate replaced the traditional anhydrous magnesium sulfate for water removal, effectively eliminating the issues of salt caking. Graphitized carbon black, octadecyl silica, and primary secondary amine were used as cleaning agents. The method showed good sensitivity, with the limits of quantification below 0.03 mg/kg for fresh chilies and below 0.15 mg/kg for dried chilies. Values of matrix effects ranged from -19.5% to 8.4%, and the recovery was 86.9% - 105.2%. The analytical method provided an effective tool for the high throughput detection of neonicotinoid pesticide residues in multiple chili matrices.

摘要

在本研究中，开发了一种基于柠檬酸盐的QuEChERS方法，并将其用于分析新鲜红辣椒、新鲜绿辣椒和干辣椒中的12种新烟碱类农药，该方法与超高效液相色谱四极杆飞行时间质谱联用（UPLC-Q-TOF/MS）。在样品制备过程中，使用含1%甲酸的乙腈作为提取溶剂。用无水硫酸钠代替传统的无水硫酸镁进行脱水，有效消除了盐结块问题。使用石墨化炭黑、十八烷基硅胶和伯仲胺作为净化剂。该方法具有良好的灵敏度，新鲜辣椒的定量限低于0.03 mg/kg，干辣椒的定量限低于0.15 mg/kg。基质效应值范围为-19.5%至8.4%，回收率为86.9% - 105.2%。该分析方法为多种辣椒基质中新烟碱类农药残留的高通量检测提供了有效工具。