食品与发酵工业 >

2024 , Vol. 50 >Issue 14: 270 - 278

DOI: https://doi.org/10.13995/j.cnki.11-1802/ts.038678

分析与检测

高效液相色谱-四级杆-飞行时间质谱法测定荔枝果实中29种农药多残留

  • 王思威 ,
  • 刘艳萍 ,
  • 丁晓波 ,
  • 李景明
展开
  • 1(广东省农业科学院 植物保护研究所, 农业农村部华南果蔬绿色防控重点实验室, 广东省植物保护新技术重点实验室,广东 广州,510640)
    2(泸州市农业科学研究院,四川 泸州,646000)
第一作者：博士,副研究员(丁晓波高级农艺师和李景明高级农艺师为共同通信作者,E-mail:dingxiaobo9@163.com;ljmljm126@126.com)

收稿日期: 2024-01-24

  修回日期: 2024-04-10

  网络出版日期: 2024-08-02

基金资助

国家荔枝龙眼产业技术体系项目(CARS-32);2021年省级乡村振兴战略专项省级项目(粤农农函[2021]21号);广东省农业科学院科技创新战略专项资金青年导师制(R2018QD-065);乡村振兴战略专项资金(农业科技能力提升)(2023TS-2-5,2023TS-2-3);广州市科技计划项目(2024E04J0596);广东省基础和应用基础研究基金(2022A1515110473)

收起

High-performance liquid chromatography-tandem quadrupole-time of flight-mass spectrometry for determination of 29 pesticides in litchi

  • WANG Siwei ,
  • LIU Yanping ,
  • DING Xiaobo ,
  • LI Jingming
Expand
  • 1(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)
    2(Luzhou Academy of Agricultural Sciences, Luzhou 646000, China)

Received date: 2024-01-24

  Revised date: 2024-04-10

  Online published: 2024-08-02

Fold

摘要

采用高效液相色谱-四极杆-飞行时间质谱技术结合优化的QuEChERS方法,建立了荔枝全果中29种农药的多残留检测分析方法。样品经乙腈提取,利用无水硫酸镁吸水和氯化钠盐析作用,进行离心分层后,取部分乙腈上清液进行净化,净化剂为无水MgSO4、N-丙基乙二胺吸附剂、石墨化碳黑吸附剂,采用电喷雾离子源正负离子交换扫描方式对29种农药数据信息进行采集。29种农药在质量浓度0.001~0.2 mg/L内具有较好线性相关性(相关系数R2均大于0.99), 在3个添加水平(0.01、0.1、0.5 mg/kg)下,29种农药的回收率均值为70.2%~102.4%,相对标准偏差为2.4%~6.2%。方法检出限为0.1～3 μg/kg,定量限为0.3～10 μg/kg。该方法具有操作便捷、回收率高和灵敏度高等特点,可用于同时快速测定荔枝中29种农药的多残留。

关键词： 荔枝; 29种农药; 高效液相色谱-四极杆-飞行时间质谱法

本文引用格式

王思威 , 刘艳萍 , 丁晓波 , 李景明 . 高效液相色谱-四级杆-飞行时间质谱法测定荔枝果实中29种农药多残留[J]. 食品与发酵工业, 2024 , 50(14) : 270 -278 . DOI: 10.13995/j.cnki.11-1802/ts.038678

Abstract

An analytical method was established for the simultaneous determination of 29 pesticides in litchi by a high-performance liquid chromatography-tandem quadrupole-time of flight-mass spectrometry (HPLC-Q-TOF/MS) technique combined with an optimized QuEChERS procedure.The samples were extracted by acetonitrile and the acetonitrile supernatant was collected for purification after salting-out (magnesium sulfate anhydrous and sodium chloride) and centrifugation.Under the optimized chromatographic and mass spectrometric conditions, the data were collected by electrospray ionization (ESI) sources in positive and negative ion modes.The calibration curves of 29 pesticides showed good linearity in a concentration range of 0.001-0.2 mg/L (R2>0.99).The average recoveries were 70.2%-102.4% at three spiked levels (0.01, 0.1, 0.50 mg/kg), while the relative standard deviations (RSD) were 2.4%-6.2%.The limits of detection and limits of quantification ranged from 0.1 μg/kg to 3 μg/kg and 0.3 μg/kg to 10 μg/kg, respectively.This method was a simple and efficient method with high sensitivity and precision and had practical value for the rapid detection of residues of 29 pesticides in litchi.

Key words： litchi; 29 pesticides; high performance liquid chromatography-tandem quadrupole-time-of-flight-mass spectrometry

参考文献

[1] IBRAHIM S R M, MOHAMED G A. Litchi chinensis: Medicinal uses, phytochemistry, and pharmacology[J]. Journal of Ethnopharmacology, 2015, 174:492-513.
[2] 庄丽娟, 邱泽慧. 2019年中国荔枝产业发展特征与政策建议[J]. 中国南方果树, 2021, 50(4):184-188.
ZHUANG L J, QIU Z H. Development characteristics and policy suggestions of litchi industry in China in 2019[J]. South China Fruits, 2021, 50(4):184-188.
[3] 陈厚彬, 苏钻贤, 杨胜男. 2023年全国荔枝生产调查与形势分析[J]. 中国热带农业, 2023(3):13-22.
CHEN H B, SU Z X, YANG S N. Investigation and analysis of the litchi production in China in 2023[J]. China Tropical Agriculture, 2023(3):13-22.
[4] 陈厚彬, 欧良喜, 李建国, 等. 新中国果树科学研究70年: 荔枝[J]. 果树学报, 2019, 36(10):1399-1413.
CHEN H B, OU L X, LI J G, et al. Fruit scientific research in New China in the past 70 years: Litchi[J]. Journal of Fruit Science, 2019, 36(10):1399-1413.
[5] 罗成, 周如, 杨春亮, 等. 国内外荔枝农药残留限量标准对比分析[J]. 中国南方果树, 2023, 52(3):236-241.
LUO C, ZHOU R, YANG C L, et al. Comparative analysis of the domestic and abroad standards of pesticide residue limit for Litchi[J]. South China Fruits, 2023, 52(3):236-241.
[6] 顾燕萍, 张树飞, 张惠云, 等. 我国荔枝龙眼中农药最大残留限量标准现状分析与建议[J]. 现代食品科技, 2024, 40(3):333-341.
GU Y P, ZHANG S F, ZHANG H Y, et al. Current standard staus analysis and suggestion for the maximum residue limits of pesticides in Chinese litchi and Longan[J]. Modern Food Science and Technology, 2024, 40(3):333-341.
[7] WANG Y D, FU Y W, WANG Y Y, et al. A comprehensive review on the pretreatment and detection methods of neonicotinoid insecticides in food and environmental samples[J]. Food Chemistry: X, 2022, 15:100375.
[8] CALZA P, GUARINO B, DAL BELLO F, et al. Integrated approach for the analysis of neonicotinoids in fruits and food matrices[J]. Food Chemistry, 2022, 372:131153.
[9] 平华, 赵天宇, 马智宏, 等. 分散固相萃取-超高效液相色谱-串联质谱法同时测定土壤中新烟碱类农药及其代谢物的残留量[J]. 理化检验-化学分册, 2023, 59(11):1276-1283.
PING H, ZHAO T Y, MA Z H, et al. Simultaneous determination of residues of neonicotinoid pesticides and their metabolites in soil by ultra-high performance liquid chromatography-tandem mass spectrometry with disperse solid phase extraction[J]. Physical Testing and Chemical Analysis (Part B (Chemical Analysis)), 2023, 59(11):1276-1283.
[10] 刘文, 车安怡, 王晋琦, 等. 固相萃取-电喷雾-离子迁移谱检测饮用水中三唑类农药残留[J]. 分析试验室, 2023, 1-7.
LIU W, CHE A Y, WANG J Q, et al. Determination of triazole pesticide residues in drinking water by solid phase extraction-electrospray ionization-ion mobility spectrometry [J]. Chinese Journal of Analysis Laboratory, 2023, 1-7.
[11] ZHENG Q, QIN D Q, YANG L P, et al. Dissipation and distribution of difenoconazole in bananas and a risk assessment of dietary intake[J]. Environmental Science and Pollution Research International, 2020, 27(13):15365-15374.
[12] KOWALSKA G, PANKIEWICZ U, KOWALSKI R. Estimation of pesticide residues in selected products of plant origin from Poland with the use of the HPLC-MS/MS technique[J]. Agriculture, 2020, 10(6):192.
[13] CAO J L, LIU X G, WU X H, et al. Uptake and distribution of difenoconazole in rice plants under different culture patterns[J]. Food Additives & Contaminants. Part A, Chemistry, Analysis, Control, Exposure & Risk Assessment, 2022, 39(6):1100-1108.
[14] ZHANG Q, CAO R, TANG T, et al. The integrated exposure assessment and potential risks of five organophosphorus pesticides in vegetables in Zhejiang, China (2018-2020)[J]. Environmental Science and Pollution Research, 2023, 30(11):28916-28924.
[15] PAÍGA P, SOUSA S, VERA J, et al. Multi-residue analysis of fifty pesticides in river waters and in wastewaters[J]. Environmental Science and Pollution Research International, 2021, 28(47):66787-66803.
[16] SIRAJ J, EJETA F. Analysis of pesticide residues in fruits and vegetables using gas chromatography-mass spectrometry: A case from West Omo and Bench-Sheko Zone, Southwest Ethiopia[J]. International Journal of Environmental Analytical Chemistry, 2024, 104(3):531-551.
[17] 吕佳宁, 许燕, 丁葵英, 等. 金属有机框架化合物ZIF-8基于QuEChERS-GC-MS/MS测定禽蛋中21种有机磷农药[J]. 中国食品添加剂, 2024, 35(1):8-15.
LYU J N, XU Y, DING K Y, et al. Determination of 21 organophosphorus pesticides in poultry eggs by metal organic framework compound ZIF-8 based on QuEChERS-GC-MS/MS[J]. China Food Additives, 2024, 35(1):8-15.
[18] NARENDERAN S T, MEYYANATHAN S N, BABU B. Review of pesticide residue analysis in fruits and vegetables. Pre-treatment, extraction and detection techniques[J]. Food Research International, 2020, 133:109141.
[19] DE O SILVA R, DE MENEZES M G G, DE CASTRO R C, et al. Efficiency of ESI and APCI ionization sources in LC-MS/MS systems for analysis of 22 pesticide residues in food matrix[J]. Food Chemistry, 2019, 297:124934.
[20] KUANG L X, WANG Z Q, CHENG Y, et al. Residue levels and risk assessment of pesticides in litchi and Longan of China[J]. Journal of Food Composition and Analysis, 2023, 115:104921.
[21] 李海, 邓金兰, 李伟华. 茂名地区荔枝农药残留膳食摄入风险评估[J]. 食品工业, 2023, 44(6):337-340.
LI H, DENG J L, LI W H. Risk assessment of dietary intake of pesticide residues in litchi from Maoming area[J]. The Food Industry, 2023, 44(6):337-340.
[22] 国家卫生健康委员会, 农业农村部, 国家市场监督管理总局. GB 2763—2021食品安全国家标准 食品中农药最大残留限量[S]. 北京: 中国标准出版社, 2021.
National Health Commission of the People's Republic of China, Ministry of Agriculture and Rural Affairs of the People′s Republic of China, State Administration for Market Regulation. GB 2763—2021 National food safety standard Maximum residue limits for pesticides in food[S]. Beijing: Standards Press of China, 2021.
Options
文章导航

/

〈 〉

技术支持：北京玛格泰克科技发展有限公司