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中国农学通报

中国农学通报 ›› 2025, Vol. 41 ›› Issue (16): 143-149.doi: 10.11924/j.issn.1000-6850.casb2024-0581

• 植物保护·农药 • 上一篇    下一篇

基于四极杆-飞行时间质谱法测定荔枝中9种杀菌剂残留量

胡福初1(), 刘艳萍2, 段云3, 陈棠钻3, 周文静1, 王祥和1(), 王思威2()   

  1. 1 海南省农业科学院热带果树研究所/农业农村部热带果蔬遗传资源评价利用重点实验室（部省共建）/海南省热带果树生物学重点实验室，海口 571100
    2 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，广州 510640
    3 中国热带农业科学院分析测试中心，海口 571101
  • 收稿日期:2024-09-10 修回日期:2025-03-22 出版日期:2025-06-05 发布日期:2025-06-05
  • 通讯作者:
    王祥和，研究员，研究方向：热带果树栽培。E-mail：。
    王思威，副研究员，研究方向：果树上化学农药残留特征研究。E-mail：。
  • 作者简介:

    胡福初，男，1982年出生，江西都昌人，研究员，博士，主要从事热带果树轻简栽培和资源育种研究。通信地址：571100 海南省海口市琼山区兴丹路14号 海南省农业科学院热带果树研究所，Tel：0898-65230558，E-mail：。

  • 基金资助:
    2021海南省重大科技计划项目“荔枝优质高效生产关键技术研究与示范”(ZDKJ2021006); 国家现代农业产业技术体系项目“国家荔枝龙眼产业技术体系”(CARS-32); 海南省荔枝产业技术体系“海南省荔枝产业技术体系高产优质栽培岗”(HNARS-08)

Detection of 9 Fungicides Residues in Lychee Based on High-performance Liquid Chromatography-tandem Quadrupole-time of Flight-mass Spectrometry

HU Fuchu1(), LIU Yanping2, DUAN Yun3, CHEN Tangzuan3, ZHOU Wenjing1, WANG Xianghe1(), WANG Siwei2()   

  1. 1 Institute of Tropical Fruit Tree, Hainan Academy of Agricultural Science/Key Laboratory of Genetic Resources Evaluation and Utilization of Tropical Fruits and Vegetables (Co-construction by Ministry and Province), Ministry of Agriculture and Rural Affairs/Key Laboratory of Tropical Fruit Tree Biology of Hainan Province, Haikou 571100
    2 Plant Protection Research Institute, 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
    3 Analysis and Testing Center, China Academy of Tropical Agricultural Science, Haikou 571101
  • Received:2024-09-10 Revised:2025-03-22 Published:2025-06-05 Online:2025-06-05

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摘要： 为科学评价9种杀菌剂在荔枝上应用的安全性，利用高效液相色谱-四极杆飞行时间质谱技术(HPLC-Q-TOF/MS)，建立9种杀菌剂在荔枝全果的多残留分析方法，并采用所建立的分析方法对田间荔枝样品杀菌剂残留量进行分析。匀浆后的样品先加入QuEChERS前处理盐包，再经乙腈提取后，将样品置于全自动QuEChERS样品处理平台振荡10 min进行净化，采用HPLC-Q-TOF/MS对9种杀菌剂进行检测。结果表明，9种杀菌剂在质量浓度0.001~0.1 mg/L内具有较好线性相关性（相关系数R2均大于0.99），在3个添加水平下(0.005、0.05、0.1 mg/kg)的平均回收率为76.6%~114.8%，相对标准偏差为1.4%~16.4%，方法检出限为1 μg/kg，定量限为3 μg/kg。吡唑醚菌酯、嘧菌酯、苯醚甲环唑和甲霜灵在荔枝全果中的残留量均低于国家规定的最大残留限制值。研究建立的分析方法可靠简便快速，适于批量样品检测需求。

关键词: 荔枝, 杀菌剂, 高效液相色谱四极杆飞行时间质谱, 农药残留, 安全应用, 检测分析

Abstract:

The paper aims to scientifically evaluate the safety of nine fungicides on lychees. A method of the simultaneous detection for 9 fungicides in lychee was established by a high-performance liquid chromatography-tandem quadrupole-time of flight-mass spectrometry (HPLC-Q-TOF/MS). The QuEChERS pre-treatment salt package were firstly added in homogenized samples, and then extracted with acetonitrile. The automated QuEChERS sample processing platform was shaken for 10 minutes to remove impurities of lychee. The data were collected by HPLC-Q-TOF/MS. The calibration curves of 9 fungicides showed good linearity in a concentration range of 0.001-0.1 mg/L (R2>0.99). The average recoveries were 76.6%-114.8% at three spiked levels (0.005, 0.05, 0.1 mg/kg), while the relative standard deviations (RSD) were 1.4%-16.4%. The limits of detection and limits of quantification were 1 μg/kg and 3 μg/kg, respectively. The residue samples were analyzed by using the established detection method. The results showed that the residues of pyrazoxystrobin, azoxystrobin, difenoconazole, and metalaxyl in the whole lychee were all below the maximum residue limit values (MRLs) set by China. The established analytical method is reliable, simple and fast, and suitable for batch samples detection.

Key words: lychee, fungicides, high-performance liquid chromatography-tandem quadrupole-time of flight-mass spectrometry, pesticide residue, safe application, detection analysis