职业与健康 ›› 2024, Vol. 40 ›› Issue (18): 2474-2477.

• 论著 • 上一篇    下一篇

液相色谱-串联质谱法测定果蔬酱中13种吡啶和嘧啶类除草剂

郭爱静1, 张立华2, 陈龙星1, 田会方1, 赵伟1   

  1. 1.石家庄市疾病预防控制中心毒物检测中心,石家庄市化学毒物检测及风险预警技术创新中心,河北 石家庄 050011;
    2.石家庄市动物园经营科,河北 石家庄 050200
  • 收稿日期:2023-12-07 修回日期:2024-01-15 发布日期:2026-03-17
  • 通信作者: 赵伟,副主任技师,E-mail:13933887009@139.com
  • 作者简介:郭爱静,女,副主任技师,主要从事理化分析工作。
  • 基金资助:
    河北省医学科学研究课题计划(20231704)

Determination of 13 pyridine and pyrimidine herbicides in fruit and vegetable sauce by liquid chromatography-tandem mass spectrometry

GUO Aijing1, ZHANG Lihua2, CHEN Longxing1, TIAN Huifang1, ZHAO Wei1   

  1. 1. Department of Poison Detection,Shijiazhuang Center for Disease Control and Prevention,Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning,Shijiazhuang,Hebei 050011,China;
    2. Management Division,Shijiazhuang Zoo,Shijiazhuang,Hebei 050200,China
  • Received:2023-12-07 Revised:2024-01-15 Published:2026-03-17
  • Contact: ZHAO Wei,Deputy chief technician,E-mail:13933887009@139.com

摘要: 目的 建立果蔬酱中13种吡啶和嘧啶类除草剂的多残留液相色谱-串联质谱方法。方法 样品经乙腈(含1%甲酸)提取、QuEChERS(quick,easy,cheap,effective,rugged and safe)技术净化后用ZORBAX SB-Aq柱(2.1 mm×150 mm,3.5 μm)分离,以乙腈-0.1%甲酸水溶液(含5 mmol/L乙酸铵)为流动相进行梯度洗脱,以液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometric,LC-MS/MS)的多反应监测模式(multi-reaction monitoring,MRM)检测,外标法定量。结果 13种吡啶和嘧啶类除草剂在各自的浓度范围内线性关系良好,相关系数(r)均>0.999,3个不同浓度的平均加标回收率为80.36%~118.74%,相对标准偏差为0.22%~9.62%,方法检出限为0.06~1.60 μg/kg。结论 该方法操作简单、灵敏度高、重复性好,可用于果蔬酱中13种吡啶和嘧啶类除草剂的同时检测。

关键词: 液相色谱-串联质谱, 果蔬酱, 吡啶和嘧啶类除草剂, QuEChERS

Abstract: Objective To establish a multi residue liquid chromatography-tandem mass spectrometric(LC-MS/MS) method for the determination of 13 pyridine and pyrimidine herbicides in fruit and vegetable sauce. Methods The samples were extracted with acetonitrile(containing 1% formic acid),purified using QuEChERS(quick,easy,cheap,effective,rugged and safe) technology,and separated using a ZORBAX SB-Aq column(2.1 mm×150 mm,3.5 μm). The gradient elution was performed using an acetonitrile 0.1% formic acid aqueous solution(containing 5 mmol/L ammonium acetate) as the mobile phase,and detected using LC-MS/MS in multiple-reaction monitoring(MRM) mode. Quantification was performed using an external standard method. Results 13 pyridine and pyrimidine herbicides showed good linear relationships within their respective concentration ranges,with correlation coefficients greater than 0.999. The average recovery rates for three different concentrations ranged from 80.36% to 118.74%,with relative standard deviations of 0.22% to 9.62%,and the limits of detection was 0.06-1.60 μg/kg. Conclusion The method is simple and sensitive,with good reproducibility,and can be used for simultaneous detection of 13 pyridine and pyrimidine herbicides in fruit and vegetable sauce.

Key words: Liquid chromatography-tandem mass spectrometry, Fruit and vegetable sauce, Pyridine and pyrimidine herbicides

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