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中国农学通报

中国农学通报 ›› 2026, Vol. 42 ›› Issue (10): 150-156.doi: 10.11924/j.issn.1000-6850.casb2025-0848

• 植物保护·农药 • 上一篇    下一篇

气相色谱-三重四级杆质谱联用仪检测红花中9种杀菌剂残留量

白铭松1(), 罗廷顺2, 熊斌1, 李成功1(), 熊彩云1, 张永1, 袁潘1   

  1. 1 祥云县检验检测所， 云南祥云 672100
    2 大理州药品检验所， 云南大理 671000
  • 收稿日期:2025-10-03 修回日期:2026-01-12 出版日期:2026-05-25 发布日期:2026-05-27
  • 通讯作者:
    李成功，男，1988年出生，云南曲靖人，工程师，硕士，主要从事食品、药品检测分析，昆虫类资源开发与利用等研究。通信地址：672100 云南省大理州祥云县祥城镇和谐大道北侧 祥云县检验检测所，E-mail：。
  • 作者简介:

    白铭松，男，1987年出生，云南大理人，主管中药师，硕士，主要从事天然药物化学成分分析、中药材化学污染物控制等研究。通信地址：672100 云南省大理州祥云县祥城镇和谐大道北侧 祥云县检验检测所，Tel：0872-3129300，E-mail：。

  • 基金资助:
    云南省药品安全监管科技项目“小儿导赤片质量标准提升的多维度探索与实践研究”(2025YNYJ20); 云南省创新引导与科技型企业培育计划乡村振兴科技专项“云南省祥云县蔬菜产业科技特派团”(202204BI090024); 云南省创新引导与科技型企业培育计划乡村振兴科技专项“服务型科技特派员”(202204BK090141)

Determination of Nine Fungicides Residues in Carthamus tinctorius by GC-MS/MS

BAI Mingsong1(), LUO Tingshun2, XIONG Bin1, LI Chenggong1(), XIONG Caiyun1, ZHANG Yong1, YUAN Pan1   

  1. 1 Xiangyun Inspection and Testing Institute, Xiangyun, Yunnan 672100
    2 Dali Institute for Drug Control, Dali, Yunnan 671000
  • Received:2025-10-03 Revised:2026-01-12 Published:2026-05-25 Online:2026-05-27

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摘要：

建立一种基于QuEChERS前处理结合气相色谱-三重四级杆质谱联用(GC-MS/MS)的分析方法，用于高效、灵敏地检测红花中氟唑环菌胺、苯并烯氟菌唑等9种杀菌剂的残留。样品经水化处理后，以乙腈为提取溶剂，采用QuEChERS方法进行提取和净化。分离采用HP-5MS毛细管柱(30 m×0.25 mm，0.25 µm)，检测采用多反应监测模式，并使用基质匹配内标法进行定量分析。结果表明，该方法能够快速提取红花中9种杀菌剂，并实现高灵敏度测定。在5~500 μg/L的质量浓度范围内，9种杀菌剂的色谱峰面积与质量浓度呈良好的线性关系，相关系数(R2)为0.9998~0.9999。方法的检出限为0.0008~0.0053 mg/kg，定量限为0.0027~0.0169 mg/kg。在低、中、高3个加标水平下，平均回收率为75.58%~89.95%，相对标准偏差为0.27%~8.43%(n=6)。经验证，该方法具有前处理简便、定量准确、灵敏度高的优点，能够满足农药残留检测分析的要求，可为红花质量安全控制及这9种杀菌剂的残留风险监测提供可靠的技术支持。

关键词: QuEChERS, 三重四级杆气相色谱质谱联用仪, 红花, 杀菌剂, 氟唑环菌胺, 基质效应

Abstract:

The purpose is to establish an analytical method for the determination of the nine fungicides (such as sedaxane and benzovindiflupyr) residues in Carthamus tinctorius using QuEChERS pretreatment combined with triple quadrupole gas chromatography-tandem mass spectrometry (GC-MS/MS). After the sample was subjected to hydration treatment, samples were extracted with acetonitrile, and purified by QuEChERS. The sample solution was separated on an HP-5 MS capillary column (30 m×0.25 mm, 0.25 μm) and analyzed in multiple reactions monitoring (MRM) mode, with quantification performed by matrix-matched internal standard method. This method enabled rapid extraction and high-sensitivity determination of the nine fungicides in C. tinctorius. The mass concentrations of the nine fungicides showed a linear correlation with the chromatographic peak areas in the range of 5-500 μg/L, with correlation coefficients (R2) of 0.9998-0.9999. The method detection limit (MDL) ranged from 0.0008-0.0053 mg/kg, and the method quantification limit (MQL) ranged from 0.0027-0.0169 mg/kg. The average recoveries at three spiked levels (high, medium and low) ranged from 75.58% to 89.95%, and the relative standard deviations of the determination results were 0.27%-8.43% (n=6). This method features simple pretreatment, accurate quantification, and high sensitivity, meeting the requirements for pesticide residue detection and analysis, and can provide reliable technical support for quality and safety control of C. tinctorius and residual risk monitoring of the nine fungicides.

Key words: QuEChERS, GC-MS/MS, Carthamus tinctorius, fungicides, sedaxane, matrix effect

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