豆粉中31种杀菌剂残留的UPLC-MS/MS测定法

职业与健康 ›› 2024, Vol. 40 ›› Issue (12): 1590-1595.

豆粉中31种杀菌剂残留的UPLC-MS/MS测定法

张波¹, 郭二菱², 黄笑晨², 郭爱静², 王可²

1.承德市食品药品检验检测中心食品检验室,河北承德 067000;
2.石家庄市疾病预防控制中心,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

收稿日期:2024-01-08 修回日期:2024-02-02 出版日期:2024-06-15 发布日期:2026-03-13
通信作者: 王可,主任技师,E-mail：wkecdc@163.com
作者简介:张波,男,食品药品高级工程师,主要从事食品检测工作。
基金资助:
河北省医学适用技术跟踪项目（GZ2022081）

Determination of 31 fungicides residues in soybean powder by UPLC-MS/MS

ZHANG Bo¹, GUO Erling², HUANG Xiaochen², GUO Aijing², WANG Ke²

1. Food Inspection Laboratory, Chengde Food and Drug Inspection and Testing Center, Chengde Hebei, 067000, China;
2. Shijiazhuang Center for Disease Control and Prevention, Shijiazhuang Technology Innovation Center for Chemical Poison Detection and Risk Early Warning, Shijiazhuang Hebei, 050011, China

Received:2024-01-08 Revised:2024-02-02 Online:2024-06-15 Published:2026-03-13
Contact: WANG Ke,Chief technician,E-mail：wkecdc@163.com

摘要/Abstract

摘要： 目的建立QuEChERS（quick、easy、cheap、effective、rugged、safe）结合超高效液相色谱-串联质谱（ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS）测定豆粉中31种苯并咪唑类和三唑类杀菌剂残留的方法。方法乙腈提取豆粉样品,用十八烷基键合硅胶（C₁₈）填料和无水硫酸镁净化上清液后氮吹干。待测样品经Kinetex^@ F5 100A（3.0×100 mm,2.6 μm）柱子进行分离,以0.1% 甲酸水溶液（A相）和甲醇（B相）作为流动相,电喷雾正离子源（electrospray ionization,ESI+）模式电离,多反应监测（multiple reaction monitoring,MRM）模式进行检测,基质匹配法定量分析。结果 31种杀菌剂浓度为0.1~100 μg/L,呈良好的线性关系（r>0.999）,各杀菌剂检出限为0.01~1.03 μg/kg,定量限为0.01~3.44 μg/kg,在3个不同浓度下的加标平均回收率为71.3%~118.7%,相对标准偏差为0.4%~9.9%。结论该方法操作简便,适用于大豆样品中31种苯并咪唑类和三唑类杀菌剂的高通量快速检测。

关键词: 超高效液相色谱-串联质谱, 苯并咪唑类杀菌剂, 三唑类杀菌剂, 豆粉, QuEChERS

Abstract: Objective To establish a QuEChERS（quick,easy,cheap,effective,rugged,safe） method combined with ultra performance liquid chromatography tandem mass spectrometry（UPLC-MS/MS） for detecting residues of 31 benzimidazole and triazole fungicides in soybean powder. Methods The soybean powder samples were extracted using acetonitrile,the supernatant was purified using octadecyl bonded silica gel（C₁₈） and anhydrous magnesium sulfate,and then blow dry with nitrogen.The samples were separated using Kinetex@F5 100A（3.0×100 mm,2.6 μm） with mobile phases consisting of 0.1% formic acid aqueous solution（phase A） and methanol（phase B）.The electrospray ionization（ESI+） mode was used for ionization,while detection was conducted using multiple reaction monitoring（MRM）. The quantitative detection was performed utilizing the matrix matching method. Results Totally 31 fungicides exhibit a good linear relationship（r>0.999） within the mass concentration range of 0.1-100 μg/L. The limits of detection of the fungicides were 0.01-1.03 μg/kg,the limits of quantitation were 0.01-3.44 μg/kg. The average recovery rate of spiked samples at three different concentrations was 71.3%-118.7%,and the relative standard deviations were 0.4%-9.9%. Conclusion The method is uncomplicated and suitable for rapidly detecting 31 triazole and benzimidazole fungicides in soybean powder samples.

Key words: Ultra performance liquid chromatography tandem mass spectrometry, Benzimidazole fungicides, Triazole fungicides, Soybean powder, QuEChERS

中图分类号:

R155.5

张波, 郭二菱, 黄笑晨, 郭爱静, 王可. 豆粉中31种杀菌剂残留的UPLC-MS/MS测定法. [J]职业与健康, 2024, 40(12): 1590-1595.

ZHANG Bo, GUO Erling, HUANG Xiaochen, GUO Aijing, WANG Ke. Determination of 31 fungicides residues in soybean powder by UPLC-MS/MS. [J]OCCUPATION AND HEALTH, 2024, 40(12): 1590-1595.

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