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| QuEChERS-液相色谱-串联质谱法检测多种植物源性食品中氰氟草酯及其代谢物残留 |
| Determination of cyhalofop-butyl and cyhalofop acid residues in foods of plant origin by QuEChERS-Liquid Chromatography-Tandem Mass Spectrometry |
| 投稿时间：2026-03-31 修订日期：2026-08-07 |
| DOI： |
| 中文关键词: 氰氟草酯 氰氟草酸 液相色谱-三重四级杆串联质谱 分散固相萃取 |
| 英文关键词:cyhalofop-butyl cyhalofop acid liquid chromatography tandem mass spectrometry QuEChERS |
| 基金项目:国家重点研发计划(2022YFF1100804)Fund: Supported by the National Key R D Program of China Foundation (2022YFF1100804)*<sup>通</sup>信作者: 王飞,高级工程师,主要研究方向为食品及农产品安全检测。E-mail: wangfei_0124@126.com*<sup>Corresponding author: </sup>WANG Fei, Senior Engineer, Tianjin Customs Animals Plants and Foods Inspection Center, Tianjin, 300457, China. E-mail: wangfei_0124@126.com ,王利强1<sup>,</sup>杨丽2<sup> </sup> |
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| 中文摘要: |
| 目的 建立一种基于QuEChERS分散固相萃取-液相色谱-串联质谱法测定多种植物源性食品中氰氟草酯及其主要代谢物氰氟草酸残留量的同步、快速确证与定量方法。方法 样品经含1%甲酸的乙腈溶液提取，采用改良QuEChERS法进行净化，质谱检测采用电喷雾离子源（ESI），在正负离子切换的多反应监测（MRM）模式下同时采集数据。结果 在优化条件下，氰氟草酸的定量限可达0.01 mg/kg，氰氟草酯的定量限可达0.02 mg/kg。两种目标物在0.05~2.0 mg/L的质量浓度范围内线性关系良好，相关系数（r2）均大于0.99。在糙米、小麦、大豆、花生、苹果、桃、番茄、黄瓜、菠菜、茶叶10种植物源性基质三个添加水平的平均回收率为68.7%~106.7%，相对标准偏差为2.6%~14.3%。结论 该方法前处理简单，准确度与精密度均符合残留分析要求，能有效克服复杂基质的干扰，满足对植物源性食品中氰氟草酯及其代谢物氰氟草酸的同时确证及定量要求，适用于大批量植物源性食品中氰氟草酯及其代谢物的日常监测与风险评估。 |
| 英文摘要: |
| Objective To establish a method for determination of cyhalofop-butyl and cyhalofop acid in foods of plant origin by liquid chromatography tandem mass spectrometry based on QuEChERS pre-treatment technology. Methods The acetonitrile contain 1% formic acid was used as the extraction solution, and the QuEChERS dispersion solid phase extraction method was used for purification. The target analytes were detected in the positive and negative ion mode using electrospray ionization (ESI) source. Results Under optimized conditions, the quantitation limit of cyhalofop acid can reach 0.01 mg/kg, while that of cyhalofop-butyl can reach 0.02 mg/kg. The linear relationship between the two target substances and their mass concentrations ranges from 0.05 to 2.0 mg/L, with correlation coefficients (r2) all greater than 0.99. In three spiked levels of ten plant-derived matrices including brown rice, wheat, soybeans, peanuts, apples, peaches, tomatoes, cucumbers, spinach, and tea, the average recovery rate ranged from 68.7% to 106.7%, with relative standard deviations ranging from 2.6% to 14.3%. Conclusion This method features a simple sample preparation procedure, with accuracy and precision compliant with the requirements for residue analysis. It effectively overcomes complex matrix interference and fulfills the criteria for the simultaneous confirmation and quantification of target analytes in plant-derived foods. Consequently, the method is well-suited for routine monitoring and risk assessment of large-scale samples. |
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