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茶叶科学 ›› 2023, Vol. 43 ›› Issue (6): 857-869.

• 研究报告 • 上一篇    下一篇

全自动固相萃取结合UPLC-MS/MS测定茶叶中的草甘膦及其代谢物

易华娟1, 朱洁灵1, 周瑞铮1, 郑耀林1, 张树权1, 杨乐1, 苏雍伦2   

  1. 1.东莞市食品药品检验所,广东 东莞 523000;
    2.广东医科大学,广东 东莞 523000
  • 收稿日期:2023-06-12 修回日期:2023-10-08 出版日期:2023-12-15 发布日期:2024-01-08
  • 作者简介:易华娟,女,助理工程师,主要从事食品安全检测与分析评价研究,872432671@qq.com
  • 基金资助:
    东莞市社会发展科技项目(20211800901872)

Determination of Glyphosate and Its Metabolites in Tea by Automatic Solid Phase Extraction Combined with UPLC-MS/MS

YI Huajuan1, ZHU Jieling1, ZHOU Ruizheng1, ZHENG Yaolin1, ZHANG Shuquan1, YANG Le1, SU Yonglun2   

  1. 1. Dongguan Institute for Food and Drug Control, Dongguan 523000, China;
    2. Guangdong Medical University, Dongguan 523000, China
  • Received:2023-06-12 Revised:2023-10-08 Online:2023-12-15 Published:2024-01-08

摘要: 建立超高效液相色谱-质谱/质谱法(UPLC-MS/MS)测定茶叶中草甘膦及其代谢物氨甲基膦酸的分析方法。用水-二氯甲烷体系对样品进行提取和初步除杂,在全自动固相萃取仪中通过聚苯乙烯键合苯磺酸混合型阳离子交换柱进一步净化样品溶液基质,利用正交试验和方差分析得出最优的衍生条件为5%硼酸钠缓冲溶液和10 mg·mL-1的9-芴基甲基三氯甲烷(FMOC-Cl)衍生剂在室温下衍生2 h,衍生后的样品溶液在HSS T3色谱柱和5 mmol·L-1乙酸铵溶液(含0.1%甲酸)-乙腈流动相体系下进行梯度洗脱分离,经UPLC-MS/MS进行内标法定量分析。草甘膦和氨甲基膦酸在0.2~50 ng·mL-1质量浓度范围内线性关系良好,相关系数(R2)均大于0.999,该方法的检出限为2 μg·kg-1,定量限为5 μg·kg-1。低、中、高3个加标水平(5、50 μg·kg-1和250 μg·kg-1)的回收率为94.2%~106.7%,相对标准偏差为3.8%~4.9%。该方法具有高效率、高准确度、高通量、基质干扰小和自动化程度高等优点,适用于实验室日常大批量茶叶样品筛查草甘膦及氨甲基膦酸残留的工作需求。

关键词: 草甘膦, 氨甲基膦酸, 全自动固相萃取仪, 超高效液相色谱-质谱联用仪

Abstract: An analytical method for the determination of glyphosate and its metabolite aminomethylphosphonic acid in tea was established by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted and preliminarily purified using a water dichloromethane system and the sample matrix was further purified by mixed-mode cation exchanger column filled with polystyrene bonded benzenesulfonic acid in an automatic solid phase extractor. The optimal derivation conditions obtained by orthogonal test and variance analysis were 5% sodium borate buffer solution and 10 mg·mL-1 FMOC-Cl derivatizing agent for derivatization at room temperature for 2 h. The derived sample solution was subjected to gradient elution separation on HSS T3 column and 5 mmol·L-1 ammonium acetate solution (containing 0.1% formic acid)-acetonitrile mobile phase system. The targets were analyzed by UPLC-MS/MS and quantified by internal standard method. The linearity of glyphosate and aminomethylphosphonic acid was good in the concentration range of 0.2-50 ng·mL-1 and the correlation coefficient (R2) was greater than 0.999. The detection limit of the method was 2 μg·kg-1, and the quantitation limit was 5 μg·kg-1. The recoveries of 5, 50 and 250 μg·kg-1 were in range of 94.2%-106.7% with relative standard deviations of 3.8%-4.9%, at low, medium and high spiked levels. The method is suitable for the determination of glyphosate and aminomethylphosphonic acid residues in daily large quantities of tea samples in the laboratory with the advantages of high efficiency, high accuracy, high throughput, low matrix interference and high degree of automation.

Key words: glyphosate, aminomethylphosphonic acid, automatic solid phase extractor, UPLC-MS/MS

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