| 超高效液相色谱-串联质谱法测定柑橘中的草甘膦及其代谢物残留 |
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| 引用本文： | 张梦娜,杨云,王立平,潘兴鲁,徐军,吴小虎,王宽,董丰收,郑永权.超高效液相色谱-串联质谱法测定柑橘中的草甘膦及其代谢物残留[J].植物保护,2023,49(4):216-223. |
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| 作者姓名： | 张梦娜 杨云 王立平 潘兴鲁 徐军 吴小虎 王宽 董丰收 郑永权 |
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| 作者单位： | 1. 农业农村部食物与营养发展研究所, 北京100081; 2. 中国农业科学院植物保护研究所, 植物病虫害综合治理全国重点实验室, 北京100193 |
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| 基金项目： | 国家自然科学基金(31901922) |
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| 摘 要： | 本研究首次建立了一种超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定柑橘中草甘膦及其代谢物N-乙酰草甘膦?氨甲基磷酸(AMPA)和N-乙酰AMPA?样品经过0.5%甲酸水提取, 以十八烷基硅烷键合硅胶柱(C18)净化, 利用水和200 mmol/L碳酸氢铵溶液(含0.1%氨水)作为流动相梯度洗脱, 在多反应监测模式下定量分析?结果表明, 草甘膦及其代谢物在0.05~1 mg/kg范围内线性关系良好, 相关系数均大于0.99; 草甘膦及其3个代谢物在柑橘全果和果肉基质中3个加标水平下回收率为 70.5%~109.5%, 相对标准偏差(RSD)为0.6%~10.1%, 定量限为0.05 mg/kg?本方法的前处理样品无需衍生, 简便?快捷?高效?准确可靠, 可用于柑橘中草甘膦及其代谢物N-乙酰草甘膦?AMPA和N-乙酰AMPA的定量检测?
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| 关 键 词： | 农药残留 柑橘 草甘膦 代谢物 |
| 收稿时间： | 2022/6/5 0:00:00 |
| 修稿时间： | 2022/7/4 0:00:00 |
Simultaneous determination of glyphosate and its metabolites in citrus by UHPLC-MS/MS |
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| ZHANG Mengn,YANG Yun,WANG Liping,PAN Xinglu,XU Jun,WU Xiaohu,WANG Kuan,DONG Fengshou,ZHENG Yongquan.Simultaneous determination of glyphosate and its metabolites in citrus by UHPLC-MS/MS[J].Plant Protection,2023,49(4):216-223. |
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| Authors: | ZHANG Mengn YANG Yun WANG Liping PAN Xinglu XU Jun WU Xiaohu WANG Kuan DONG Fengshou ZHENG Yongquan |
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| Institution: | 1. Institute of Food and Nutrition Development, Ministry of Agriculture and Rural Affairs, Beijing100081, China; 2. State Key Laboratory for Biology of Plant Disease and Insect Pests, Institute of Plant Protection, Chinese Academy of Agricultural Sciences, Beijing100193, China |
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| Abstract: | An analytical method for the simultaneous determination of glyphosate and its metabolites N-acetyl-glyphosate, aminomethylphosphonic acid and N-acetyl aminomethylphosphoric acid in citrus samples by ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) was established for the first time. The samples were extracted with 0.5% formic acid aqueous solution and purified by matrix dispersion extraction with 40 mg C18 as adsorbent. The mobile phase was eluted with water and 200 mmol/L ammonium bicarbonate solution (with 0.1% ammonia water), and determined by the LC-MS/MS under multiple reaction monitoring (MRM) mode. The results showed that a good linearity ranged from 0.05-1 mg/kg was obtained with the correlation coefficients all higher than 0.99. The average recoveries of glyphosate and its metabolites in citrus and pulp at three spiked levels were 70.5%-109.5%, with the RSD of 0.6%-10.1% and the limit of quantitative (LOQ) was 0.05 mg/kg, respectively. The pretreatment samples of this method does not need derivatization, which was convenient, rapid, accurate and reliable, and could be applied for quick detection of glyphosate and its metabolites. |
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| Keywords: | pesticide residue citrus glyphosate metabolite |
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