| 姬乐园, 王平平, 朱丽珍, 毛连纲, 张兰, 蒋红云, 刘新刚*.液相色谱串联质谱法检测草铵膦、草甘膦及其代谢物在水和土壤中的残留[J].植物保护,2024,50(2):235-239. |
| 液相色谱串联质谱法检测草铵膦、草甘膦及其代谢物在水和土壤中的残留 |
| Determination of glufosinate-ammonium, glyphosate and their metabolites in soil and water by HPLC-MS/MS |
| 投稿时间：2023-03-09 修订日期：2023-03-30 |
| DOI：10.16688/j.zwbh.2023115 |
| 中文关键词: 水和土壤 草铵膦 草甘膦 代谢物 UHPLC-MS/MS 残留检测 |
| 英文关键词:water and soil glufosinate-ammonium glyphosate metabolite UHPLC-MS/MS residue analysis |
| 基金项目:国家自然科学基金国际(地区)合作与交流项目（32261133527） |
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| 中文摘要: |
| 利用超高效液相色谱-串联质谱仪(UHPLC-MS/MS),结合固相萃取净化建立了在水和土壤中同时快速测定草甘膦、草铵膦及其6种代谢物的多残留分析方法。前处理采用Oasis MCX和Oasis MAX固相萃取柱提取,2%甲酸甲醇-水(体积比为1∶1)洗脱,旋干后0.1%氨水定容,UHPLC-MS/MS检测。方法的线性范围为0.02～0.5 mg/L;在水中添加水平为0.000 1 mg/L和0.001 mg/L时,草甘膦、草铵膦及其代谢物的回收率为72.8%~94.2%,RSD为2.3%~16.1%;土壤中添加水平为0.001 mg/kg和0.01 mg/kg时,草甘膦、草铵膦及其代谢物的回收率为70.6%~88.5%,RSD为3.6%~12.8%。本方法准确、灵敏、全面,适用于草甘膦、草铵膦及其代谢物在水土环境中的残留检测及监测。 |
| 英文摘要: |
| An ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) combined with solid-phase extraction purification was used to establish a multi-residue analysis method for the simultaneous determination of glyphosate, glufosinate-ammonium and their six metabolites in water or soil. Oasis MCX and Oasis MAX solid phase extraction columns were used in pre-treatment, and then 2% formic acid methanol water (volume ratio of 1∶1) was used for elution. The eluent collected was evaporated to dryness by a rotary evaporator and diluted with 0.1% ammonia. The linear range of the method was 0.02-0.5 mg/L. Under the spiked level of 0.000 1 and 0.001 mg/L in the purified water, the recoveries were 72.8%-94.2% and the relative standard deviations were 2.3%-16.1%, respectively. Under the spiked level of 0.001 mg/kg and 0.01 mg/kg in the soil, the recoveries were 70.6%-88.5% and the relative standard deviations were 3.6%-12.8%, respectively. The method is accurate, sensitive and comprehensive, which could be used to analyze the content of glyphosate, glufosinate-ammonium and their metabolites in low concentration samples in environmental test. |
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