| 第 48 卷第 4 期 |  | Vol. 48 No. 4 | | 2018 年 8 月 | Aug 2018 |
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所属栏目：分析与测试
草铵膦原药杂质3-氨基-4-甲氧基-4-羰基丁基（甲基）膦酸铵的鉴定和定量分析 |
| 项 军1，2，胡 礼1，2，孙 炯1，2，张 萍1，2，黄 路1，2
（1. 湖南化工研究院有限公司 国家农药创制工程技术研究中心，湖南 长沙 410014；2. 农用化学品湖南省重点实验室，湖南 长沙410014） |
| 摘 要：采用高效液相色谱-质谱联用和液相色谱法对草铵膦原药中的有机杂质进行定性和定量分析。建立了草铵膦有机杂质的定量分析方法：采用高效液相色谱法，使用ZORBAX-SAX色谱柱和紫外检测器，以13.6 g磷酸二氢钾溶于970 mL水中，加30 mL甲醇为流动相，在195 nm波长下测定杂质3-氨基-4-甲氧基-4-羰基丁基（甲基）膦酸铵的含量。该分析方法的线性相关系数为0.999 98，标准偏差为0.009，变异系数为0.71%，平均回收率为99.42%，最低检出浓度为0.01%。建立了草铵膦原药中有机杂质的定性和定量的分析方法，可以为草铵膦原药质量分析和控制提供依据。 |
| 关键词：草铵膦；杂质；鉴定；定量分析 |
| 中图分类号：O657 文献标识码：A 文章编号：1009-9212（2018）04-0060-03 |
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| Identification and Quantitative Analysis of Impurities 3-Amino-4-methoxy-4-oxobutyl(methyl)phosphinic acid in Glufosinate |
| XIANG Jun1,2, HU Li1,2, SUN Jiong1,2, ZHANG Ping1,2, HUANG Lu1,2
(1. National Engineering Research Center for Agrochemicals, Hunan Research Institute of Chemical Industry, Changsha 410014, China; 2. Hunan Province Key Laboratory for Agrochemicals, Changsha 410014, China) |
| Abstract：Qualitative and quantitative analysis of organic impurities in glufosinate were conducted by high performance liquid chromatography-mass spectrometry (HPLC-MS) and liquid chromatography (LC). The HPLC method of quantitative analysis of the organic impurities in glufosinate was established, using column ZORBAC-SAX with UV detector and dissolving 13.6 g of KH2PO4 into 970 mL of water, then adding 30 mL methanol as mobile phase at the wave length of 195 nm. This method was used to detect the content of 3-amino-4-methoxy-4-hydroxy butyl (methyl) ammonium phosphate. The correlation coefficient RSD and coefficient of variation were of 0.999 98, 0.009 and 0.71%, respectively. The detectable limit of concentration was of 0.01%. This method was established for qualitative and quantitative analysis of organic impurities in glufosinate, and provided a basis for the quality analysis and control of the glufosinate technical. |
| Key words：glufosinate; impurities; identification; quantitative analysis |
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作者简介：项 军（1983-），男，湖南常德人，研究方向：农药全组分分析（E-mail: xiangjun19831024@163.com）
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收稿日期：2018-07-05
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