| 第 48 卷第 4 期 |  | Vol. 48 No. 4 | | 2018 年 8 月 | Aug 2018 |
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所屬欄目：分析與測試
草銨膦原藥雜質(zhì)3-氨基-4-甲氧基-4-羰基丁基（甲基）膦酸銨的鑒定和定量分析 |
| 項 軍1，2，胡 禮1，2，孫 炯1，2，張 萍1，2，黃 路1，2
（1. 湖南化工研究院有限公司 國家農藥創(chuàng )制工程技術(shù)研究中心，湖南 長(cháng)沙 410014；2. 農用化學(xué)品湖南省重點(diǎn)實(shí)驗室，湖南 長(cháng)沙410014） |
| 摘 要：采用高效液相色譜-質(zhì)譜聯(lián)用和液相色譜法對草銨膦原藥中的有機雜質(zhì)進(jìn)行定性和定量分析。建立了草銨膦有機雜質(zhì)的定量分析方法：采用高效液相色譜法，使用ZORBAX-SAX色譜柱和紫外檢測器，以13.6 g磷酸二氫鉀溶于970 mL水中，加30 mL甲醇為流動(dòng)相，在195 nm波長(cháng)下測定雜質(zhì)3-氨基-4-甲氧基-4-羰基丁基（甲基）膦酸銨的含量。該分析方法的線(xiàn)性相關(guān)系數為0.999 98，標準偏差為0.009，變異系數為0.71%，平均回收率為99.42%，最低檢出濃度為0.01%。建立了草銨膦原藥中有機雜質(zhì)的定性和定量的分析方法，可以為草銨膦原藥質(zhì)量分析和控制提供依據。 |
| 關(guān)鍵詞：草銨膦；雜質(zhì)；鑒定；定量分析 |
| 中圖分類(lèi)號：O657 文獻標識碼：A 文章編號：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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作者簡(jiǎn)介：項 軍（1983-），男，湖南常德人，研究方向：農藥全組分分析（E-mail: xiangjun19831024@163.com）
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收稿日期：2018-07-05
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