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顶空气相色谱法测定氟尼辛葡甲胺原料药中有机溶剂残留量

胡慧廉

色谱2012,Vol.30Issue(1):99-102,4.
色谱2012,Vol.30Issue(1):99-102,4.DOI:10.3724/SP.J.1123.2011.09009

顶空气相色谱法测定氟尼辛葡甲胺原料药中有机溶剂残留量

Determination of residual organic solvents in flunixin meglumine raw material by headspace gas chromatography

胡慧廉1

作者信息

  • 1. 华东理工大学分析测试中心,上海200237
  • 折叠

摘要

Abstract

A method for the determination of five kinds of residual organic solvents in flunixin meglumine raw material was developed by headspace gas chromatography. An HP-FFAP capillary column (30 m xO. 32 mm x 1. 0 jim), a flame ionization detector and the external standard method were used for the separation and quantitative analysis. The effects of equilibrium temperature and equilibrium time on the determination of residual organic solvents were investigated. The good results were obtained in the equilibrium temperature of 90 t! And equilibrium time of 30 min. The standard curves were linear in the range of 0. 40 - 7. 93 mg/L (r = 0. 999 8) for ethyl acetate, 7. 32 - 146. 48 mg/L (r = 0. 999 6) for methanol, 4. 53 - 90. 61 mg/L (r = 0. 999 9) for isopropanol, 3. 62 - 72. 32 mg/L (r = 0. 999 8) for ethanol and 2.31- 46. 24 mg/L (r = 0. 999 6) for acetonitrile. The recoveries for the five residual organic solvents were between 95. 96% and 100.31% with relative standard deviations (RSDs) (n =6) of 1.97% -3.28%. The detection limits of ethyl acetate, methanol, isopropanol, ethanol and acetonitrile were 0. 08, 0. 9, 0. 2, 0. 4 and 0. 3 mg/L, respectively. The proposed method was successfully applied to analyze the residual organic solvents in the real sample of flunixin meglumine raw material. The results showed that only isopropanol and ethanol were found in the sample with the contents of 177. 44 jtg/g and 69. 32 |xg/g, respectively. The method is rapid, sensitive and accurate for the content determination of residual solvents in flunixin meglumine raw material.

关键词

顶空气相色谱法/有机溶剂残留/氟尼辛葡甲胺

Key words

headspace gas chromatography ( HS-GC)/ residual organic solvents/ flunixin meglumine

分类

化学化工

引用本文复制引用

胡慧廉..顶空气相色谱法测定氟尼辛葡甲胺原料药中有机溶剂残留量[J].色谱,2012,30(1):99-102,4.

色谱

OA北大核心CSCDCSTPCD

1000-8713

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