色谱

色谱 ›› 2012, Vol. 30 ›› Issue (01): 99-102.DOI: 10.3724/SP.J.1123.2011.09009

• 技术与应用 • 上一篇    下一篇

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*   

  1. 华东理工大学分析测试中心, 上海 200237
  • 收稿日期:2011-09-06 修回日期:2011-10-10 出版日期:2012-01-28 发布日期:2012-03-01
  • 通讯作者: 胡慧廉,硕士,高级工程师,从事气相色谱方法开发和应用研究. Tel: (021)64253223,

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

HU Huilian*   

  1. Research Center of Analysis and Testing, East China University of Science and Technology, Shanghai 200237, China
  • Received:2011-09-06 Revised:2011-10-10 Online:2012-01-28 Published:2012-03-01

PDF

428

被引次数

36

摘要： 建立了氟尼辛葡甲胺原料药中乙酸乙酯、甲醇、异丙醇、乙醇和乙腈有机溶剂残留量的顶空气相色谱分析方法。以HP-FFAP色谱柱(30 m×0.32 mm×1.0 μm)为分离柱,火焰离子化检测器检测,外标法定量,并考察了顶空平衡温度、平衡时间等对残留有机溶剂测定的影响。实验结果表明,在顶空平衡温度为90 ℃、平衡时间为30 min条件下获得较好的定量结果。乙酸乙酯、甲醇、异丙醇、乙醇和乙腈的线性范围分别为0.40～7.93 mg/L (r=0.9998)、7.32～146.48 mg/L (r=0.9996)、4.53～90.61 mg/L (r=0.9999)、3.62～72.32 mg/L (r=0.9998)和2.31～46.24 mg/L (r=0.9996);平均回收率范围为95.96%～100.31%,精密度(以相对标准偏差计,n=6)为1.97%～3.28%;检出限分别为0.08、0.9、0.2、0.4和0.3 mg/L。利用该方法对实际样品氟尼辛葡甲胺原料药中有机溶剂残留量进行了检测。结果表明,该样品中含有异丙醇和乙醇,其含量分别为177.44 μg/g与69.32 μg/g。本方法快速、灵敏、准确,适用于氟尼辛葡甲胺原料药中残留溶剂的检测。

关键词: 顶空气相色谱法, 氟尼辛葡甲胺, 有机溶剂残留

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×0.32 mm×1.0 μm), 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 ℃ and equilibrium time of 30 min. The standard curves were linear in the range of 0.40~7.93 mg/L (r=0.9998) for ethyl acetate, 7.32~146.48 mg/L (r=0.9996) for methanol, 4.53~90.61 mg/L (r=0.9999) for isopropanol, 3.62~72.32 mg/L (r=0.9998) for ethanol and 2.31~46.24 mg/L (r=0.9996) 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 μg/g and 69.32 μg/g, respectively. The method is rapid, sensitive and accurate for the content determination of residual solvents in flunixin meglumine raw material.

Key words: flunixin meglumine, residual organic solvents, headspace gas chromatography （HS-GC）