毛细管气相色谱柱顶空进样法测定利福平及氯诺昔康中有机溶剂残留量

王建;施华琴

中国药学杂志 ›› 2003, Vol. 38 ›› Issue (04) : 291-293.

中国药学杂志 ›› 2003, Vol. 38 ›› Issue (04) : 291-293.
药品质量及检验

毛细管气相色谱柱顶空进样法测定利福平及氯诺昔康中有机溶剂残留量

  • 王建;施华琴
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Determination of the residual organic volatile solvents in rifampin and lornoxicam by capillary gas chromatography with headspace sampling

  • WANG Jian1,SHI Hua-qin2
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摘要

目的测定利福平及氯诺昔康中有机溶剂残留量。方法毛细管气相色谱柱顶空进样法,FID检测器。利福平以5%苯基甲基聚硅氧烷为固定相,柱温50℃;氯诺昔康以聚乙二醇为固定相,柱温50℃维持15min,以10℃·min-1的速率升温至165℃,维持5min。结果甲醇、丙酮、氯仿、正丁醇线性关系r分别为0.9999,0.9999,0.9984,0.9998;平均回收率分别为96.0%,97.3%,81.1%,93.9%,RSD分别为2.7%,1.9%,8.8%,2.5%(n=5)。结论方法柱效高、灵敏、准确,适用于利福平及氯诺昔康中有机溶剂残留量测定。

Abstract

OBJECTIVE To determine the residual organic volatile solvents in rifampin and lornoxicam.METHOD S The samples were injected on sillica capillary column by headspace sampler with FID detector.The determination of rifampin was performed on a HP5 5% phenyl methyl siloxane.The column temperature was 50℃.The determination of lornoxicam was performed on a AC 20 polyethylene glycol column which was kept the initial temperature at 50℃,then raised to 165℃ at the rate of 10℃·min-1 and sustained for 5 min.RESULTS The correlation r in methanol,acetone,chloroform and butanol was respectively 0.999 9,0.999 9,0.998 4 and 0.999 8.The recovery was 96.0%,97.3%,81.1% and 93.9% with RSD 2.7%,1.9%,8.8% and 2.5%,(n=5) respectively.CONCLUSION The method appeared to be sensitive and accurate,and can be used for the determination of the residual organic volatile solvents in rifampin and lornoxicam.

关键词

利福平 / 氯诺昔康 / 气相色谱法 / 有机溶剂残留量

Key words

rifampin / lornoxicam / gas chromatography / residual organic volatile solvents

引用本文

导出引用
王建;施华琴. 毛细管气相色谱柱顶空进样法测定利福平及氯诺昔康中有机溶剂残留量[J]. 中国药学杂志, 2003, 38(04): 291-293
WNG Jin;SHI Hu-qin. Determination of the residual organic volatile solvents in rifampin and lornoxicam by capillary gas chromatography with headspace sampling[J]. Chinese Pharmaceutical Journal, 2003, 38(04): 291-293

参考文献

[1]USP ⅩⅩⅣ[S].2000:1342;1877.

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