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顶空气相色谱法测定硝酸布康唑中有机溶剂残留量

Determination of Organic Solvents Residue in Butoconazole Nitrate by Headspace Gas Chromatography

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【作者】 刘薇芝胡汉昆刘萍刘巍张觅郑保根刘安妮颜锵周丽娟刘一鸣

【Author】 LIU Weizhi;HU Hankun;LIU Ping;LIU Wei;ZHANG Mi;ZHENG Baogen;LIU Anni;YAN Qiang;ZHOU Lijuan;LIU Yiming;Department of Pharmacy,Zhongnan Hospital Wuhan University;The Second Clinical College of Wuhan University;School of Economics,Wuhan University;Wuhan Yaogu Bio-tech Co.,Ltd;Jackson State University;

【机构】 武汉大学中南医院药学部武汉大学第二临床学院武汉大学经济学院武汉药谷生物工程有限公司Jackson State University

【摘要】 目的建立测定硝酸布康唑原料药中乙酸乙酯、三氯甲烷、N,N-二甲基甲酰胺3种有机溶剂残留量的分析方法。方法采用毛细管气相色谱法,程序升温,检测器:FID;检测器温度:250℃;进样器温度:200℃;载气:氮气;顶空进样。结果在上述色谱条件下,乙酸乙酯,三氯甲烷,N,N-二甲基甲酰胺分别在0.066~0.588,0.062~0.556,0.896~8.061μg·m L-1质量浓度范围内呈良好线性关系。平均回收率分别为99.18%,102.84%,98.71%,RSD分别为3.87%,4.33%,3.71%。结论该检测方法灵敏、准确、可靠,可用于硝酸布康唑原料药的质量控制。

【Abstract】 Objective To establish a gas chromatograph method for determing Chloroform,ethyl acetate and N,Ndimethyl formamide in butoconazole nitrate. Methods The samples was detected by Headspace Gas Chromatography.Temperature programming method was adpoted and FID was used as detector. The injector temperature was 200 ℃,and the detector temperature was reach 250 ℃. Nitrogen was used as carrier gas in the experiment. Results In the mentioned chromatographic conditions,Chloroform,ethyl acetate and N,N-dimethyl formamide had good linear relationships in the ranges of 0.066-0. 588,0. 062- 0. 556 and 0. 896- 8. 061 μg · m L-1respectively. The average recoveries were 99. 18%,102. 84% and98.71%.RSD were 3.87%,4.33% and 3.71%. Conclusion The detection method is sensitive,accurate,reliable,and can be used as a quality control for butoconazole nitrate.

【基金】 2013年湖北省重大科技创新计划(2013ACA006);光谷第七批“3551光谷人才计划”创新人才项目
  • 【文献出处】 医药导报 ,Herald of Medicine , 编辑部邮箱 ,2015年08期
  • 【分类号】O657.71;R927.1
  • 【下载频次】58
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