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

作　　者：刘薇芝[1] 胡汉昆[1] 刘萍[1] 刘巍[1] 张觅[1] 郑保根 刘安妮[3] 颜锵 周丽娟 刘一鸣 

机构地区：[1]武汉大学中南医院药学部,武汉430071 [2]武汉大学第二临床学院,武汉430071 [3]武汉大学经济学院,武汉430071 [4]武汉药谷生物工程有限公司,武汉430000 [5]Jackson State University,Jackson 39209

出　　处：《医药导报》2015年第8期1072-1074,共3页Herald of Medicine

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

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。Objective To establish a gas chromatograph method for determing Chloroform, ethyl acetate and N, N- dimethyl 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 0.896-8.061μg·m L^-1 respectively.The average recoveries were 99.18%, 102.84% and 98.71%.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.

关 键 词：布康唑 硝酸 色谱法 气相 有机溶剂残留 

分 类 号：R978.5[医药卫生—药品] R927.1[医药卫生—药学]