顶空毛细管气相色谱法测定硝酸异康唑中5种有机溶剂残留  

Determination of residues of five organic solvents in isoconazole 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 周利娟 Yiming Liu 张元珍[1] 

机构地区：[1]武汉大学中南医院药学部,湖北武汉430071 [2]武汉大学第二临床学院,湖北武汉430071 [3]武汉大学经济学院,湖北武汉430072 [4]武汉药谷生物工程有限公司,湖北武汉430074 [5]Jackson State University,39209

出　　处：《中国医院药学杂志》2016年第1期9-12,共4页Chinese Journal of Hospital Pharmacy

基　　金：2013年湖北省重大科技创新计划(重大关键技术研发类)(编号:2013ACA006)

摘　　要：目的:建立测定硝酸异康唑原料药中甲基叔丁基醚、甲醇、二氯甲烷、三氯甲烷、四氢呋喃5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,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,甲基叔丁基醚、四氢呋喃、甲醇、二氯甲烷和三氯甲烷分别在10.28~92.52μg·mL^(-1)(γ=0.999 4),14.49~130.43μg·mL^(-1)(γ=0.999 4),62.86~565.74μg·mL^(-1)(γ=0.999 3),13.52~121.68μg·mL^(-1)(γ=0.999 5),2.76~24.84μg·mL^(-1)(γ=0.999 1)质量浓度范围内线性关系良好。平均回收率分别为97.19%(RSD为1.21%),99.90%(RSD为0.28%),99.29%(RSD为1.21%),99.15%(RSD为0.65%),100.14%(RSD为2.58%)。结论:该检测方法灵敏、准确、可靠,可用于硝酸异康唑原料药的质量控制。OBJECTIVE To establish a gas chromatograph method for determination of methyl tert-butyl ether,methanol,dichloromethane,chloroform,tetra hydrofuran in isoconazole nitrate.METHODS The samples were detected by headspace gas chromatography.The detector was FID,detector temperature was 250 ℃ and injector temperature was 200 ℃,with nitrogen as carrier gas.RESULTS In the chromatographic conditions,concentrations of methyl tert-butyl ether,tetrahydrofuran,methanol,methylene chloride and chloroform,were 10.28-92.52μg·mL^-1（γ=0.999 4）,14.49-130.43μg·mL^-1（γ=0.999 4）,62.86-565.74μg·mL^-1（γ=0.999 3）,13.52-121.68μg·mL^-1（γ=0.999 5）and 2.76-24.84μg·mL^-1（γ=0.999 1）,respectively,with a good linear relationship.The average recoveries were 97.19%（RSD of 1.21%）,99.90%（RSD of 0.28%）,99.29%（RSD of 1.21%）,99.15%（RSD of 0.65%）and 100.14%（RSD2.58%）,respectively.CONCLUSION The detection method is sensitive,accurate,reliable,and can be used for quality control of isoconazole nitrate.

关 键 词：气相色谱法 硝酸异康唑 有机溶剂残留 

分 类 号：R917[医药卫生—药物分析学]