顶空毛细管气相色谱法测定盐酸拉贝洛尔中有机残留量  

Determination of organic solvent residual volume in labetalol hydrochloride by headspace gas chromatography

作　　者：黄宁华[1,2] 刘雅琼[1,2] 王京宇[1,2] 欧阳荔[1,2] 

机构地区：[1]北京大学医学部公卫学院中心仪器室,北京100191 [2]北京大学医药卫生分析中心生命元素组学实验室,北京100191

出　　处：《实验技术与管理》2010年第12期54-57,共4页Experimental Technology and Management

基　　金：科技部“重大新药创制”专项支持(2009ZX09502)

摘　　要：目的：建立了盐酸拉贝洛尔中丙酮、乙酸乙酯、甲醇、异丙醇、乙醇、二氧六环残留量的测定方法。方法：使用DB-WAX柱（30 m×0.32 mm,0.5μm）,以高纯氮气为载气,以岛津2010气相色谱仪为检测器;程序升温,初始温度40℃,保持5 min,以5℃/min升温至80℃;50℃/min升温至200℃,保持5.5 min。进样口温度为200℃,检测器温度为250℃。结果：丙酮、乙酸乙酯、甲醇、异丙醇、乙醇、二氧六环具有良好的线性;相对标准偏差均小于7.5%,平均回收率99.53%～106.77%。结论：此方法简单、准确,灵敏度高,可用于检测盐酸拉贝洛尔中的丙酮、乙酸乙酯、甲醇、异丙醇、乙醇和二氧六环的残留量的测定。AIM： To develop a headspace GC method for determination of acetone,ethyl acetate,methanol,Isopropanol,ethanol and 1,4-dioxane in labetalol hydrochloride.METHODS： The determination was performed on head headspace GC with FID detector,by using nitrogen as the carries gas.The capillary column was DB-WAX（30m ×0.32 mm,0.5μm） and the temperature was initially maintained at 40 ℃ for five minutes and increased to 80 ℃ at a rate of 5 ℃/min,then 50 ℃/min raised to 200 ℃ and subsequently sustained for 5.5 minutes.The temperatures of injector and detector were 200 ℃ and 250 ℃,respectively.RESULTS： The correlation coefficient of calibration curve of each contents was 0.999.The limits of determination were 0.3,0.4,2.7,1.5,2.0,1.5 μg/min respectively.The recoveries were between 99.53% and 106.77%,the RSD4.5%（n=3）.CONCLUSIONS： The method was proved to be accurate,sensitive and reliable.The results for linearity,precision and recoveries were good and suitable for the determination of organic solvent residual volume in labetalol hydrochloride.

关 键 词：盐酸拉贝洛尔 顶空气相色谱法 有机溶剂残留 

分 类 号：R917[医药卫生—药物分析学]