毛细管气相色谱法测定间尼索地平原料药中有机溶剂残留量  

Capillary GC method for determination of residual organic solvents in m-nisoldipine

作　　者：韩学静[1] 袁志芳[2] 杜玉民[2] 景秀娟[2] 张兰桐[2] 

机构地区：[1]河北省药品检验所,石家庄050011 [2]河北医科大学药学院药物分析教研室,石家庄050017

出　　处：《药物分析杂志》2009年第7期1193-1195,共3页Chinese Journal of Pharmaceutical Analysis

基　　金：河北省科技厅支撑计划重大课题(课题号06276407D);河北省自然基金(课题号C2008001073)

摘　　要：目的:建立间尼索地平原料药中3种有机溶剂残留量的气相色谱测定方法。方法:采用毛细管气相色谱法,以二甲基甲酰胺为溶剂,HP-INNOWax毛细管柱(30m×0.53mm×1.0μm),FID检测器。结果:3种有机溶剂丙酮、甲醇、乙醇均达到了完全分离,在考察的浓度范围内具有良好线性,丙酮、甲醇、乙醇的最低检测浓度分别为0.08,0.06,0.08μg·mL-1,精密度RSD均小于2.0%,平均回收率为95%～105%。样品均符合要求。结论:该方法灵敏度、准确度均达到有机溶剂残留量的检测要求,可用于间尼索地平原料药中3种残留溶剂的同时检测与分析。Objective：To develop a capillary GC method for simultaneous determining the residual organic solvents acetone, methanol and ethanol in m - nisoldipine. Methods： The samples were dissolved in N, N - dimethylformamide. The three organic solvents were separated on a HP - INNOWax capillary column （ 30 m ×0.53 mm × 1.0 μm） using programmable increased temperature. The intial temperature was kept at 50 ℃ for 2 rain and then up to 80 ℃ at the rate of 5 ℃ · min^-1 for 1 min and eventually raised to 180 ℃ at the rate of 40 ℃ ~ min-I for 5 min. Results： Three residual organic solvents eonsisting of acetone, methanol and ethanol in m - nisoldipine were completely separated. It appears a good linearity in the experimental concentration. The limit of detection for acetone, methanol and ethanol were 0. 08, 0. 06 and 0. 08 μg·mL^-1 , respectively. The RSD values of precision were all less than 2. 0%. The average recoveries were 95% - 105% and the samples coincided with the requirements. Conclusion ： The method was proved to be accurate and sensitive after validation. It is suitable to determine residual organic solvents in m- nisoldipine.

关 键 词：气相色谱法 残留有机溶剂 间尼索地平 

分 类 号：R917[医药卫生—药物分析学]