摘要
目的建立盐酸普拉克索中残留溶剂的测定方法。方法盐酸普拉克索中甲醇、乙醇、丙酮、异丙醇和四氢呋喃的残留量采用顶空进样毛细管气相色谱法,DB-624毛细管柱,FID检测器,柱温采用程序升温。结果各有机溶剂均能得到有效分离,甲醇的浓度在59.87-374.20μg/ml范围内线性关系良好（r=0.9991）,平均回收率为97.40%,RSD为1.26%;乙醇的浓度在100.60-628.75μg/ml范围内线性关系良好（r=0.9991）,平均回收率为96.79%,RSD为1.58%;丙酮的浓度在100.22-626.38μg/ml范围内线性关系良好（r=0.9992）,平均回收率为96.55%,RSD为1.80%;异丙醇的浓度在99.78-623.65μg/ml范围内线性关系良好（r=0.9992）,平均回收率为96.43%,RSD为1.55%;四氢呋喃的浓度在14.98-93.63μg/ml范围内线性关系良好（r=0.9995）,平均回收率为96.97%,RSD为2.22%。结论本方法可以准确测定盐酸普拉克索中的残留溶剂,可用于盐酸普拉克索原料药中有机溶剂的检测。
Objective To establish determination method of residual solvent in pramipexole dihydrochloride. Methods Residual amount of methanol,ethanol,acetone,isopropyl alcohol and tetrahydrofuran in pramipexole dihydrochloride was used headspace sampling capillary gas chromatography,DB-624 capillary column,FID detector and temperature programme was used for column temperature. Results The organic solvent can be effectively separated.The linear relationship was well when concentration of methanol in 59.87-374.20 μg/ml scope（r=0.9991）.Average recovery rate was 97.40%,RSD was1.26%.The linear relationship was well when concentration of ethanol in 100.60-628.75 μg/ml scope（r=0.9991）.Average recovery rate was 96.79%,RSD was 1.58%.The linear relationship was well when concentration of acetone in 100.60-628.75 μg/ml scope（r=0.9992）.Average recovery rate was 96.55%,RSD was 1.80%.The linear relationship was well when concentration of isopropyl alcohol in 99.78-623.65 μg/ml scope（r=0.9992）.Average recovery rate was 96.43%,RSD was1.55%.The linear relationship was well when concentration of tetrahydrofuran in 14.98-93.63 μg/ml scope（r=0.9995）.Average recovery rate was 96.97%,RSD was 2.22%. Conclusion This method can accurately determine residual solvent in hydrochloric acid pramipexole,and can be used for analysis of organic solvent determination of raw material medicine in hydrochloric acid pramipexole.
出处
《中国当代医药》
2015年第35期7-10,共4页
China Modern Medicine
关键词
顶空进样毛细管气相色谱法
盐酸普拉克索
残留溶剂
Headspace sampling capillary gas chromatography
Pramipexole dihydrochloride
Residual solvent
