摘要
目的:测定胰激肽原酶中乙酸、乙醇、乙醚、丙酮的残留量。方法:采用顶空气相色谱法,FID检测器,分别以键合和改性的交联聚乙二醇为固定液的毛细管柱和6%氰丙基苯基-94%二甲基聚硅氧烷为固定液的毛细管柱为色谱柱,程序升温,顶空温度为85℃,平衡时间30 min,进样口温度250℃,检测器温度250℃,载气为氮气,以水为溶剂配制对照品溶液及样品溶液,采用外标法定量。结果:4种残留溶剂在对应于限度的50%～150%浓度范围内有良好的线性关系(r=0.996 6～0.999 5),平均回收率为97.8%～103.7%。结论:该法简便,结果准确,适用于胰激肽原酶中有机溶剂残留量的测定。
Objective： A method was developed for the determination of the Acetic acid, Ethanol, Ethylether, Acetone in Pancreatic Kininogenase by HS-GC. Method： System 1 ： The analytical column was Agilent FFAP （ 30 m × 0. 32 mm, 1.8 um）, System 2 ： Agilent DB-624 （30 m × 0. 32 mm, 1.8 um） . The injector temperature was 250 ℃ and the detector temperature was 250 ℃. The column temperature was programmed raised. The carrier gas was nitrogen, and the solvent was water. The acetic acid, ethanol, ethylether, acetone were quantified external standard. Results： The correlation coefficients of linearity ranged from 0. 996 6 to 0. 999 5 for the four residual solvents within the concentration of 50% to 150% of relative individual limit specified. The average recovery was 97. 8% to 103.7%. Conclusions： This method is convenient and quick for the quantitative determination of the acetic acid, ethanol, ethylether, acetone in Pancreatic Kininogenase, and can be used for the quality control.
出处
《中国药品标准》
CAS
2012年第6期451-454,共4页
Drug Standards of China
关键词
顶空气相色谱法
胰激肽原酶
有机溶剂
残留量
HS-GC
Pancreatic Kininogenase
acetic acid
ethanol
ethylether
acetone
