毛细管气相色谱法测定利拉奈酯原料药中溶剂残留量

Determination of Residual Organic Solvents in Liranaftate by Capillary Gas Chromatography

目的:建立测定利拉奈酯原料药中丙酮、甲醇、乙醇、三氯甲烷4种有机溶剂残留量的方法。方法:采用毛细管气相色谱法。色谱柱为INNOMAX石英毛细管柱,柱温采用程序升温,检测器为氢火焰离子化检测器,检测器温度为250℃,进样口温度为200℃,载气为氮气,流速为3·0mL·min-1,分流比为1:1,进样量为1μL。结果:丙酮、甲醇、乙醇、三氯甲烷的检测浓度线性范围分别为0·05～1·1(r=0·9999)、0·03～0·6(r=0·9995)、0·05～1·0(r=0·9996)、0·0018～0·012mg·mL-1(r=0·9999);平均回收率为97·7%～101·4%(RSD为2·2%～5·7%);4批样品中4种有机溶剂残留量均符合《中国药典》2010年版要求。结论:该方法操作简便、精密度好,结果准确、可靠。

OBJECTIVE：To establish a method for the content determination of residual organic solvents in liranaftate,i.e.acetone,methanol,alcohol and chloroform.METHODS：Capillary gas chromatography was adopted.The determination was separated on INNOMAX capillary column using temperature programming.FID was used as detector with a temperature of 250 ℃,and the inlet temperature was 200 ℃.Nitrogen was used as carrier gas at the flow rate of 3.0 mL·min-1,the split ratio was 1：1 and the injection volume was 1 μL.RESULTS：The linear ranges of acetone,methanol,alcohol and chloroform were 0.05～1.1 mg·mL-1（r=0.999 9）,0.03～0.6 mg·mL-1（r=0.999 5）,0.05～1.0 mg·mL-1（r=0.999 6）,0.001 8～0.012 mg·mL-1（r=0.999 9）,respectively.The average recoveries ranged from 97.7%～101.4% with RSD of 2.2%～5.7%.The residual levels for the organic solvents in 4 batches of samples were all up to the standard stipulated in Chinese Pharmacopeia（2010 edition）.CONCLUSION：The method is simple,precise,accurate and reliable.