摘要
目的:建立伊曲康唑薄膜衣片中2种有机溶剂二氯甲烷和乙醇残留量的顶空气相色谱测定法。方法:采用顶空进样毛细管气相色谱法,色谱柱为 DB-624石英毛细管柱,载气:氮气,FID 检测器,程序升温:起始柱温50℃维持5min,再以90℃·min^(-1)升温至120℃,维持5min。测定了伊曲康唑薄膜衣片中二氯甲烷与乙醇的残留量。结果:2种有机溶剂完全分离,二氯甲烷与乙醇分别在0.0909~0.00606mg·mL^(-1)及0.7539~0.05026mg·mL^(-1)范围内具有良好线性,相关系数分别为0.9994和0.9999,平均回收率分别为99.1%和92.1%(n=5)。结论:该方法准确,灵敏,重现性好。
Objective:To establish a method for determination of residual solvents dichloromethane and ethanol in itraconazole film - coated Tablets. Method: The residual dichloromethane and ethanol in the preparation were quantitatively determined by headspace GC on DB -624 column,with FID detector, nitrogen as the carrier gas. Column temperature(Program Temperature) :50 ℃ (5 min) 90 ℃ · min^-1 120 ℃ (5 min). Result:The two residual solvents were separated completely. A good linearity of dichloromethane and ethanol were obtained from 0. 0909 - 0. 00606 mg ·mL^-1 (r =0. 9999) and 0. 7539 -0. 05026 mg·mL^-1 respectively. The mean recovery of dichloromethane and ethanol were 99. 1% (RSD =4. 5% ,n =5) and 92. 1% (RSD =3.2% ,n =5) respectively. Conclusion :The method is accurate, sensitive with good reproducibility.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2006年第6期862-864,共3页
Chinese Journal of Pharmaceutical Analysis