顶空毛细管气相色谱法测定地塞米松磷酸钠有机溶剂残留量  

Determination of residual organic volatile solvents in dexamethasone sodium phosphate by headspace gas chromatography

作　　者：安彦[1] 王卫[1] 唐素芳[1] 

机构地区：[1]天津市药品检验所

出　　处：《天津药学》2010年第4期12-14,共3页Tianjin Pharmacy

摘　　要：目的：建立地塞米松磷酸钠中有机溶剂残留量的测定方法。方法：顶空毛细管气相色谱法;色谱柱为DB-624（6%氰丙基苯基-94%二甲基聚硅氧烷）石英毛细管柱;程序升温,初始温度为40℃,以5℃/min升至120℃,保持1min测定;FID检测器;载气为氮气,以正丙醇为内标物测定地塞米松磷酸钠中甲醇、乙醇及丙酮的残留量。结果：3种溶剂及内标均可完全分离,各溶剂在考查范围内线性关系良好,相关系数r为0.9997~0.9998,平均加样回收率分别为100.7%、101.1%和108.8%,最低检出浓度分别为2.5、5.0和15μg/ml。结论：本方法灵敏、准确,适用于地塞米松磷酸钠中有机溶剂残留量的测定。Objective：To establish a method for determination of three residual organic solvents in dexamethasone sodium phosphate.Methods： Headspace gas chromatography system was constituted of a flame-ionization detector,a capillary column coated with 6% cyanopropylpolysiloxane and 94% dimethylpolysiloxane,and nitrogen gas as a carrier.The initial temperature of column was 40 ℃ and the temperature was slowly raised to 120 ℃ by the rate of 5 ℃/min and sustained for one minute.Under this chromatographic condition,three residual organic volatile solvents（methanol,ethanol and acetone） were determined with n-propyl alcohol as an internal standard.Results： Three residual organic volatile solvents and the internal standard were separated thoroughly.Each solvent had a good linear relationship between peak areas and concentrations,r ranging within 0.9997 and 0.9998.Average recoveries of the three volatile solvents were 100.7%,101.1% and 108.8% respectively,and limits of detection 2.5 μg/ml,5.0 μg/ml and 15 μg/mlrespectively.Conclusions： The method is sensitive,accurate,and suitable for the determination of residual organic solvents in dexamethasone sodium phosphate.

关 键 词：气相色谱 地塞米松磷酸钠 残留溶剂 

分 类 号：R927.11[医药卫生—药学]