顶空气相色谱法测定聚普瑞锌中的残留溶剂

Determination of Residual Organic Solvents in Sevelamer Hydrochloride Drug Substance by Headspace Gas Chromatography

关键词:  顶空气相色谱法  聚普瑞锌  残留溶剂

Key words:  HS-GC  polaprezinc  residual organic solvents

摘要:

目的 建立以顶空气相色谱法测定聚普瑞锌原料药中甲醇、乙醇、三氯甲烷和甲苯4种有机溶剂残留量的方法。方法 以1 mol·L^-1硫酸溶液为溶剂，采用Agilent DB-FFAP(30 m×0.32 mm，0.5 μm)毛细管柱，载气为氮气，柱流速为2 mL·min^-1；柱温为程序升温，氢火焰离子化检测器(FID)，检测器温度为250 ℃；进样口温度为200 ℃；顶空瓶平衡温度为80 ℃。结果 甲醇、乙醇、三氯甲烷和甲苯均能较好的分离，呈现良好的线性关系，平均回收率分别为102.9%，105.4%，93.8%，95.7%，RSD分别为2.9%，2.1%，3.3%，3.5%(n=9)。结论 本方法简便快速，准确性好，灵敏度高，可用于聚普瑞锌原料药中残留溶剂的测定，同时也为难溶性原料药中的残留溶剂测定提供一个思路。

Abstract:

OBJECTIVE To establish an HS-GC method for the determination of residual organic solvents including menthanol, alcohol, trichloromethane and toluene in polaprezinc. METHODS The samples were dissolved in 1 mol·L^-1 sulfuric acid solution, and this method utilized an Agilent DB-FFAP GC column, nitrogen as carrier gas. FID was used as detector with the temperature of 250 ℃, and the inlet temperature was 200 ℃. This method used temperature program. RESULTS The four residual organic solvents menthanol, alcohol, trichloromethane and toluene were completely separated, the linear relationship was good, and the average recoveries were 102.9%, 105.4%, 93.8% and 95.7%, and the RSD were 2.9%, 2.1%, 3.3%, 3.5%(n=9), respectively. CONCLUSION This method is simple, rapid, accurate and highly sensitive, which can be used for the determination of the residual organic solvents in polaprezinc. Also provide a way of determination of residual organic solvents in slightly soluble crude drug.