摘要
目的建立毛细管柱GC法测定羟丙甲纤维素中甲氧基和羟丙氧基含量的方法。方法通过氢碘酸与羟丙甲纤维素中的甲氧基和羟丙氧基反应生成挥发性的碘甲烷和2-碘丙烷,毛细管柱GC法测定碘甲烷和2-碘丙烷来计算羟丙甲纤维素中甲氧基和羟丙氧基的含量。采用DB-624石英毛细管柱(30m×0.53mm,3.0μm);检测器:氢火焰离子化检测器;柱温:程序升温,100℃保持10min,然后以50℃·min-1升温至230℃,保持2min;进样口温度200℃;检测器温度250℃;载气:氮气;流速:3.0mL·min-1。以正辛烷为内标物,内标法定量。结果甲氧基在(2.443~19.57)g·L-1内与峰面积呈良好的线性关系(r=0.9991,n=7),回收率98.8%(RSD=0.64%,n=9);羟丙氧基在(0.4351~7.494)g·L-1内与峰面积呈良好的线性关系(r=0.9995,n=7),回收率99.1%(RSD=0.45%,n=9);分析了3批样品,甲氧基的含量为29.0%~29.4%,羟丙氧基的含量为8.48%~8.61%。结论本法专属性强,分离度高,操作简便,结果准确,为更好地控制羟丙甲纤维素的质量提供了切实可行的方法。
OBJECTIVE To establish a capillary column GC method for the determination of methoxy and hydroxypropoxy content in hypromellose. METHODS Iodomethane and 2-iodopropane were obtained by the reactions of methoxy and hydroxypropoxy in hypromellose. Their concentrations were determined and used for calculating the contents of methoxy and hyproxypropoxy of hypromellose by GC method. The separation was performed on a DB-624 quartz capillary column(30 mm×0.53 mm, 3.0 μm) with FID. The initial temperature of column was kept at 100 ℃ for 10 min, then raised to 230 ℃ for 2 min at the rate of 50 ℃·min-1. Injector temperature was 200 ℃. Detector temperature was was 250 ℃. Carrier gas was nitrogen. The flow rate was 3.0 mL.min-1. The n-octane was used as internal standard. RESULTS There was a good linear relationship between the concentration ofmethoxy and hydroxypropoxy in the ranges of (2.443-19.57) g.L 1 (r=0.999 1, n=7) and (0. 435 1--7.494) g.L-1(r=0.999 5, n=7) by the standard curve respectively. The average recoveries were 98.8% (RSD=0.64%, n=9) for methoxy and 99.1% (RSD=0.45%, n=9) for hydroxypropoxy. Three batches of samples were analyzed and the contents of methoxy and hydroxypropoxy were from 29.0% to 29.4% and from 8.48% to 8.61%. CONCLUSION A selective, simple, accurate, feasible way for the quality control of hypromellose was provided.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2009年第20期1585-1588,共4页
Chinese Pharmaceutical Journal
基金
浙江省科技厅大仪协作平台科研课题(2008F70049)