摘要
目的:建立毛细管柱GC法测定甲基纤维素中甲氧基含量的方法。方法:通过氢碘酸与甲基纤维素中的甲氧基反应生成挥发性的碘甲烷,通过GC法测定碘甲烷来计算甲基纤维素中甲氧基的含量。采用DB-624石英毛细管柱(30 m×0.53 mm×3.0μm);氢火焰离子化检测器,柱温为程序升温,100℃保持10 min,然后以50℃.min-1升至230℃,保持2 min;进样口温度200℃,检测温度250℃,载气为氮气;流速为3.0 mL.min-1。以正辛烷为内标物,内标法定量。结果:甲氧基在2.19～19.38 g.L-1浓度范围内与峰面积呈良好的线性关系(γ=0.999 7,n=7),回收率99.3%(RSD=1.14%,n=9)。分析了4批样品,甲氧基的含量为29.66%～30.31%。结论:本法专属性强、简便、准确,为更好地控制甲基纤维素的质量提供了切实可行的方法。
Objective：To establish GC method for the determination of methoxy content in methylcellalose. Methods：The determination of the amount of methyl iodide, which was gotten by methoxy in methylcellulose reacted with hydriodic acid ,was used for calculating the methoxy of methylcellulose. DB-624 quartz capillary column （30 m×0.53mm×3.0μm） and FID were used; Column temperature：temperature programmed ,initial temperature was kept at 100 ℃ for 10 rain, then raised to 230 ℃ for 2 min at the rate of 50 ℃C · min^-1 ; Injector temperature：200℃ ; Detector temperature：250℃ ; Carrier gas：nitrogen;Flow rate：3.0 mL · min^-1. The internal standard was n-octane. The internal calibration to quantify was adopted in the paper. Results ：The standard curve of methoxy as a good linear relationship in the range of 2. 19 - 19.38 g ·L^-1 （T =0. 999 7,n =7） ;The average recovery was 99.3% （RSD = 1.14% ,n =9） . Four batches of samples were analyzed, and the contents of methoxy were from 29. 66% to 30. 31%. Conclusion ：The method provided a selective, simple, accurate feasible way for controlling the quality of methylcellulose.
出处
《中国药品标准》
CAS
2009年第6期455-458,共4页
Drug Standards of China
