毛细管柱气相色谱法测定羟丙甲纤维素中甲氧基和羟丙氧基的含量
郑金琪 1,郑国钢 1,李会林 1,朱伟 2(1.
杭州 310015) 浙江省食品药品检验所,杭州 310004;2. 浙江大学城市学院医学与生命科学学院,
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(30 m×0.53 mm,3.0 μm);检测器: 氢火焰离子化检测器;柱温: 程序升温,100 ℃保持 10 min,然后以 50 ℃min-1 升温至 230 ℃,保持 2 min;进样口温度 200 ℃;检测器温度 250 ℃; 载气: 氮气;流速:3.0 mLmin-1.以正辛烷为内标物, 内标法定量.结果 甲氧基在(2.443～19.57) gL- 1 内与峰面积呈 良好的线性关系(r=0.999 1,n=7),回收率 98.8%(RSD=0.64% ,n=9);羟丙氧基在(0.4351～7.494) gL- 1 内与峰面积呈良好 的线性关系(r=0.999 5,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 供了切实可行的方法. 关键词:羟丙甲纤维素;甲氧基;羟丙氧基;气相色谱法 中图分类号:R917 文献标识码:A 文章编号:1001-2494(2009)20-1585-04 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
Determination of the of Contents Methoxy and Hydroxypropoxy in Hypromellose by GC ZHENG Jin-qi1, ZHENG Guo-gang1, LI Hui-lin1, ZHU Wei2 (1.Zhejiang Institute for Food and Drug Control, Hangzhou
310004, China;2. Medicine and Life Sciences College, Zhejiang University City College, Hangzhou 310015, China) ABSTRACT:OBJECTIVE To establish a capillary column GC method for the determination of methoxy and hydroxypropoxy Iodomethane and 2-iodopropane were obtained by the reactions of methoxy and
content in hypromellose. METHODS
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 m×0.53 mm, 3.0 m) 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 mLmin-1. The n-octane was used as internal standard. RESULTS There was a good linear relationship between the concentration of methoxy and hydroxypropoxy in the ranges of (2.443～19.57) - 1 (r=0.999 1, n=7) and (0. 435 1～7.494) gL- 1(r=0.999 5, gL 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 control of hypromellose was provided. KEY WORDS:hypromellose;methoxy;hydroxypropoxy;GC A selective, simple, accurate, feasible way for the quality

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