气相色谱法测定盐酸法舒地尔中有机溶剂残留量(1)
 |
| 第1页 |
参见附件。
[摘要] 目的 建立气相色谱法测定盐酸法舒地尔中有机溶剂残留量的方法。 方法 采用气相色谱法，FID检测器，以毛细管色谱柱SE-54(30 m×0.53 mm，5.0 μm)为分析柱。柱温为程序升温，用初始柱温55℃平衡0.5 min，以40℃/min的速度升温至70℃，平衡1 min，以40℃/min的速度升温至180℃，平衡3 min 程序升温分别测定甲醇、二氯甲烷。用初始柱温50℃平衡3 min，以20℃/min的速度升温至180℃，平衡3min程序升温测定N，N-二甲基甲酰胺。载气为氮气，进样口温度200℃，检测器温度250℃。 结果 3种有机溶剂完全分离，在所考察的浓度范围内具有良好线性关系，3个溶剂相关系数均大于0.999 0，甲醇、二氯甲烷、N，N-二甲基甲酰胺的检测限分别为0.065 7、1.100 0、0.016 6 μg/mL，平均回收率分别为99.8%、98.4%、99.1%。 结论 本试验建立的方法简便灵敏，结果准确可靠，适用于盐酸法舒地尔原料药中有机溶剂残留量的检测。
[关键词] 盐酸法舒地尔；有机溶剂残留量；气相色谱法
[中图分类号] R284.2 [文献标识码] A [文章编号] 1673-7210(2012)02(b)-0114-03
Determination of the residual organic solvents in Fasudil hydrochloride by GC
FANG Haiyan1 FANG Xueqin2 LIU Yuansheng2
1.Lab of Biochemical Detection, Huangshi Institute for Food and Drug Control, Hubei Province, Huangshi 435000, China; 2.Huangshi Shixing Pharmaceutical Co., Ltd, Hubei Province, Huangshi 435003, China
[Abstract] Objective To establish a method for determination of residual organic solvents in Fasudil hydrochloride by headspace gas chromatography. Methods The residual solvents was determined by GC. The FID detector was adopted, SE-54 capillary column (30 m×0.53 mm, 5.0 μm) was used, the column temperature was programmed temperature, the initial column temperature was 55℃ maintained for 0.5 minutes and then raised (40℃/min) to 70℃ for 1 minute, raised (40℃/min) to 180℃ for 3 minutes for methanol and methylene chloride detection, respectively. The initial column temperature was 50℃ maintained for 3 minutes and then raised (20℃/min) to 180℃ for 3 minutes for N, N-dimethyl formamide detection. The carriergas was nitrogen, the inlet temperature was 200℃ and the detector temperature was 250℃. Results Three kinds of organic solvents methanol, methylene chloride and N, N-dimethyl formamide completely separated, they showed a good linearity within the designed range of concentration, all the correlation coefficients were above 0.999 0. Methanol, methylene chloride and N, N-dimethyl formamide minimum detectable concentrations were 0.065 7, 1 ......
您现在查看是摘要介绍页，详见PDF附件(2515kb)。