[关键词]
[摘要]
目的 对盐酸川芎嗪在冻干制备工艺中的稳定性进行考察,为保障含有该成分的其他冻干粉针剂产品的质量提供依据。方法 采用HPLC法测定盐酸川芎嗪的量。色谱条件:流动相为甲醇-水(45:55),体积流量为1.0 mL/min,柱温25℃,进样量10 μL,检测波长为295 nm。检测盐酸川芎嗪在升华干燥0、12、24、48 h后的含量变化。结果 盐酸川芎嗪在10.5~168 μg/mL内呈良好的线性关系,回归方程为Y=25.837X+10.669(R2=1)。此方法检测盐酸川芎嗪在升华干燥12 h后含量减少9%,24 h其含量减少40%以上,48 h几乎完全损失。结论 盐酸川芎嗪在冷冻干燥过程中随时间延长会因升华而使含量损失加重。
[Key word]
[Abstract]
Objective To study the stability of tetramethylpyrazine hydrochloride in the process of freeze-drying preparation, and to provide a basis for freeze-drying powder injections which contain tetramethylpyrazine hydrochloride. Methods To determinate the content of tetramethylpyrazine hydrochloride by High Performance Liquid Chromatography (HPLC). It was the chromatographic conditions that mobile phase constitution was methanol-water, and methanol:water= 45:55, flowing rate was 1.0 mL/min; and column temperature was 40℃, sample volume:10 μL. Detecting wavelength was set at 295 nm, and the content of tetramethylpyrazine hydrochloride at different sublimation-drying was detected at 0 h, 12 h, 24 h and 48 h. Results Tetramethylpyrazine hydrochloride showed good linear relationship between the concentration of 10.5 μg/mL and 168 μg/mL, and the regression equation was Y=25.837X + 10.669 (R2=1). The content of tetramethylpyrazine hydrochloride reduced respectively 9% and 50% at 12 h and 24 h during the course of sublimation-drying, and almost completely lost at 48 h. Conclusion The content of tetramethylpyrazine hydrochloride lost more with the extension of the course of freeze-drying process.
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[基金项目]
国家科技部国际科技合作专项(2010DFA31890);中国中医科学院自主选题研究项目(ZZ2013003)