目的 對(duì)鹽酸川芎嗪在凍干制備工藝中的穩(wěn)定性進(jìn)行考察，為保障含有該成分的其他凍干粉針劑產(chǎn)品的質(zhì)量提供依據(jù)。方法 采用HPLC法測(cè)定鹽酸川芎嗪的量。色譜條件：流動(dòng)相為甲醇-水（45：55），體積流量為1.0 mL/min，柱溫25℃，進(jìn)樣量10 μL，檢測(cè)波長為295 nm。檢測(cè)鹽酸川芎嗪在升華干燥0、12、24、48 h后的含量變化。結(jié)果 鹽酸川芎嗪在10.5~168 μg/mL內(nèi)呈良好的線性關(guān)系，回歸方程為Y=25.837X+10.669（R²=1）。此方法檢測(cè)鹽酸川芎嗪在升華干燥12 h后含量減少9%，24 h其含量減少40%以上，48 h幾乎完全損失。結(jié)論 鹽酸川芎嗪在冷凍干燥過程中隨時(shí)間延長會(huì)因升華而使含量損失加重。

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.

國家科技部國際科技合作專項(xiàng)（2010DFA31890）；中國中醫(yī)科學(xué)院自主選題研究項(xiàng)目（ZZ2013003）