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目的:建立采用差示扫描量热法(DSC)准确测定中药浸膏粉玻璃化转变温度的方法,为玻璃化转变理论在中药固体制剂过程中的应用提供参考。方法:利用DSC测定中药浸膏粉的玻璃化转变温度,确认中药浸膏粉存在玻璃化转变现象。通过单因素试验考察热历史、载气流速、升温速率、试样量等参数对中药浸膏粉玻璃化转变温度的影响,采用Dixion法考察测试方法的精密度。结果:DSC检测条件为载气氮气,载气流速40mL·min-1,升温速率10℃·min-1,试样量6mg。离群值分析表明在95%的置信度水平下,玻璃化转变温度测试满足试验方法的要求。当归、黄芪、板蓝根、山楂、枸杞子、菊花、大黄、参灵草的玻璃化转变温度分别为68.9,77.0,75.8,35.8,3.4,56.0,56.3,80.0℃。结论:建立的方法操作简便、精密度良好,适用于中药浸膏粉玻璃化转变温度的测定。
OBJECTIVE: To establish a method for the accurate determination of glass transition temperature of traditional Chinese medicine extract powder by differential scanning calorimetry (DSC), and to provide a reference for the application of glass transition theory in solid preparation of traditional Chinese medicine. Methods: The glass transition temperature of traditional Chinese medicine extract powder was determined by DSC, and the glass transition phenomenon of traditional Chinese medicine extract powder was confirmed. The single factor test was used to investigate the influence of heat history, carrier gas flow rate, heating rate and sample volume on the glass transition temperature of Chinese medicine extract powder. The precision of the test method was examined by Dixion method. Results: The conditions of DSC were nitrogen carrier gas, carrier gas flow rate 40mL · min-1, heating rate 10 ℃ · min-1 and sample amount 6mg. Outlier analysis shows that at 95% confidence level, the glass transition temperature test meets the requirements of the test method. Angelica, Astragalus, Radix, hawthorn, medlar, chrysanthemum, rhubarb, ginseng grass glass transition temperature was 68.9,77.0,75.8,35.8,3.4,56.0,56.3,80.0 ℃. Conclusion: The established method is simple and convenient to operate and has good precision. It is suitable for the determination of glass transition temperature of traditional Chinese medicine extract powder.