大黄消痔栓的工艺改进及有效成分含量测定

Technological Improvement of Dahuang Xiaozhi Suppository and Determination of Its Active Components

目的改进大黄消痔栓的制备工艺,并对有效成分含量进行测定。方法在栓剂成型的前提下,以工艺中混合脂肪酸甘油酯与蜂蜡比例、灌模温度、脱模冷却时间为考察因素,以栓剂外观形态、重量差异、融变时限为评价指标,采用综合评分法评价制得栓剂的优劣,优选最佳制备工艺;采用高效液相色谱法测定大黄中五种蒽醌类成分芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量。结果大黄消痔栓的最优制备工艺为混合脂肪酸甘油酯:蜂蜡=8∶1,灌模温度75℃,常温冷却脱模时间5 min;芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚分别在2.25~36.00μg·mL^(-1)、1.36~21.76μg·mL^(-1)、1.90~30.40μg·mL^(-1)、1.90~30.40μg·mL^(-1)、0.70~11.20μg·mL^(-1)浓度范围内与峰面积呈良好线性关系(r分别为0.9995、0.9996、0.9996、0.9995、0.9997);精密度、重复性试验结果RSD值均小于2%;样品在12 h内峰面积RSD均小于2%;平均加样回收率均在96.0%~103.5%内,RSD均小于2%。结论该工艺下制备的大黄消痔栓成形性好,不需冷冻,常温冷却脱模时间短,重量差异及融变时限符合规定,工艺可行性高;含量测定方法重复性好,专属性强,结果可靠,可用于该栓剂的质量控制。

Objective:To improve the preparation technology of Dahuang Xiaozhi suppository and determine the content of effective components. Methods: On the premise of suppository forming, the proportion of mixed fatty acid glyceride and beeswax, pouring temperature and cooling time of demoulding were taken as the factors, and the appearance, weight difference and melting time of suppository were taken as the evaluation indexes. The quality of suppository was evaluated by comprehensive scoring method, and the best preparation process was optimized. Five anthraquinones in Rhubarb were determined by HPLC.The contents of emodin, rhein, emodin, chrysophanol and physcion were determined. Results:The optimal preparation process of Dahuang Xiaozhi suppository was as follows: mixed fatty acid glyceride: beeswax = 8∶1, injection temperature: 75 ℃, room temperature cooling demoulding time: 5 min;aloe emodin, rhein, emodin, chrysophanol, physcion were 2.25 ~ 36.00 μ g · ml^(-1), 1.36 ~ 21.76 μ g · ml^(-1), 1.90 ~ 30.40 μ g · ml^(-1), 1.90 ~ 30.40 μ g · ml^(-1), 0.70 ~ 11.20 μ g · ml^(-1), respectively.There was a good linear relationship between the concentration range and the peak area(r = 0.9995, 0.9996, 0.9996, 0.9995, 0.9997), the RSD values of precision and repeatability were less than 2%, the RSD values of peak area within 12 h were less than 2%, and the average recoveries were 96.0%-103.5%, RSD values were less than 2%. Conclusion:Dahuang Xiaozhi suppository prepared by this process has good formability, no need of freezing, short time of demoulding at room temperature, weight difference and melting time, and high feasibility;the content determination method has good repeatability, strong specificity and reliable results, which can be used for the quality control of the suppository.