【作者】 李正翔； 金晶；

【机构】 天津医科大学总医院；

【摘要】 目的:制备复方红藤颗粒剂及建立其质量控制方法。方法:选用Kromasil C18色谱柱(250mm×4.6mm,5μm),流动相为甲醇-0.6%磷酸水溶液(85∶15),检测波长为290nm,流速为1.0mL/min,柱温为25℃。以此色谱条件作为复方红藤颗粒剂中大黄素的含量测定方法。利用正交试验,对影响大黄素提取的三个重要因素即加水量、提取时间和提取次数进行考察,筛选出最佳提取工艺,并制备颗粒剂。利用TLC对复方红藤颗粒剂中绿原酸进行薄层鉴别:将绿原酸对照品液及供试品液点于同一以羧甲基纤维素钠为黏合剂的硅胶H薄层板上,以乙酸丁酯-甲酸-水(7:2.5:2.5)为展开剂,展开并置紫外光灯(365nm)下检视。选用Kromasil C18色谱柱(250mm×4.6mm,5μm),流动相为甲醇-0.6%磷酸水溶液(85∶15),检测波长为265nm,流速为1.0mL/min,柱温为25℃。在此条件下建立复方红藤颗粒剂的HPLC指纹图谱。结果:大黄素进样量在0.1600μg～0.5200μg范围内线性关系良好,r=0.9999,平均回收率为102.7%,相对标准偏差(RSD)为1.27%。按正交试验筛选出的提取条件即加8倍量水、提取3次、每次提取2小时制备出颗粒剂,建立了复方红藤颗粒剂的HPLC指纹图谱。结论:本试验科学地筛选了药物提取条件,制备了颗粒剂,建立以大黄素为定量指标的含量测定方法,该方法操作简便、结果准确、重现性好,可以作为复方红藤颗粒剂的质量控制方法;指纹图谱的建立有助于全面地控制复方红藤颗粒剂的质量。更多还原

【Abstract】 Objective: Prepared fufanghongteng granules and established the quality control method. Methods: Kromasil C18 column (250mm×4.6 mm,5μm)was used. The mobile phase was methanol-0.6%H3PO4 (85:15).The detective wavelength was 290 nm and flow rate was 1.0 mL/ min. Column temperature was 25℃.This HPLC condition was the assay method of emodin in fufanghongteng granules . Orthogonal test was performed to choose volume of water, extracting time and times and decide the best condition, then prepared the granules. Chlorogenic acid in fufanghongteng granules was carried out thin-layer identification by TLC: chlorogenic acid standard solution and sample solution were on the same thin-layer plate which was made by silica gela H adhered with CMC-Na, developing solution was butyl acetate-formic acid-water(7:2.5:2.5), and inspected under the ultraviolet lamp(365nm).The HPLC fingerprint was established with Kromasil C18 column,the mobile phase of methanol-0.6%H3PO4 (85:15), the detective wavelength of 265 nm , the flow rate of 1.0 mL/ min and the column temperature of 25℃. Results: The linear range was 0.1600μg～0.5200μg, r = 0.9999.The average recovery was 102.7% with RSD 1.27%. Prepared the granules under the condition of 8 times water, extracting 3 times and each time 2 hours. The HPLC fingerprint was established. Conclusion: This experiment selected the extracting condition, prepared granules and established the assay method which used emodin to be the quantitation index.This method was easy to operate with accurate result and good reproducibility, and can be used to control the quality of fufanghongteng granules. Establishing the HPLC fingerprint can be helped to roundly control the quality of fufanghongteng granules.更多还原