Abstract:ObjectiveTo establish quality standards for Guanxinping Tablet. MethodsRadix Angelicae Sinensis,Pericarpium Trichosanthis and Radix Notoginseng were identified by TLC, and the content of polysaccharides was determined by UVspectro. photometry. ResultsThe TLC spots developed were quite clear. The hightest content was 14.76% , the lowest content was 12.24%, the average content of polysaccharides was 13.36%. The average recouery of polysaccharides was 97.38%,with RSD of 5.51%, respectively . ConclusionThe method is convenient, reliable. It is one of the ways that can be used for the quality control of Guanxinping tablet.
精密称取105 ℃ 干燥至恒重的葡萄糖对照品36.3 mg,置100 ml 量瓶中,加水溶解并稀释至刻度,摇匀,即得(每毫升中含无水葡萄糖0.363 mg)。
2.2.2 测定波长的选择
精密吸取对照品溶液0.1 ml,置10 ml 具塞刻度试管中,加水至2.0 ml 摇匀,在冰水浴中缓缓滴加0.2%蒽酮-硫酸溶液至刻度,混匀,放冷后置水浴中保温10 min ,取出,立即置冰水浴中冷却10 min ,取出,以相应试剂为空白,在400 ~700 nm波长范围内扫描,绘制吸收光谱,结果表明,葡萄糖在528 nm处有最大吸收。
2.2.3 标准曲线的制备
精密量取对照品溶液0.1,0.2 ,0.3,0.4,0.5, 0.6 ml分别置10 ml 具塞刻度试管中,各加水至2.0 ml 摇匀,在冰水浴中缓缓滴加0.2%蒽酮-硫酸溶液至刻度,混匀,放冷后置水浴中保温10 min ,取出,立即置冰水浴中冷却10 min ,取出,以相应试剂为空白。照紫外-分光光度法,在528 nm 波长处测得吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线。见图4。
取已知含量的成品(批号041111)2片,研细,精密称定,加80%的乙醇100 ml,加热回流1 h,滤过,滤渣用80%的乙醇洗涤3次后,再精密加入105 ℃ 干燥至恒重的葡萄糖对照品后,加水100 ml回流提取1 h,滤过,滤液置200 ml容量瓶中,加水至刻度,摇匀,精密量取此液0.2 ml,按“标准曲线的制备”项下“各加水至2.0 ml 摇匀,在冰水浴中缓缓滴加0.2%蒽酮-硫酸溶液至10 ml 刻度”起操作,依法测得吸光度。结果见表1。表1 回收率实验结果(略)
2.6 样品的测定
取本品4片,研细,精密称定,置圆底烧瓶中,加80%乙醇150 ml ,置水浴中回流1 h,趁热滤过,残渣用80%热乙醇洗涤3次,10 ml/次,将残渣及滤纸置烧瓶中,加水150 ml,置沸水浴中加热回流1 h,趁热滤过,残渣及烧瓶用热水洗涤4次,10 ml/次,合并滤液及洗液,放冷,转移至250 ml 量瓶中,加水至刻度,摇匀,精密量取0.1 ml, 置10 ml 具塞干燥试管中,按“标准曲线的制备”项下“各加水至2.0 ml 摇匀,在冰水浴中缓缓滴加0.2%蒽酮-硫酸溶液至10 ml 刻度”起操作,依法测得吸光度,计算样品含量。结果见表2。表2 冠心平多糖含量测定结果(略)