地骨皮药材的质量标准提升研究

Study on the improvement of quality standard for Lycii Cortex

目的:提升地骨皮药材的质量标准。方法:观察地骨皮药材的性状鉴别,采用显微鉴别和薄层色谱法对27批不同产地的地骨皮药材进行鉴别,按照2020年版《中国药典》(四部)通则中的方法,测定地骨皮的杂质、水分、总灰分、酸不溶性灰分、水溶性浸出物,建立高效液相色谱法测定该药材中地骨皮甲素和地骨皮乙素的含量。结果:地骨皮药材呈筒状或槽状,外表面灰黄色至棕黄色,有不规则裂纹,易成鳞片状剥落,质脆,易折断,断面外层黄棕色,内层灰白色;其粉末呈浅棕色,显微特征清晰,可见众多砂晶、纤维、淀粉粒、木栓细胞等。TLC鉴别结果显示,在供试品色谱图中,与对照品(东莨菪苷)色谱相应位置上显相同颜色的荧光斑点。27批药材的水分、总灰分、酸不溶性灰分、水溶性浸出物的含量分别为5.0%~10.6%、4.5%~22.6%、0.1%~2.9%、5.5%~23.4%。含量测定方法学考察结果均符合药典要求;27批地骨皮样品中地骨皮乙素、地骨皮甲素的含量分别为0.000%~0.143%、0.000%~1.109%。结论:本研究在地骨皮药材已有质量标准的基础,修订了显微鉴别、TLC鉴别、总灰分等检查项,增加了杂质、水溶性浸出物和含量测定检查项。并初步拟定地骨皮药材中杂质不得过5%、水分不得过11.0%、总灰分不得过13.0%、酸不溶性灰分不得过3.0%、水溶性浸出物不得少于10.0%、地骨皮甲素和地骨皮乙素的总含量不得低于0.50%。

Objective:To improve the quality standard of Lycii Cortex.Methods:The properties of Lycii Cortex were observed.27 batches Lycii Cortex of different origin was identified by microscopic identification and thin layer chromatography.According to the method stated in 2020 edition of the general rules of the Fourth part of Chinese Pharmacopoeia,impurity,water content,total ash content,acid-insoluble ash content and water-soluble extract content were determined.High performance liquid chromatography(HPLC)method was used to determine the contents of Kukoamine A and Kukoamine B in Lycii Cortex.Results:The character of Lycii Cortex were tubular or trough,and the exterior surface was grayish yellow to brownish yellow.Lycii Cortex had irregular cracks,and easy to flake off in scales.Tts texture was brittle and easy to break.The outer cross section was yellowbrown,and the inner cross section was gray-white.Its powder were light brown,and the microscopic features of the powder were clear,and numerous calcium oxalate alluvial gold,fibers,starch grains,cork cell were all found.The results of TLC identification showed that there were fluorescent spots of the same color in the chromatogram of Lycii Cortex and the corresponding position of substance control(Scopolin).The content ranges of water content,total ash content,acid-insoluble ash content and watersoluble extract were 5.0%-10.6%、4.5%-22.6%、0.1%-2.9%、5.5%-23.4%,respectively.The results of content determination methodology Kukoamine A and Kukoamine B in 27 batches of Lycii Cortex were 0.000%-0.143%,0.000%-1.109%.Conclusion:On the basis of the original quality standard of Lycii Cortex,microscopic identification,TLC identification and total ash are revised.The examination items of impurity,water-soluble extract and content determination are added.It is preliminarily proposed that impurity content,water content,total acid-insoluble ash content and water-soluble extract content should not exceed 5%,11.0%,13.0%,3.0%and 10.0%,respectively.The total contents of Kukoamine A and Kukoamine B should not be less than 0.50%.