摘要
目的提升毛大丁草药材的质量标准。方法观察毛大丁草药材的性状并对其粉末进行显微鉴别;按2020年版《中国药典》(四部)通则方法测定该药材中的水分、总灰分、酸不溶性灰分和醇溶性浸出物;采用高效液相色谱法测定该药材中紫花前胡苷、木犀草素-7-O-β-D-芦丁糖苷、木犀草苷、芹菜素-7-O-β-D-芦丁糖苷、芹菜素-7-O-β-D-葡萄糖苷、异紫花前胡内酯的含量。结果毛大丁草药材呈皱缩状,密被灰白色绵毛;须根多数,表面呈灰褐色或灰棕色,质脆,易折断,断面呈黄白色,中央有一明显细小木心。其粉末呈棕褐色,镜下可见非腺毛、石细胞、草酸钙方晶、导管、纤维等。15批药材样品的水分、总灰分、酸不溶性灰分、醇溶性浸出物测定值分别为8.63%~11.34%、10.39%~14.93%、3.29%~6.37%、9.03%~15.02%,平均值分别为10.01%、12.26%、4.61%、12.36%。紫花前胡苷、木犀草素-7-O-β-D-芦丁糖苷、木犀草苷、芹菜素-7-O-β-D-芦丁糖苷、芹菜素-7-O-β-D-葡萄糖苷、异紫花前胡内酯的质量浓度分别在3.87~154.88、1.64~65.41、1.60~64.00、1.92~76.96、1.27~50.93、0.40~15.89μg/mL范围内与各自峰面积成良好的线性关系(r均不低于0.9991);精密度、稳定性(24 h)、重复性试验的RSD均小于3%;平均加样回收率分别为101.88%、100.89%、102.64%、95.75%、96.71%、103.48%,RSD分别为0.55%、0.43%、0.34%、0.49%、0.47%、0.37%(n=6);样品中上述6种成分的含量分别为0.1527~0.8522、0.0845~0.6697、0.1367~0.9610、0.1260~1.1932、0.1288~1.1022、0.0469~0.6780 mg/g。结论所建方法可用于毛大丁草药材的质量控制。初步拟定毛大丁草药材中水分不得过12.0%,总灰分不得过15.0%,酸不溶性灰分不得过6.0%,醇溶性浸出物不得少于9.0%,木犀草苷、芹菜素-7-O-β-D-葡萄糖苷的含量不得少于0.016%。
OBJECTIVE To improve the quality standard for Gerbera piloselloides.METHODS The properties of G.piloselloides were observed and microscopic identification was conducted for powder.The moisture,total ash,acid-insoluble ash and ethanol-soluble extract were detected according to the method stated in 2020 edition of Chinese Pharmacopoeia(partⅣ).The contents of nodakenin,luteolin-7-O-β-D-lutinoside,luteoloside,apigenin-7-O-β-D-lutinoside,apigenin-7-O-β-D-glucopyranoside and marmesin were determined by high performance liquid chromatography method.RESULTS G.piloselloides were shrunken,densely covered with thick white cotton wool,with many fibrous roots;the surface was taupe or gray-brown;its texture was brittle and easy to break;the cross section was yellow-white,and there was an obvious small wooden heart in the center.Its powder was tan,and non-glandular hairs,stone cells,calcium oxalate cubes,ducts,fibers could be seen under microscope.The measured values of moisture,total ash,acid-insoluble ash and alcohol-soluble extract for 15 batches of samples were 8.63%-11.34%,10.39%-14.93%,3.29%-6.37%and 9.03%-15.02%,respectively;average values were 10.01%,12.26%,4.61%,12.36%.The linear ranges of nodakenin,luteolin-7-O-β-D-rutinoside,luteoloside,apigenin-7-O-β-D-lutinoside,apigenin-7-O-β-D-glucopyranoside and marmesin were 3.87-154.88,1.64-65.41,1.60-64.00,1.92-76.96,1.27-50.93,0.40-15.89μg/mL,respectively(r≥0.9991).RSDs of precision,stability(24 h)and repeatability tests were all less than 3%.The average recoveries were 101.88%,100.89%,102.64%,95.75%,96.71%and 103.48%,respectively;RSDs were 0.55%,0.43%,0.34%,0.49%,0.47%and 0.37%,respectively(n=6);the contents of above 6 components were 0.1527-0.8522,0.0845-0.6697,0.1367-0.9610,0.1260-1.1932,0.1288-1.1022,0.0469-0.6780 mg/g.CONCLUSIONS The established method can be used for the quality control of G.piloselloides.It is preliminarily proposed that the moisture in G.piloselloides is not more than 12.0%;the total ash is not more than 15.0%,the acid-insoluble ash is not more than 6.0%,the alcohol-soluble extract is not less than 9.0%;the contents of luteoloside and apigenin-7-O-β-D-glucopyranoside are not less than 0.016%.
作者
杨贵香
吴莹莹
马雪
刘春花
郑林
李勇军
王永林
YANG Guixiang;WU Yingying;MA Xue;LIU Chunhua;ZHENG Lin;LI Yongjun;WANG Yonglin(Engineering Research Center for the Development and Application of Ethnic Medicine and TCM/State Key Laboratory of Functions and Applications of Medicinal Plants,Guizhou Medical University,Guiyang 550004,China;School of Pharmacy,Guizhou Medical University,Guiyang 550004,China;Dept.of Pharmacy,Bijie Medical College,Guizhou Bijie 551700,China;Guizhou Provincial Key Laboratory of Pharmaceutics,Guizhou Medical University,Guiyang 550004,China)
出处
《中国药房》
CAS
北大核心
2022年第4期408-412,424,共6页
China Pharmacy
基金
国家自然科学基金委-贵州喀斯特中心项目子课题(No.U1812403)
贵州省科技计划项目(No.黔科合支撑[2019]2779号,No.黔科合平台人才[2016]5677)。
关键词
毛大丁草
质量标准
高效液相色谱法
性状鉴别
显微鉴别
木犀草苷
芹菜素-7-O-β-D-葡萄糖苷
Gerbera piloselloides
quality standard
high performance liquid chromatography method
property identification
microscopic identification
cynaroside
apigenin-7-O-β-D-glucopyranoside
