毛大丁草药材的质量标准提升

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%。

Improvement of the quality standard of Gerbera piloselloides

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%.