毛大丁草药材的质量标准提升
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篇名: 毛大丁草药材的质量标准提升
TITLE: Improvement of the quality standard of Gerbera piloselloides
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(24h)、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、0.0469~0.6780mg/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%。
ABSTRACT: OBJECTIVE To improve th e 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 (part Ⅳ). 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 unde r 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 we re 3.87-154.88,1.64-65.41,1.60-64.00,1.92-76.96, 1.27-50.93,0.40-15.89 μg/mL,respectively(r≥0.999 1). 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 0.152 7-0.852 2, 0.084 5-0.669 7,0.136 7-0.961 0,0.126 0-1.193 2,0.128 8-1.102 2,0.046 9-0.678 0 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%.
期刊: 2022年第33卷第04期
作者: 杨贵香,吴莹莹,马雪,刘春花,郑林,李勇军,王永林
AUTHORS: YANG Guixiang ,WU Yingying ,MA Xue,LIU Chunhua ,ZHENG Lin,LI Yongjun ,WANG Yonglin
关键字: 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
KEYWORDS: Gerbera piloselloides;quality standard ;high performance liquid chromatography method ;property identification ;
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