藏药悬钩木的质量标准研究
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篇名: 藏药悬钩木的质量标准研究
TITLE:
摘要: 目的:建立藏药悬钩木的质量标准。方法:从性状特征、显微特征、薄层色谱(TLC)等方面对药材进行定性鉴别;测定药材水分、灰分、浸出物的含量。采用高效液相色谱法测定药材中芦丁和金丝桃苷的含量,色谱柱为Diamonsil C18,流动相为乙腈-0.1%磷酸溶液(18 ∶ 82,V/V),流速为1.0 mL/min,检测波长为360 nm,柱温为30 ℃,进样量为10 μL。结果:药材表面呈灰红色至灰红褐色,有纵向皱沟,外皮易剥离,髓部较大、疏松、呈海绵状。药材粉末呈浅黄色,木纤维成束或单个散在,韧皮纤维较粗。药材样品中金丝桃苷的TLC图斑点清晰,分离度好;水分为6.71%~7.55%,总灰分为1.43%~1.67%,酸不溶性灰分为0.41%~0.48%,水浸出物为17.70%~19.31%,醇浸出物为13.76%~16.99%;金丝桃苷、芦丁检测质量浓度线性范围均为3.13~50 μg/mL(r分别为0.999 2、0.999 5)、定量限分别0.5、1.8 μg/mL,检测限分别为0.2、0.9 μg/mL,精密度、稳定性、重复性试验的RSD<2.0%(n=6),加样回收率分别为92.8%~98.8%(RSD=2.25%,n=9)、94.0%~98.6%(RSD=1.71%,n=9)。结论:药材水分、总灰分、酸不溶性灰分分别不得过10.0%、3.0%、0.6%;水浸出物、醇浸出物、芦丁和金丝桃苷总量分别不得少于15.0%、12.0%、1.0 mg/g。所建标准可用于藏药悬钩木的质量控制。
ABSTRACT: OBJECTIVE: To establish the quality standard of Tibetan medicine Rubus biflorus. METHODS: The qualitative identification was conducted from characters characteristics, microscopic characteristics, TLC. The contents of moisture, ash and extract were determined. HPLC method was adopted for content determination of rutin and hyperoside. The determination was performed on Diamonsil C18 column with mobile phase consisted of acetonitrile-0.1% phosphoric acid solution(18 ∶ 82,V/V) at the flow rate of 1.0 mL/min. The detection wavelength was set at 360 nm, column temperature was 30 ℃, and sample size was 10 μL. RESULTS: The surface of the medicinal material was grayish red to grey red brown, with longitudinal wrinkle grooves, and the peel was easy to peel off. The pith of the medicinal material was large, loose, sponge-like. The powder of the medicine was light yellow; wood fiber was bundle or scattered individually; bast fiber was thick. TLC spot of hyperoside was clear and well-separated. The contents of moisture, total ash, acid-insoluble ash, water-soluble extract and ethanol extract were 6.71%-7.55%, 1.43%-1.67%, 0.41%-0.48%, 17.70%-19.31% and 13.76%-16.99%. The linear range was 3.13-50 μg/mL for rutin (r=0.999 2)  and hyperoside (r=0.999 5). The limits of quantitation were 0.5,1.8 μg/mL, and the limits of detection were 0.2,0.9 μg/mL. RSDs of precision, stability and reproducibility tests were all lower than 2.0% (n=6). The recoveries were 92.8%-98.8%(RSD=2.25%,n=9),94.0%-98.6%(RSD=1.71%,n=9) . CONCLUSIONS: The moisture content, total ash and acid insoluble ash content of medicinal materials is not more than 10.0%, 3.0% and 0.6%, respectively. The total amount of water extract, alcohol extract, rutin and hyperoside is not less than 15.0%, 12.0%, 1.0 mg/g, respectively. Established standard can be used for quality control of Tibetan medicine R. biflorus.
期刊: 2018年第29卷第2期
作者: 马志良,多杰
AUTHORS: MA Zhiliang,DUO Jie
关键字: 藏药;悬钩木;质量标准;芦丁;金丝桃苷;薄层色谱法;高效液相色谱法
KEYWORDS: Tibetan medicine; Rubus biflorus; Quality standard; Rutin; Hyperoside;TLC;HPLC
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