活血散的质量标准研究
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篇名: 活血散的质量标准研究
TITLE:
摘要: 目的:建立活血散的质量标准。方法:采用显微鉴别法对散剂中天南星、土鳖虫、黄柏、地肤子进行定性鉴别。采用高效液相色谱法对制剂中黄柏碱、虎杖苷、药根碱、小檗碱、大黄素的含量进行测定:色谱柱为ZORBAX  Eclipse  Plus C18,流动相为甲醇-0.1%磷酸(梯度洗脱),流速为0.4 ml/min,检测波长为240 nm,柱温为30 ℃,进样量为5 μl。结果:天南星、土鳖虫、黄柏、地肤子的显微鉴别图谱清晰。黄柏碱、虎杖苷、药根碱、小檗碱、大黄素检测进样量线性范围分别为0.159~5.073 μg(r=0.997 4)、0.149~4.761 μg(r=0.999 9)、0.239~7.649 μg(r=0.995 5)、0.165~5.268 μg(r=0.997 2)、0.012~0.382 μg(r=0.999 9);精密度、稳定性、重复性试验的RSD<3.0%;加样回收率分别为98.9%~104.1%(RSD=1.9%,n=6)、96.1%~101.7%(RSD=2.5%,n=6)、99.6%~105.1%(RSD=2.6%,n=6)、90.3%~98.2%(RSD=2.9%,n=6)、92.9%~96.4%(RSD=2.0%,n=6)。结论:该研究所建标准可用于活血散的质量控制。
ABSTRACT: OBJECTIVE: To establish the quality standard of Huoxuesan. METHODS: Microscopic identification method was adopted for the qualitative identification of Rhizoma pinelliae, Eupolyphaga seu, Phellodendron amurense and Fructus kochiae in the preparation. HPLC was adopted for the contents determination of phellodendrine,polydatin, jatrorrhizine, berberine and emodin: the column was ZORBAX  Eclipse  Plus C18 with methanol-0.1% phosphoric acid(gradient elution)at a flow rate of 0.4 ml/min, the detection wavelength was 240 nm, column temperature was 30 ℃, and the injection volume was 5 μl. RESULTS: Microscopic identification map of R. pinelliae, E. seu, P. amurense and F. kochiae was clear.  The linear range was  0.159-5.073 μg(r=0.997 4)for phellodendrine、0.149-4.761 μg(r=0.999 9)for polydatin、0.239-7.649 μg(r=0.995 5)for jatrorrhizine、0.165-5.268 μg(r=0.997 2)for berberine、0.012-0.382 μg(r=0.999 9)for emodin; RSDs of precision, stability and reproducibility tests were lower than 3.0%; recoveries were 98.9%-104.1%(RSD=1.9%,n=6), 96.1%-101.7%(RSD=2.5%,n=6), 99.6%-105.1% (RSD=2.6%,n=6), 90.3%-98.2% (RSD=2.9%,n=6) and 92.9%-96.4% (RSD=2.0%,n=6) respectively. CONCLUSIONS: The established standard can be used for the quality control of Huoxuesan.
期刊: 2016年第27卷第15期
作者: 赵颖,周芙琼,朱维娜,李文,谈瑄忠
AUTHORS: ZHAO Ying,ZHOU Fuqiong,ZHU Weina,LI Wen,TAN Xuanzhong
关键字: 活血散;显微鉴别;含量测定;黄柏碱;虎杖苷;药根碱;小檗碱;大黄素
KEYWORDS: Huoxuesan; Microscopic identification; Content determination; Phellodendrine; Polydatin; Jatrorrhizine; Berberine; Emodin
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