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目的:建立补肾祛瘀颗粒的质量标准。方法:采用薄层色谱(TLC)法对补肾祛瘀颗粒中的金樱子、菟丝子、制何首乌、紫草进行定性鉴别;采用紫外分光光度法测定补肾祛瘀颗粒中总多糖的含量;采用高效液相色谱(HPLC)法对补肾祛瘀颗粒中芦丁、槲皮素、金丝桃苷进行含量测定,色谱柱为BDS C18,流动相为乙腈-0.08%磷酸溶液(梯度洗脱),流速为1 mL/min,柱温为30 ℃,检测波长为370 nm,进样量为10 μL。结果:4种药材的TLC供试品色谱与对照品或对照药材在相应位置上呈现相同斑点或荧光。葡萄糖、芦丁、槲皮素、金丝桃苷的检测质量浓度线性范围分别为0.003~0.018 mg/mL、0.225~7.20 μg/mL、0.07~2.24 μg/mL、1.25~39.88 μg/mL(r=0.999 5或0.999 9,n=6),精密度、稳定性、重复性试验的RSD均≤3.80%(n=6),平均回收率分别为102.2%、101.2%、100.9%、101.0%(RSD=1.28%、2.93%、2.41%、1.59%,n=6),平均含量分别为0.46 g/g、5.48 μg/g、8.18 μg/g、102.88 μg/g(n=3)。结论:本研究建立的补肾祛瘀颗粒的质量标准准确可靠,可为补肾祛瘀颗粒的质量控制提供科学依据。
OBJECTIVE: To establish the quality standard for Bushen quyu granules. METHODS: TLC was used for qualitative identification of Rosa laevigata, Cuscuta chinensis, processed Fallopia multiflora and Lithospermum erythrorhizon in Bushen quyu granules. And then, the content of total polysaccharides in Bushen quyu granules was determined by UV spectrophotometry. HPLC method was used for the content determination of rutin, quercetin and hyperin in Bushen quyu granules. The determination was performed on BDS C18 column with mobile phase consisted of acetonitrile-0.08% phosphoric acid solution (gradient elution) at the flow rate of 1 mL/min. The column temperature was 30 ℃, and detection wavelength was set at 370 nm. The sample size was 10 μL. RESULTS: TLC test sample chromatogram of 4 medicinal materials showed the same spot or fluorescence at the corresponding position with the reference substance and control medicinal materials. The linear range of glucose, rutin, quercetin and hyperin were 0.003-0.018 mg/mL, 0.225-7.20 μg/mL, 0.07-2.24 μg/mL and 1.25-39.88 μg/mL(r=0.999 5 or 0.999 9, n=6). RSDs of precision, stability and reproducibility tests were all less than 3% (n=6). Average recoveries were 102.2%, 101.2%, 100.9%, 101.0% (RSD=1.28%, 2.93%, 2.41%, 1.59%, n=6). Average contents were 0.46 g/g, 5.48 μg/g, 8.18 μg/g and 102.88 μg/g(n=3). CONCLUSIONS: Established quality standard of Bushen quyu granules is accurate and reliable, and can provide scientific reference for quality control of Bushen quyu granules.
补肾祛瘀颗粒质量标准薄层色谱法紫外分光光度法多糖高效液相色谱法芦丁槲皮素金丝桃苷
Bushen quyu granulesQuality standardTLCUV spectrophotometryTotal polysaccharideHPLCRutinQuercetinHyperin
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