摘要
目的:提升双石通淋胶囊质量标准.方法:采用薄层色谱(TLC)法对制剂中粉萆薢进行定性鉴别;采用高效液相色谱(HPLC)双波长法测定制剂中的盐酸小檗碱、丹参酮ⅡA、京尼平苷酸、苍术素的含量,色谱柱为Welch XtimateC18 4.6 mm × 150 mm,3 μm,以乙腈为流动相A,以0.1％磷酸溶液(含0.02 mol/L磷酸二氢钠)为流动相B,进行梯度洗脱,流速为0.8 mL/min,检测波长为254 nm和345 nm,柱温为30℃,进样量为10 μL.结果:粉萆薢的TLC图斑点清晰,分离度高,阴性样品无干扰.盐酸小檗碱、丹参酮ⅡA、京尼平苷酸、苍术素的浓度分别在6.196～198.257 μg/mL、1.598～51.131 μg/mL、6.364～203.656 μg/mL、0.156～4.985 μg/mL 范围内与峰面积线性关系良好;精密度、稳定性、重复性试验RSD均小于2.0％;平均加样回收率分别为99.25％、99.95％、98.13％、98.20％,RSD分别为2.50％、2.80％、1.38％、2.71％(n=6).结论:该方法操作简便、结果准确、重复性好,可用于提升双石通淋胶囊的质量标准.
Abstract
Objective To improve the existing quality standard of Shuangshi Tonglin Caspules.Methods The thin-layer chroma-tography(TLC)method was used to identify Dioscoreae Hypoglaucae Rhizoma in preparation qualitatively.The high-performance liquid chromatography(HPLC)-dual wavelength method was used to determine the contents of Berberine Hydrochloride,Tanshi-none ⅡA,Geniposidic Acid and Atractylodin in the preparation;the chromatographic column was Welch Xtimate C18 4.6 mm × 150 mm,3 μm,the mobile phase was acetonitrile-0.1％phosphoric acid aqueous solution(with 0.02mol/L sodium dihydrogen phos-phate),the flow rate was 0.8 mL/min,the detection wavelength was 254 nm and 345 nm,the column temperature was 30 ℃,and the injection volume was 10 μL.Results The TLC chromatography of Dioscoreae Hypoglaucae Rhizoma showed clear spots,high reso-lution,and no interference from the negative reference.The linear ranges of Berberine Hydrochloride,Tanshinone ⅡA,Geniposidic Acid,Atractylodin were 6.196-198.257 μg/mL,1.598-51.131 μg/mL,6.364-203.656 μg/mL,0.156-4.985 μg/mL re-spectively.The RSDs of precision,stability and repeatability were all lower than 2.0％.The average recovery rates of Berberine Hydrochloride,Tanshinone ⅡA,Geniposidic Acid,Atractylodin were 99.25％,99.95％,98.13％,98.20％,with RSD of 2.50％,2.80％,1.38％,2.71％respectively(n=6).Conclusion This method is simple,accurate and repeatable,which can be used to improve the quality standard of Shuangshi Tonglin Caspules.
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