安太胶囊质量标准的提升研究

Study on the improvement of quality standard for Antai capsules

目的:完善和提高安太胶囊的质量标准。方法:采用薄层色谱法(TLC)对安太胶囊中大豆异黄酮、大黄、肉桂进行定性鉴别;采用高效液相色谱法(HPLC)对安太胶囊中大黄素进行含量测定,色谱柱为Kromasil C18(250mm×4.6mm,5μm),流动相为甲醇-0.1%磷酸溶液(97∶3),检测波长为290nm,流速为1.0mL·min^-1,柱温为室温,进样量为20μL。结果:在TLC图谱中,斑点清晰,分离度好,阴性样品无干扰。大黄素在4.4~22μg·mL^-1范围内与峰面积呈良好线性关系(r=0.9999),平均加样回收率为97.87%(RSD=1.8%,n=6),精密度、稳定性和重复性试验的RSD分别为0.32%、0.26%和0.19%(n=6),大黄素的平均含量为0.115mg/粒(n=3)。结论:该方法快速、准确、专属性强,可作为安太胶囊质量控制的方法,并初步拟定其有效成分大黄以大黄素(C15H10O5)计,每粒含大黄素不低于0.05mg。

OBJECTIVE To optimize and improve the quality standard for Antai capsules.METHODS Catherine genistein and Rhei radix et rhizome and Cinnamomi cortex were identified by TLC qualitatively.The content of emodin was determined by HPLC.The chromatographic separation were carried out by using Kromasil C18(250mm×4.6mm,5μm)column.The mobile phase consisted of methanol-0.1%phosphate solution(97∶3)for emodin at a flow rate of 1.0mL·min^-1,detection wavelength was 290nm,column temperature were 25℃,and the injection volume was 20μL.RESULTS In TLC of Catherine genistein and Rhei radix et rhizome and Cinnamomi cortex tset samples,same color spots were shown in the corresponding positions of the control chromatogram,spots were clear without any interference.The linearity of emodin was 4.4-22μg·mL^-1(r=0.9999).The average recovery was 97.87%(RSD=1.8%,n=6).RSDs of precision,stability and reproducibility tests were 0.32%,0.26%and 0.19%(n=6).The average content of emodin was 0.115mg in each capsule(n=3).CONCLUSION The method was fast,accurate and has good specificity and can be used for quality control of Antai capsules,and it was preliminarily formulated that its effective ingredient was calculated as emodin(C15H10O5)and the content is not less than 0.05mg in each capsule.