论文部分内容阅读
目的建立同时测定调经丸中芍药苷、毛蕊花糖苷、阿魏酸、盐酸益母草碱、橙皮苷、丹皮酚、黄芩苷、川续断皂苷VI、柠檬苦素、白术内酯I、白术内酯III、茯苓酸12种成分的RP-HPLC方法。方法采用RP-HPLC法,色谱柱为Venusil MP C18(250 mm×4.6 mm,5.0μm);流动相为乙醇-乙腈(40∶60,A)和0.2%磷酸水溶液(B),梯度洗脱,体积流量0.8m L/min;柱温45℃。结果 12种指标成分芍药苷、毛蕊花糖苷、阿魏酸、盐酸益母草碱、橙皮苷、丹皮酚、黄芩苷、川续断皂苷VI、柠檬苦素、白术内酯I、白术内酯III、茯苓酸分别在0.5~50.0 mg/L(r=0.999 5)、0.1~10.0 mg/L(r=0.999 1)、0.2~20.0 mg/L(r=0.999 2)、0.3~30.0 mg/L(r=0.999 3)、4.0~400.0 mg/L(r=0.999 8)、0.2~20.0 mg/L(r=0.999 1)、0.6~60.0 mg/L(r=0.999 4)、1.5~150.0 mg/L(r=0.999 8)、7.0~700.0 mg/L(r=0.999 9)、0.5~50.0 mg/L(r=0.999 3)、0.5~50.0 mg/L(r=0.999 4)、1.0~100.0 mg/L(r=0.999 6)与峰面积呈良好的线性关系;精密度良好,RSD≤0.97%;重复性良好,RSD≤1.25%;加样回收率在98.5%~103.5%,RSD≤1.24%。供试品溶液在室温条件下24 h内稳定,RSD≤1.09%。12批次供试品中芍药苷、毛蕊花糖苷、阿魏酸、盐酸益母草碱、橙皮苷、丹皮酚、黄芩苷、川续断皂苷VI、柠檬苦素、白术内酯I、白术内酯III、茯苓酸质量分数分别为4.328~4.688、0.033~0.054、0.073~0.091、0.177~0.199、0.243~0.283、0.043~0.069、1.144~1.173、0.037~0.061、0.094~0.126、0.127~0.157、0.155~0.179、0.285~0.327 mg/g。结论所建立的方法快速、灵敏度高、准确度高、专属性好,为调经丸的质量控制提供依据。
OBJECTIVE To establish a method for the simultaneous determination of paeoniflorin, verbascoside, ferulic acid, Leonurine hydrochloride, hesperidin, paeonol, baicalin, dipsaciolide VI, limonin, atractylodes I, III, Pachyrin acid RP-HPLC method of 12 components. Methods The RP-HPLC method was used. The chromatographic column was Venusil MP C18 (250 mm × 4.6 mm, 5.0 μm). The mobile phase consisted of ethanol-acetonitrile (40:60, A) and 0.2% Volume flow 0.8m L / min; column temperature 45 ℃. Results 12 indicators of paeoniflorin, verbascoside, ferulic acid, Leonurine hydrochloride, hesperidin, paeonol, baicalin, Chuan Duan saponin VI, limonin, atractylen I, atracta lactone III, Pomacenic acid could be found in the range of 0.5-50.0 mg / L (r = 0.999 5), 0.1-10.0 mg / L (r = 0.999 1), 0.2-20.0 mg / L (r = 0.999 8), 0.2-20.0 mg / L (r = 0.999 1), 0.6-60.0 mg / L (r = 0.999 4) and 1.5-150.0 mg / (R = 0.999 9), 0.5-50.0 mg / L (r = 0.999 3), 0.5-50.0 mg / L (r = 0.999 4), 1.0-100.0 (r = 0.999 6) and the peak area showed a good linear relationship; good precision, RSD ≤ 0.97%; good repeatability, RSD ≤ 1.25%; sample recovery was 98.5% ~ 103.5%, RSD ≤ 1.24 %. The test solution was stable within 24 h at room temperature, RSD ≤ 1.09%. 12 batches of test for the paeoniflorin, verbascoside, ferulic acid, Leonurine hydrochloride, hesperidin, paeonol, baicalin, Chuan Duan saponin VI, limonin, atractylodes I, atractylodes III and Porosinic acid were 4.328 ~ 4.688,0.033 ~ 0.054,0.073 ~ 0.091,0.177 ~ 0.199,0.243 ~ 0.283,0.043 ~ 0.069,1.144 ~ 1.173,0.037 ~ 0.061,0.094 ~ 0.126,0.127 ~ 0.157,0.155 ~ 0.179,0.285 ~ 0.327 mg / g. Conclusion The established method is rapid, sensitive, accurate and specific, providing the basis for the quality control of Tiaojing Pills.