HPLC法同时测定利胆排石片中14个成分的含量

目的：建立同时测定利胆排石片中绿原酸、柚皮苷、橙皮苷、新橙皮苷、黄芩苷、汉黄芩苷、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、木香烃内酯、去氢木香内酯、大黄酚共14个成分的高效液相色谱法。方法：采用Phenomenex Luna 5u-C₁₈色谱柱（4.6 mm×250 mm，5 μm），以0.5%磷酸水溶液（A）-乙腈（B）为流动相，梯度洗脱，流速1 mL·min^-1，柱温30℃，检测波长：254 nm。结果：各待测组分分离度良好；绿原酸、柚皮苷、橙皮苷、新橙皮苷、黄芩苷、汉黄芩苷、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、木香烃内酯、去氢木香内酯、大黄酚14个成分在相应的范围内线性关系良好，相关系数（r）不低于0.999 1，精密度试验的RSD均小于2.0%；平均回收率为97.8%~100.7%。样品中14个测定成分的含量范围分别为0.05~0.25、0.00~4.30、0.28~1.03、1.39~34.45、2.85~5.71、0.32~0.97、0.89~1.43、0.06~0.33、0.05~0.26、0.43~0.95、0.09~0.38、0.04~0.12、0.03~0.14、0.22~0.54 mg·片^-1。结论：经方法学验证，本方法可用于利胆排石片中绿原酸、柚皮苷、橙皮苷、新橙皮苷、黄芩苷、汉黄芩苷、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、木香烃内酯、去氢木香内酯、大黄酚14个成分的含量测定。

Objective: To develop an HPLC method for simultaneous determination of chlorogenic acid, naringin, hesperidin, neohesperidin, baicalin, wogonoside, baicalein, aloeemodin, rhein, wogonin, emodin, costunolide, dehydrocostus lactone and chrysophanol in Lidanpaishi tablets. Methods: The chromatographic separation was on Phenomenex Luna 5u-C₁₈ column(4.6 mm×250 mm, 5 μm) with a mobile phase consisting of 0.5% phosphoric acid solution(A) -acetonitrile(B) in a gradient mode at 30℃. The flow rate was 1 mL·min^-1 and the UV detection wavelength was set at 254 nm. Results: Excellent chromatographic separation was achieved with good linearity (r ≥ 0.999 1) within the linear range of chlorogenic acid, naringin, hesperidin, neohesperidin, baicalin, wogonoside, baicalein, aloeemodin, rhein, wogonin, emodin, costunolide, dehydrocostus lactone and chrysophanol; RSD of the precision test was less than 2.0%. The average recoveries of the fourteen components were in the range of 97.8%-100.7%. The contents of fourteen components in each tablet sample were 0.05-0.25 mg, 0.00-4.30 mg, 0.28-1.03 mg, 1.39-34.45 mg, 2.85-5.71 mg, 0.32-0.97 mg, 0.89-1.43 mg, 0.06-0.33 mg, 0.05-0.26 mg, 0.43-0.95 mg, 0.09-0.38 mg, 0.04-0.12 mg, 0.03-0.14 mg, and 0.22-0.54 mg, respectively. Conclusion: Proved by method validation, this method could be used to determine chlorogenic acid, naringin, hesperidin, neohesperidin, baicalin, wogonoside, baicalein, aloeemodin, rhein, wogonin, emodin, costunolide, dehydrocostus lactone and chrysophanol in Lidanpaishi tablets.

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