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目的建立半夏泻心汤胃内滞留片质量控制方法。方法采用薄层色谱法对方中黄芩、黄连定性鉴别,高效液相色谱法定量分析黄芩苷、盐酸小檗碱的含量及体外药物释放。Diamonsil C_(18)色谱柱,黄芩苷以甲醇-水-磷酸(47∶53∶0.2)等度洗脱,280 nm波长处检测;盐酸小檗碱以乙腈-0.05 mol/L磷酸二氢钾(50∶50)等度洗脱,345 nm波长处检测。结果半夏泻心汤胃内滞留片中黄芩、黄连中的黄芩苷、盐酸小檗碱在薄层色谱中有良好的分离度。黄芩苷和盐酸小檗碱的线性回归方程分别为Y=40 763X-54 322(R~2=0.999 1)和Y=624 71X-163 59(R~2=0.999 7),分别在4~20 mg/L和5~25 mg/L范围内线性关系良好,方法学考察均符合要求。测定6批半夏泻心汤胃内滞留片中黄芩苷和盐酸小檗碱的含量分别为(19.95±0.72)mg/片和(13.02±1.05)mg/片。体外10 h释药达90%以上,确定体外释药时间点为2、6、10 h。结论本研究所建立的定性、定量分析方法灵敏可靠、简便、精密度高、重现性好,体外释放取样点的确定符合《药典》要求,可用于半夏泻心汤胃内滞留片的质量控制。
Objective To establish a quality control method of Banxiaxiexin decoction in the stomach. Methods The contents of baicalin and berberine hydrochloride and the drug release in vitro were quantitatively analyzed by TLC, qualitative identification of Radix Scutellariae and Coptis chinensis Franch and high performance liquid chromatography. Diamonsil C_ (18) column, baicalin was eluted with isocratic elution of methanol-water-phosphoric acid (47:53:0.2) and detected at 280 nm. Berberine hydrochloride was eluted with acetonitrile-0.05 mol / L potassium dihydrogen phosphate 50:50) isocratic elution, 345 nm wavelength detection. Results Banxiaxiexin soup stomach retention tablets Scutellaria, Coptis in the baicalin, berberine in thin layer chromatography with good resolution. The linear regression equations of baicalin and berberine were Y = 40 763X-54 322 (R ~ 2 = 0.999 1) and Y = 624 71X-163 59 (R ~ 2 = 0.999 7) The linear relationship between mg / L and 5 ~ 25 mg / L was good, and the methodological investigation met the requirements. The contents of baicalin and berberine in 6 batches of Banxiaxiexin decoction were (19.95 ± 0.72) mg / tablet and (13.02 ± 1.05) mg / tablet, respectively. In vitro 10 h release of more than 90%, in vitro release time points to determine 2, 6, 10 h. Conclusion The qualitative and quantitative analysis methods established in this study are sensitive, simple, accurate and reproducible. The determination of in vitro release sampling points is in accordance with the requirements of the Pharmacopoeia and can be used for the quality of the pelvic tablets of Banxiaxiexin Decoction control.