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目的采用高效液相色谱法,建立吴茱萸次碱的含量测定方法。方法选择合适的固定相,调整流动相组成、配比、流速以及柱温,在最大吸收波长下测定,使指标峰分离完全,理论塔板数符合要求。配制系列浓度的对照品溶液,以色谱峰的峰面积为纵坐标,以进样浓度为横坐标,进行线性回归,得回归曲线并考察线性范围。分别考察测定方法的精密度、重现性、稳定性和加样回收率。取3批样品分别测定指标成分的含量。结果吴茱萸次碱色谱条件为:Thermo(200 mm×4.6 mm,5μm)色谱柱,流动相:0.04%辛烷磺酸钠-乙腈(45∶55),流速0.8 mL.min 1,柱温25℃,检测波长345 nm。吴茱萸次碱在8.52~85.2μg.mL 1范围内线性关系良好,r为0.999 8。该方法精密度、中间精密度、耐用性、重复性、在12 h内稳定性和加样回收率的RSD分别为0.37%、0.87%、1.02%、1.34%、1.24%、0.41%,加样回收率为99.6%,样品中吴茱萸次碱含量不低于0.067 mg.粒1。结论以公认的有效成分作为含量测定指标,采用高效液相色谱法进行检测,准确度高,专属性强,重复性好,能有效控制制剂质量。
Objective To establish a method for the determination of rutaecarpine by high performance liquid chromatography. Methods The appropriate stationary phase was selected to adjust the composition of the mobile phase, the ratio, the flow rate and the column temperature. The peak was determined at the maximum absorption wavelength, and the index peak was completely separated. The number of theoretical plates met the requirements. Preparation of a series of concentrations of the reference solution to peak peak area of the vertical axis to the sample concentration as the abscissa for linear regression regression curve obtained and to investigate the linear range. Investigate the determination of the precision, reproducibility, stability and sample recovery rate. Three batches of samples were taken to determine the content of the index components. Results The chromatographic conditions of rutaecarpine were as follows: Thermo (200 mm × 4.6 mm, 5 μm) column, the mobile phase consisted of 0.04% sodium octane sulfonate and acetonitrile (45:55), the flow rate was 0.8 mL.min 1, , Detection wavelength 345 nm. Rutaecarpine showed a good linearity in the range of 8.52 ~ 85.2μg.mL 1 with r of 0.999 8. The RSD of the method was 0.37%, 0.87%, 1.02%, 1.34%, 1.24% and 0.41%, respectively, within 12 h. The precision, precision, durability and repeatability of the method were good The recovery was 99.6%. The content of rutaecarpine in the sample was not less than 0.067 mg. Conclusion The accepted active ingredients as the determination of the content of indicators, the use of high performance liquid chromatography for detection, high accuracy, specificity, reproducibility, and can effectively control the quality of the preparation.