艾附暖宫胶囊中吴茱萸次碱含量测定的研究

Study of Determination of Rutecarpine in Aifunuangong Capsule

关键词:  艾附暖宫胶囊  含量测定  高效液相色谱法  吴茱萸次碱

Key words:  aifunuangong capsule  method of measuring the content  HPLC  rutecarpine

摘要:

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，5 μm)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8.52~85.2 μg·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。

Abstract:

OBJECTIVE Setting the method of measuring the content of Rutecarpine by using highly-effective liquid chromatography. METHODS Choosing proper stationary phase and adjusting the components, proportion, flow rate of mobile phase and column temperature in the condition of wavelength (nm) max to make theoretical plate number meet the standard. Preparing reference substance solution of different concentration, performing linear regression with chromatographic peak area as y-axis and sampling concentration as x-axis to get curvilinear regression and investigating linearity range. Investigating precision, ruggedness, stability and sample recovery rate of the method. Determining the content of components in three batches of samples according to the methods mentioned above. RESULTS The concentration of rutaecarpin was determined using a HPLC system at the wavelength of 345 nm. The separation was achieved by using a Thermo column (200 mm×4.6 mm, 5 μm), at a rate of 0.8 mL·min^-1. The temperature of column was 25 ℃. The mobile phase consisted of 0.04% octane sodium alkane sulphonate and acetonitrile at a ratio of 45∶55, with a good linear relationship among 8.52-85.2 μg·mL^-1, r is 0.999 8. The RSD% of precision, precision in middle, durable property, reproducibility, the stability within 12 hours and analytical recovery were 0.37%, 0.87%, 1.02%, 1.34%, 1.24%, 0.41%, respectively. The analytical recovery was 99.6%. It was no less than 0.067mg in per granule of the content of Rutecarpine. CONCLUSION Regarding the accepted active ingredients as a target of determining the content, using highly-effective liquid chromatography to measure rutecarpine, has good accuracy, exdusivity repe atability and the method is able to ensure the quality.