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目的:建立测定复方醋酸棉酚片中(-)-棉酚及(+)-棉酚含量的高效液相色谱方法。方法:以N,N-二甲基甲酰胺为溶剂,(R)-(-)-2-胺基-1-丙醇为衍生化试剂,90℃下水浴加热30 min进行衍生化反应。含量测定使用Agilent XDBC18色谱柱(250 mm×4.6 mm,5μm),流动相为10 mmol·L-1磷酸二氢钾缓冲液(pH=3.0)-乙腈(20∶80),流速1.0 mL·min-1,检测波长247 nm,柱温40℃。结果:(-)-棉酚和(+)-棉酚浓度分别在1.88~37.6μg·mL-1和1.98~30.7μg·mL-1范围内呈良好线性关系;(-)-棉酚及(+)-棉酚的平均回收率分别为101.0%和101.2%,RSD分别为2.3%和2.0%。结论:该方法可以准确测定复方醋酸棉酚片中(-)-棉酚及(+)-棉酚含量,有效提高其现有标准的质量控制水平。
Objective: To establish a HPLC method for the determination of (-) - gossypol and (+) - gossypol in compound gossypol acetate tablets. Methods: Derivatization was carried out using N, N-dimethylformamide as solvent and (R) - (-) - 2-amino-1-propanol as derivatization reagent in water bath at 90 ℃ for 30 min. The content was determined by using an Agilent XDBC18 column (250 mm × 4.6 mm, 5 μm) with a mobile phase of 10 mmol·L -1 potassium dihydrogen phosphate buffer (pH = 3.0) -acetonitrile (20:80) at a flow rate of 1.0 mL · min -1, detection wavelength 247 nm, column temperature 40 ℃. Results: The concentrations of (-) - gossypol and (+) - gossypol were linear in the range of 1.88-37.6μg · mL-1 and 1.98-30.7μg · mL-1, respectively. +) - gossypol were 101.0% and 101.2%, respectively, with RSDs of 2.3% and 2.0%, respectively. Conclusion: This method can accurately determine the contents of (-) - gossypol and (+) - gossypol in compound gossypol acetate tablets and effectively improve the quality control level of its existing standard.