论文部分内容阅读
目的建立硫酸特布他林特殊杂质3,5-二羟基-ω-叔丁基苯乙酮定量分析的高效液相色谱法。方法采用Kromasil C_(18)色谱柱(4.6 mm×150 mm,5μm),以缓冲液[己烷磺酸钠4.23 g溶于0.05 mol·L~(-1)甲酸钠溶液(用甲酸调节pH值至3.0)770mL]-甲醇(77∶23)为流动相,流速1.0 mL·min~(-1),检测波长为276 nm,柱温30℃,进样量20μL。采用加校正因子的面积归一化法对特殊杂质3,5-二羟基-ω-叔丁基苯乙酮进行定量分析。结果特殊杂质3,5-二羟基-ω-叔丁基苯乙酮与特布他林及其降解产物的分离度良好;该杂质质量浓度在0.10~579μg·mL~(-1)(r=1.000 0)内呈良好的线性关系;该杂质相对于硫酸特布他林的校正因子为3.6。结论本实验采用加校正因子的面积归一化法对已知杂质进行定量,既可以解决杂质对照品持续供应困难的问题,又可准确计算出杂质的真实含量,为质量控制提供了高效便捷的检测方法。
OBJECTIVE To establish a HPLC method for the quantitative analysis of terbutaline sulfate special impurity 3,5-dihydroxy-ω-tert-butylacetophenone. Methods Kromasil C 18 column (4.6 mm × 150 mm, 5 μm) was used in the buffer [sodium hexanesulfonate 4.23 g in 0.05 mol·L -1 sodium formate solution 3.0) 770mL] -methanol (77:23) as mobile phase at a flow rate of 1.0 mL · min -1 with a detection wavelength of 276 nm and a column temperature of 30 ℃. Quantitative analysis of 3,5-dihydroxy-ω-tert-butylacetophenone, a specific impurity, was carried out by area normalization with a correction factor. Results The separation of 3,5-dihydroxy-ω-tert-butylacetophenone from terbutaline and its degradation product was good. The impurity concentration ranged from 0.10 to 579 μg · mL -1 (r = 1.000 0). The calibration curve of this impurity relative to terbutaline sulfate was 3.6. Conclusion In this experiment, the area normalization method with the correction factor was used to quantify the known impurities, which can not only solve the problem of continuous supply of impurity reference substance, but also accurately calculate the true content of impurities, providing an efficient and convenient method for quality control Detection method.