HPLC法检查丙胺卡因原料药有关物质方法研究

Study on HPLC method for the determination of related substances in procaine injectons

目的建立HPLC对丙胺卡因原料药有关物质的测定方法。方法以Waters Xbridge BEH十八烷基硅烷键合硅胶为填充剂(C18,150 mm×4.6 mm×5μm的色谱柱);以磷酸盐缓冲液-乙腈(70∶30)为流动相进行等度洗脱,流速为1.0 mL/min;柱温为25℃;检测波长为240 nm;进样体积20μL。结果溶剂空白对系统适用性各组分测定无干扰,系统适用性中各组分及样品的分离度均达到标准,杂质A、杂质B、杂质C、杂质D、杂质E、杂质F、杂质G的浓度分别在0.10~500.32μg/mL、0.01~51.35μg/mL、0.20~500.51μg/mL、1.00~500.71μg/mL、0.10~499.05μg/mL、0.20~510.45μg/mL、0.10~498.75μg/mL内与其峰面积呈较好的线性关系,其r均在0.9995及以上;平均回收率分别为91.2%、95.9%、96.7%、98.1%、96.5%、97.1%、98.7%,RSD分别为0.68、0.54、0.75、0.36、0.72、0.36、0.61。结论HPLC法检查丙胺卡因原料药有关物质方法具有专属性强、灵敏度高、准确度高、精密度好,可满足丙胺卡因原料药有关物质检测需求。

Objective To establish an HPLC method for the determination of related substances in prilocaine bulk drug.Methods Waters Xbridge BEH octadecylsilane bonded silica gel was used as filler(C18,150 mm×4.6 mm×5 um column).Phosphate buffer-acetonitrile(70:30)was used as mobile phase for isometric elution at a flow rate of 1.0 mL/min.Column temperature is 25℃.The detection wavelength was 240 nm.The injection volume is 20μL.Results The solvent blank did not interfere with the determination of components in system applicability,and the separation degree of components and samples in system applicability met the standard.The concentrations of impurity A,B,C,D,E,F,and G were 0.10-500.32μg/mL,0.01-51.35μg/mL,0.20-500.51μg/mL,1.00-500.71μg/mL,and 0.10-499.05,respectively In the range of 0.20-510.45μg/mL and 0.10-498.75μg/mL,there is a good linear relationship with its peak area,and its r is 0.9995 or above.The average recoveries were 91.2%,95.9%,96.7%,98.1%,96.5%,97.1%,98.7%,and RSDS were 0.68,0.54,0.75,0.36,0.72,0.36,0.61,respectively.Conclusion HPLC method for the detection of the related substances of propionacaine has strong specificity,high sensitivity,high accuracy and good precision,and can meet the requirements for the detection of related substances of propionacaine.