盐酸尼非卡兰的有关物质及含量测定方法

 目的分别用HPLC和非水酸碱滴定法建立起盐酸尼非卡兰有关物质检查及含量测定的方法,为原料的质量控制提供有效的分析方法。方法采用岛津CLC-ODS(6mm×150mm,5μm)柱,流动相:乙腈-0.02mol·L^-1的磷酸二氢钾溶液(NaOH溶液调pH至5.0)=25∶75;检测波长:268nm;流速:1.0mL·min^-1;柱温:30℃。结果在选定的色谱条件下,盐酸尼非卡兰与7个有关物质分离完全;盐酸尼非卡兰在5～100mg·L^-1内,峰面积与浓度线性关系良好,r=0.9999;检测限为0.2ng。结论方法简便,准确,专属性强,可用于盐酸尼非卡兰的有关物质检查及含量测定。

Determination of Nifekalant Hydrochloride and Its Related Substances by HPLC and Nonaqueous Acid-Base Titration

OBJECTIVE To develop HPLC and nonaqueous acid-base titration for the determination of nifekalant hydrochloride and its related substances for quality control.METHODS Chromatography was carried out on a Shimadzu CLC-ODS column (6 mm×150 mm,5 μm), using the mobile phase of acetonitrile-0.02 mol·L^-1 phosphate buffer(pH 5.0 adjusted by sodium hydroxide solution 25∶75) at a flow rate of 1.0 mL·min^-1. The ultraviolet detection wavelength was set at 268 nm,the column temperature was 30 ℃. RESULTS Under the established chromatographic conditions,nifekalant hydrochloride and the related substances were separated completely.The method was validated, and stability tests under various conditions were performed.The standard curve was linear within the range of 5～100 mg·L^-1 with the correlation coefficient of 0.999 9, the limit of detection was 0.2 ng. CONCLUSION The established methods were simple, accurate,specific and could be used for quality control of nifekalant hydrochloride.