HPLC法测定长春西汀氯化钠注射液中长春西汀的含量与有关物质

目的建立HPLC法测定长春西汀氯化钠注射液中长春西汀的含量与有关物质。方法色谱柱为Kromasil C18柱(250 mm×4.6 mm,5μm),流动相为体积分数为0.5%的二乙胺溶液-乙腈-异丙醇(体积比为36∶55∶9),检测波长为280 nm。采用外标法和不加校正因子的主成分自身对照相结合的方法对注射液中的有关物质进行检查,其中杂质A、B、C、D采用外标法,其他未知杂质采用不加校正因子的主成分自身对照法。结果在选定的色谱条件下,长春西汀主峰与有关物质峰基线分离,长春西汀在0.02⁰.18 g·L-1内质量浓度与峰面积线性关系良好,高、中、低浓度的回收率分别为99.2%、98.9%和100.3%,相对标准偏差RSD分别为0.54%、0.59%和1.38%(n=3);有关物质的检测结果均在限度范围之内。结论本法可用于长春西汀氯化钠注射液中长春西汀的含量与有关物质的检测。

Determination of vinpocetine content and related substances in vinpocetine sodium chloride injection by HPLC

Objective To establish an HPLC method for determing the content of vinpocetine and screening its related substances in vinpocetine sodium chloride injection.Methods The chromatographic conditions adopted were：Kromasil C₁₈ column（250 mm×4.6 mm,5 μm）,a mobile phase of 0.4%(w) diethylamine solution-acetonitrile-isopropanol(V:V:V=36:55:9),and a detection wavelength of 280 nm.The related substances in injection were determined by external standard method and main component self-compare without calibration factor method. Impurities A, B, C and D were checked by external standard method, other unknown impurities were checked by the method of main component self-compare without calibration factor. Results The related substances could be completely seprarated from vinpocetine. For vinpocetine,the linearity of the determination was over the range of 0.02-0.18 g·L^-1 the high, medium and low recoveries were 99.2%, 98.9% and 100.3%, the relative standard deviations were 0.54%, 0.59% and 1.38% (n=3). The test results of the related substances were within the limits. Conclusion A simple,accurate and specific method is established for determination of the content of vinpocetine and its related substances.