吡拉西坦原料药及注射液中3种有关物质定性及定量分析

目的： 建立吡拉西坦原料药及注射液中3种有关物质的定性及定量分析方法。 方法： 采用高效液相色谱法，色谱柱：CAPCELL PAK C₁₈（4.6 mm×250mm，5μm）；流动相：0.03%三乙胺溶液-乙腈（95：5）用稀磷酸调节pH至6.5；检测波长：205 nm；流速：1.0 mL·min^-1。测定3种有关物质的校正因子，分别采用标准曲线法、不加校正因子的主成分自身对照法以及加校正因子的主成分自身对照法对有关物质进行定量分析。 结果： 分别测得了3种有关物质对照品的标准曲线及校正因子，杂质A、B、C浓度分别在0.05090~20.36μg·mL^-1（r=1.000）、0.05195~20.78 μg·mL^-1（r=1.000）、0.06180~24.72 μg·mL^-1（r=1.000）范围内呈良好的线性关系，平均回收率为100.0%（RSD=1.5%，n=9）、100.3%（RSD=1.3%，n=9）、100.6%（RSD=1.9%，n=9）。杂质2-吡咯烷酮（A）、2-氧代-吡咯烷乙酸甲酯（B）及（2-氧代-吡咯烷-1-基）乙酸（C）校正因子分别为0.8、1.3、1.4。经过比较，加校正因子的主成分自身对照法计算有关物质的含量更准确、简便。[结论： 本方法可用于吡拉西坦原料药及注射剂中有关物质的定性及定量分析，采用加校正因子的主成分自身对照法可以更准确地反映其有关物质的含量。

Objective: To establish a qualitative and quantitative analysis method for the determination of three related substances in piracetam raw materials and its injection. Methods: The high performance liquid chromatography(HPLC)was used for the analysis;CAPCELL PAK C₁₈ column(4.6 mm×250mm, 5μm) was used as the analytical column;0.03% triethyl amine-acetonitrile(95:5) (adjusted to pH 6.5 with dilute phosphoric acid)was used as the mobile phase at a flow rate of 1.0 mL·min^-1;and the detection wavelength was 205 nm.To determine the correction factors of three related substances,the standard curve method,and the main component self-control method with and without correction factor were used for the quantitative analysis of the related substances respectively. Results: The regression equation and correction factors of three related substances were measured respectively.And the results showed that the method had good linearity for impurities A,B and C in the range of 0.05090-20.36μg·mL^-1(r=1.000),0.05195-20.78 μg·mL^-1(r=1.000) and 0.06180-24.72 μg·mL^-1(r=1.000).The average recoveries of impurities A,B and C were 100.0%(RSD=1.5%,n=9),100.3%(RSD=1.3%,n=9) and 100.6%(RSD=1.9%,n=9),respectively.The correction factors of impurities(2-oxopyrrolidine-1-yl) acetic acid,2-pyrrolidone,and methyl 2-oxo-pyrrolidine acetate were 0.8,1.3 and 1.4,respectively.By comparison,the main component self-control method with correction factors was more accurate and simpler to calculate the contents of related substances.Conclusion: The method can be used for the qualitative and quantitative analysis of the related substances in piracetam injection and raw materials,and the main component self-control method with correction factors can reflect the contents of related substances more accurately.

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