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    高效液相色谱法测定造影剂碘普罗胺中的相关杂质

    Determination of Related Impurities in Contrast Agent Iopromide by High Performance Liquid Chromatography

    • 摘要: 提出采用高效液相色谱法测定一种非离子型碘造影剂碘普罗胺中5种杂质含量的方法。以Eclipse C18 Plus色谱柱为分离柱,以不同体积比混合的水和体积比为55:40:5的水-乙腈-2-丁醇混合溶液为流动相进行梯度洗脱,在检测波长245 nm处对5.0 g·L-1的样品溶液中的5种杂质进行测定。结果显示:杂质1~5标准曲线的线性范围分别为2.57~51.4 mg·L-1,5.05~101 mg·L-1,2.56~51.2 mg·L-1,1.01~20.2 mg·L-1,0.51~10.2 mg·L-1。检出限(3S/N)分别为0.10,0.20,0.15,0.12,0.10 mg·L-1。对实际样品进行3个浓度水平的加标回收试验,杂质1~5的回收率分别为105%,93.7%,95.2%,97.8%,112%,重复性和中间精密度试验结果显示,杂质1~5测定值的相对标准偏差(n=6)均在15%以内。

       

      Abstract: A method for the determination of five impurities in iopromide, a non-ionic contract agent, was proposed by high performance liquid chromatography. Eclipse C18 Plus chromatographic column was used as the separation column, and the mixed solution of water-acetonitrile-2-butanol with a volume ratio of 55:40:5 and water with various volume ratios was used as the mobile phase for gradient elution. Five impurities in 5.0 g·L-1 sample solution were determined at the detection wavelength of 245 nm. As found by results that linerity ranges of standard curves were kept in the ranges of 2.57-51.4 mg·L-1, 5.05-101 mg·L-1, 2.56-51.2 mg·L-1, 1.01-20.2 mg·L-1, 0.51-10.2 mg·L-1, respectively, with detection limits (3S/N) of 0.10, 0.20, 0.15, 0.12, 0.10 mg·L-1, respectively. Spiked recovery tests were made on the actual sample at three concentration levels, giving recoveries of impurities of 1-5 were 105%, 93.7%, 95.2%, 97.8%, 112%, respectively. Results of tests for repeatability and intermediate precision showed that RSDs (n=6) of measured values of impurities of 1-5 were all less than 15%.

       

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