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目的运用UPLC法测定头孢替坦二钠的有关物质。方法采用Waters UPLC@BEH phenyl色谱柱(100 mm×2.1 mm,1.7μm),流动相:醋酸溶液(pH=1.23)-甲醇-乙腈(体积比为84∶8∶8),流速:0.3 m L·min~(-1),检测波长:254 nm,柱温:40℃。结果破坏试验结果显示,本方法能够将主峰和杂质峰完全分离,专属性强;在5℃条件下存放,3 h内溶液稳定;系统精密度RSD为0.45%;重复性、中间精密度:最大杂质RSD为2.5%,总杂质RSD为1.9%;检测限质量浓度:81.4 g·L-1,定量限质量浓度:126 g·L~(-1);该方法在流速、色谱柱批次、柱温、有机相比例、流动相pH值微小变动的条件下,耐用性良好。结论该方法大大提高了头孢替坦二钠有关物质的检测效率。
Objective To determine the related substances of cefotetan disodium by UPLC method. Methods A Waters UPLC @ BEH phenyl column (100 mm × 2.1 mm, 1.7 μm) was used. The mobile phase consisted of acetic acid solution (pH = 1.23) -methanol-acetonitrile (84:8:8 by volume) · Min ~ (-1), detection wavelength: 254 nm, column temperature: 40 ℃. Results The results of sabotage test showed that this method can completely separate the main peak and the impurity peak, and is highly specific. When stored at 5 ℃, the solution is stable within 3 h. The system precision RSD is 0.45%. The repeatability and intermediate precision The impurity RSD was 2.5%, the total impurity RSD was 1.9%. The limit of detection mass concentration was 81.4 g · L-1, the limit of quantification concentration was 126 g · L -1. The column temperature, the ratio of the organic phase, the pH of the mobile phase under the conditions of small changes, durability is good. Conclusion This method greatly improves the detection efficiency of cefotetan disodium related substances.