UPLC法测定头孢替坦二钠的有关物质

Determination of related substances of cefotetan disodium by UPLC

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 related substances of cefotetan disodium by UPLC. Methods UPLC was performed on Waters UPLC@BEH phenyl column（ 100 mm × 2. 1 mm,1. 7 μm） at 40 ℃,with the mobile phase of acetic acid buffer solution（ pH 1. 23）-methnol-acetonitrile（ V ∶ V ∶ V = 84 ∶ 8 ∶ 8）,at a flowrate of0. 3 m L·min^-1. And the ultraviolet detection wavelength was 254 nm. Results Forced degradation experiment showed that this chromatographic condition could completely separate the main peak from impurity peaks with good system precision（ RSD = 0. 45%）,good repeatability and good intermediate precision. The solution of cefotetan disodium could be stable for 3 hours under the condition of 5 ℃. The RSD of major impurity was 2. 5% and total impurities RSD was 1. 9%. The detection limit concentration was 81. 4 g·L^-1 and limit of quantification concentration was 126 g·L^-1. Good durability was obtained with the slight variations of the flowrate,batch of column,column temperature,organic phase ratio,pH value of mobile phase. Conclusions The proposed method is suitable for the determination of relative substances of cefotetan disodium.