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目的建立反相离子对色谱法测定替卡西林钠中的有关物质的含量。方法色谱柱为Chromegabond TMS C_1(150 mm×4.6 mm,5μm)柱;流动相A为乙腈-磷酸盐缓冲液(含浓度5mmol·L~(-1)四丁基溴化铵的20mmol·L~(-1)的磷酸二氢钠溶液,用磷酸调节pH值至3.0,体积比1∶4),流动相B为乙腈-磷酸盐缓冲液(含5mmol·L~(-1)四丁基溴化铵的20mmol·L~(-1)的磷酸二氢钠溶液,用磷酸调节pH值至3.0,体积比1∶1),梯度洗脱;流速为1.5 mL·min~(-1);检测波长为230nm;柱温为30℃。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;精密度RSD为0.36%;替卡西林杂质A重复性、中间精密度RSD为0.19%、0.33%,替卡西林杂质D重复性、中间精密度RSD为0.94%、1.14%,最大杂质重复性、中间精密度RSD为1.03%、0.95%,总杂质的重复性、中间精密度RSD为0.86%、1.27%;在4℃条件下存放,12h内溶液稳定;替卡西林的质量浓度在10.116~101.16mg·L~(-1)内与峰面积呈良好的线性关系(r>0.999 9,n=5);检测限质量浓度为0.105mg·L~(-1),定量限质量浓度为0.260mg·L~(-1)。结论该方法可用于替卡西林钠的质量控制。
Objective To establish an RP-HPLC method for the determination of related substances in ticarcillin sodium. Methods The mobile phase A was acetonitrile-phosphate buffer (containing 20 mmol·L -1 tetrabutylammonium bromide with concentration of 5 mmol·L -1) on the column of TMS C_1 (150 mm × 4.6 mm, 5 μm) (-1) sodium dihydrogen phosphate solution, adjusting the pH value to 3.0 with phosphoric acid, the volume ratio is 1: 4), mobile phase B is acetonitrile-phosphate buffer solution containing 5 mmol·L -1 tetrabutyl bromide Ammonium dihydrogen phosphate solution (20 mmol·L -1) was adjusted to pH 3.0 with phosphoric acid and the volume ratio was 1: 1. The gradient elution was carried out. The flow rate was 1.5 mL · min -1. The wavelength is 230nm; the column temperature is 30 ℃. Results The results of destructive test showed that this method can separate the main peak and impurity peak completely; the RSD of precision is 0.36%; the repeatability of ticarcillin impurity A, the RSD of intermediate precision is 0.19% and 0.33%, the repeatability of ticarcillin impurity D , The RSD of the intermediate precision was 0.94%, 1.14%, the maximum impurity repeatability, the intermediate precision RSD was 1.03%, 0.95%, the total impurity repeatability, the intermediate precision RSD was 0.86%, 1.27%; at 4 ℃ The concentration of ticarcillin showed a good linear relationship (r> 0.999 9, n = 5) with the peak area within the range of 10.116 ~ 101.16 mg · L ~ (-1). The limit of detection mass concentration 0.105 mg · L -1, the limit of quantification was 0.260 mg · L -1. Conclusion This method can be used for ticarcillin quality control.