论文部分内容阅读
目的建立测定替卡西林钠及注射用替卡西林钠克拉维酸钾中有关物质的高效液相色谱梯度洗脱法。方法采用HPLC梯度洗脱法,色谱柱为Waters XBridge~(TM) C_(18)柱(4.6 mm×250 mm,5μm);以0.01 mol·L~(-1)磷酸氢二铵溶液(p H 7.0)为流动相A,0.01 mol·L~(-1)磷酸氢二铵溶液(pH 7.0)-甲醇(50∶50)为流动相B,梯度洗脱;流速为1.0 m L·min~(-1);检测波长为220 nm;柱温为30℃。结果与等度洗脱法比较,梯度洗脱法具有更强的分析杂质的能力,样品中各成分的分离度及检出灵敏度均满足有关物质测定要求。替卡西林杂质A与破坏条件下产生的降解杂质与主成分峰分离较好;替卡西林的最低检出限为4.8 ng,克拉维酸的最低检出限为7.3 ng;原料药与制剂样品中替卡西林杂质A均<1.5%,最大单个杂质均<2.0%,总杂质均<4.0%。结论本方法专属性好,灵敏度高,可用于替卡西林钠原料药和注射用替卡西林钠克拉维酸钾中有关物质的测定。
OBJECTIVE To establish a high performance liquid chromatography gradient elution method for the determination of related substances in ticarcillin sodium and tacrolimin sodium clavulanate for injection. Methods HPLC gradient elution was performed on a Waters XBridge C18 column (4.6 mm × 250 mm, 5 μm). The column was eluted with 0.01 mol·L -1 diammonium phosphate solution (p H 7.0) was used as mobile phase A. The mobile phase A was eluted with 0.01 mol·L -1 diammonium phosphate (pH 7.0) -methanol (50:50) as mobile phase B at a flow rate of 1.0 mL · min -1 -1); detection wavelength was 220 nm; column temperature was 30 ℃. Results Compared with the isocratic elution method, the gradient elution method has a stronger ability to analyze impurities. The separation and detection sensitivity of the components in the sample all meet the requirements of related substances determination. Tacrolimus impurity A and destructive conditions generated degradation impurities and the main component peak separation is good; ticarcillin detection limit of 4.8 ng, the detection limit of clavulanic acid was 7.3 ng; raw materials and preparations of the sample The median tacrolimus impurity A was less than 1.5%, the largest single impurity was less than 2.0% and the total impurity was less than 4.0%. Conclusion This method is of good specificity and high sensitivity and can be used for the determination of related substances in ticarcillin sodium and clavulanic acid potassium in ticarcillin sodium for injection.