HPLC法测定注射用氨苄西林钠舒巴坦钠中聚合物

Determination of high molecular mass impurities in ampicillin sodium and sulbact sodium for injection by HPLC

目的建立反相高效液相色谱梯度洗脱法,测定注射用氨苄西林钠舒巴坦钠中的二聚物。方法采用Diamonsil C18(250 mm×4.6 mm,5μm)。流动相:A相[12%醋酸溶液:0.2 mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:50:900)];B相[12%醋酸溶液:0.2 mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:400:550)]。梯度洗脱(A相起始比例为85%,保持8.5 min,30 min内下降至0,保持该比例15 min),流速为1.0 mL/min,检测波长为254 nm。结果氨苄西林在0.675～5.4 mg/mL范围内与氨苄西林二聚物峰面积呈良好的线性关系(r=1.0000)。结论该方法能较好地分离舒巴坦、氨苄西林、氨苄西林二聚物及其他杂质,方法简便,结果可靠,可用于注射用氨苄西林钠舒巴坦钠中氨苄西林二聚物的检测。

Objective To develop a RP-HPLC gradient elution method for determination of dimmer ampicillin in ampicillin sodium and sulbactam sodium for injection.Methods The analytical column was C18 column（250 mm ×4.6 mm,5 μm）,the mobile phase was A[12% acetic acid-0.2 mol/L potassium dihydrogen phosphate-acetonitrile-water（0.5：50：50：900） ]and B[12% acetic acid -0.2 mol/L potassium dihydrogen phosphate-acetonitrile-water（0.5∶50：400：550）]（initial ratio of A was 85% for 8.5 min,then decreasing to 0 in 30 min and maintaining this ratio for 15min）,the flow rate was 1.0 mL/min,and the detecting wavelength was 254 nm.Results The dimmer ampicillin＇ scalibration curve was linear in the range of 0.675～5.4 mg/mL for ampicillin with good correlation coefficient（r=1.000 0）.Conclusion The method achieves satisfactory separation among ampicillin,sulbactam,dimmer ampicillin and related substances.It is simple and quick with high sensitivity,and it is applicable for the determination of dimmer ampicillin in ampicillin sodium and sulbactam sodium for injection.