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有关物质  

Determination of related substances in ampicillin sodium and sulbactam sodium for injection by RP-HPLC gradient elution method

作　　者：周明昊[1] 胡楚楚[1] 

机构地区：[1]浙江省食品药品检验所,杭州310004

出　　处：《中国抗生素杂志》2009年第3期158-162,共5页Chinese Journal of Antibiotics

摘　　要：目的建立用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有关物质。方法色谱柱为十八烷基硅烷键合硅胶柱(UltimateTM AQ-C18,4.6mm×250mm,5μm),检测波长为254nm,采用A相[12%乙酸溶液:0.2mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:50:900)]—B相[(12%乙酸溶液:0.2mol/L磷酸二氢钾溶液:乙腈:水(0.5:50:400:550)]为流动相进行梯度洗脱(A相起始比例为90%,保持15min,25min内下降至0,保持该比例10min),流速为1.0ml/min,柱温为25℃,进样量为20μl。结果舒巴坦的碱性降解产物(舒巴坦青霉胺)、舒巴坦、氨苄西林的碱性降解产物、氨苄西林、头孢拉定和氨苄西林二聚物等相关物质在本色谱条件下均能实现较好分离,杂质相对检出率较高。结论本法基线稳定,重现性好,准确度高,可同时测定氨苄西林钠舒巴坦钠的有关物质。Objective To develop a RP-HPLC gradient elution method for determination of related substances in ampicillin sodium and sulbactam sodium for injection. Method UltimateTM AQ-C18 column（4. 6mm × 250mm,μm）with temperature at 25℃ was used, the mobile phase was A[12% acetic acid solution-0. 2mol/L potassium dihydrogen phosphate-acetonitrile-water（0. 5： 50： 50： 900）]--B[ 12% acetic acid solution-0. 2mol/L potassium dihydrogen phosphate-acetonitrile-water（0. 5： 50： 400： 550）] （initial ratio of A was 90% for 15min, then decreased to 0 in 25min and maintain this ratio for 10min）, the detecting wavelength was 254nm, the flow rate was 1.0mol/L and the sample volume was 20μ1. Results The re.lated substances in ampicillin sodium and sulbactam sodium, such as sulbactam alkaline degradation product, ampicillin alkaline degradation product, cefradine and dimmer ampicillin were separated successfully. The reproducibility and accuracy, sodium for iniection. relative detection rate for impurity is good. is suitable for the determination of related Conclusion This method with good baseline, substances in ampicillin sodium and sulbactam sodium for injection.

关 键 词：反相高效液相色谱 氨苄西林 舒巴坦 梯度洗脱 

分 类 号：R978.11[医药卫生—药品]