葡聚糖凝胶色谱法测定注射用头孢曲松钠他唑巴坦 - 中国药品标准杂志.doc

对《中国药典》注射用氨苄西林钠舒巴坦钠有关物质的建议 姚永青，刘英（河南省食品药品检验所，郑州450003） 《中国药典》注射用氨苄西林钠舒巴坦钠有关物质取氨苄西林系统适用性对照品适量，加流动相溶解并稀释制成每1 ml中约含2 mg的溶液，记录的色谱图应与标准图谱一致氨苄西林钠舒巴坦钠中图分类号：R921.2 文献标志码：A Suggestion about the Locating Method of Ampicillin Dimer -Related Substance of Ampicillin Sodium and Sulbactam Sodium for Injection in Chinese Pharmacopoeia Yao Yongqing，L Ying*（Henan Institute for Food and Drug Control，Zhengzhou 450003）Abstract Objective: To improve the locating method of Ampicillin dimer - related substance of Ampicillin Sodium and Sulbactam Sodium for Injection in Chinese Pharmacopoeia. Methods: Three different chromatographic columns were examined by pharmacopoeia method and Ampicillin system suitability standard diagram method，their results were inspected for consistency ot . Results: The results of two methods were not consistent. Conclusion: The current standard is inappropriate, the dimer locating method should be amended as: take the right amount of Ampicillin system suitability CRS, plus the initial mobile phase dissolved and diluted to make per 1 ml containing about 2 mg of solution, take 10 μl injected to liquid chromatograph, the recorded chromatograms should be consistent with the standard diagram. Key words: Ampicillin Sodium and Sulbactam Sodium；Ampicillin dimer 注射用氨苄西林钠舒巴坦钠由氨苄西林钠β-内酰胺酶抑制剂舒巴坦钠，《中国药典》2015年版β-内酰胺笔者在试验中定位氨苄西林二聚存在问题10 μl注入液相色谱仪，与氨苄西林峰相对保留时间约1.7倍处的较大杂质峰为氨苄西林二聚峰某样品在与氨苄西林峰相对保留时间约1.7倍处有杂质峰，[7-8]。 因此本试验尝试用氨苄西林系统适用性对照品来定位氨苄西林二聚体峰，先用氨苄西林色谱条件[9]确定二聚体峰的位置，然后用氨苄西林舒巴坦色谱条件分别进样氨苄西林系统适用性对照品溶液和供试品高温破坏溶液，考察该方法定位二聚体与现行标准方法是否一致。 1 仪器与试药 Waters2695/2487高效液相色谱仪及Empower色谱工作站（美国waters公司）；Sartorius BP211D电子天平；Orion Star pH计（Thermo公司） 氨苄西林系统适用性对照品（中国食品药品检定研究院，批号130618-201202）；注射用氨苄西林钠舒巴坦钠（厂家A，规格1.5 g，批；乙腈为色谱纯，磷酸二氢钾、磷酸二氢钠、醋酸、磷酸均为分析纯，水为纯净水。 2 方法与结果 2.1 色谱条件[9] 色谱柱Agela Venusil XBP C18(L)（4.6 mm×250 mm，5 μm）；流动相A为12%醋酸溶液-0.2 mol﹒L-1磷酸二氢钾溶液-乙腈-水（0.550∶50∶900），流动相B为12%醋酸溶液-0.2 mol﹒L-1磷酸二氢钾溶液-乙腈-水（0.550∶400∶550），先以流动相A流动相B（8515）等度洗脱，待氨苄西林峰洗脱完毕后立即按表进行线性