氨基己酸注射液中有关物质检查方法的研究  

Study on the detection of related substances in aminocaproici acid injection

作　　者：江文明[1] 宋冬梅[1] 任美婷[1] 杨永健[1] 

机构地区：[1]上海市食品药品检验所,上海201203

出　　处：《药物分析杂志》2016年第7期1258-1262,共5页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:对氨基己酸注射液中的有关物质进行研究。方法:采用Agilent Eclipse Plus C18色谱柱(100 mm×3.0 mm,1.8μm),流动相为0.02 mol·L^(-1)甲酸铵缓冲液(含0.1%的甲酸)(A)-乙腈(B),梯度洗脱,流速0.4 m L·min^(-1),柱温30℃;在电喷雾离子源正离子模式下,对杂质进行定性研究,确定主要杂质的结构。采用Kromasil 100-5 C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.55%己烷磺酸钠溶液(25∶75,含1%磷酸二氢钾,用磷酸调节pH至2.2),流速1.0 m L·min^(-1),柱温30℃,检测波长210 nm,对杂质进行定量测定。结果:建立了氨基己酸注射液中有关物质的检测方法,氨基己酸注射液中的主要杂质为己内酰胺与氨基己酸二聚体,含量分别为标示量的0.002%~0.02%和0.009%~0.05%。结论:本法可用于氨基己酸注射液中有关物质的检测。Objective：To study the related substances in aminocaproici acid injection.Method：An Agilent Eclipse Plus C18 column（100 mm×3.0 mm,1.8 μm）was adopted in the study with mobile phase consisting of 0.02 mol·L（-1） ammonium formate containing 0.1% formic acid（solvent A）and acetonitrile（solvent B）.The structures of major unknown impurities were identified by LC-MS-QTOF（electrospray ion source,positive ion mode）with gradient elution at a flow rate of 0.4 m L·min-（-1） and column temperature at 30 ℃.The quantitative determination of the impurities was realized on a Kromasil 100-5 C18 column（250 mm×4.6 mm,5 μm）（column temperatureat 30 ℃）with methanol-0.55% sodium hexanesulfonate（25∶75,containing potassium 1% dihydrogen phosphate,pH adjusted to 2.2 by phosphoric acid）as mobile phase at the flow rate of 1.0 m L·min-（-1）,and the detection wavelength was 210 nm.Results：Caprolactam and aminocaproic acid dimer were identified as the major impurities in aminocaproici acid injection.The method for related substances detection of caprolactam and aminocaproic acid dimer in aminocaproici acid injection was established,and the contents were ranged in 0.002% to 0.02% and 0.009% to 0.05% of labeled amount,respectively.Conclusion：The established method can be used for the determination of related substances in aminocaproici acid injection.

关 键 词：氨基己酸注射液 有关物质检测 己内酰胺 氨基己酸二聚体 杂质结构鉴定 杂质含量测定 高效液相色谱 液相色谱-质谱联用 

分 类 号：R917[医药卫生—药物分析学]