HPLC法测定门冬氨酸钾镁注射液中门冬氨酸有关物质及含量  

HPLC determination of aspartate in potassium aspartate and magnesium aspartate injection and its related substances

作　　者：肖菁 朱志玲 王蓉蓉 缪建荣 左利民[2] 刘桂霞[2] 山广志[2] XIAO Jing1 , ZHU Zhi-ling2, WANG Rong-rong1, MIAO Jian-rong 1, ZUO Li-ming2, LIU Gui-xia2, SHAN Guang-zhi2(1. Hunan Institute for Drug Control, Changsha, 410001, China; 2. Institute of Medicinal Biotechnology, Chinese Academy of Medical Sciences, Beijing 100050, China)

机构地区：[1]湖南省药品检验研究院,长沙410001 [2]中国医学科学院医药生物技术研究所,北京100050

出　　处：《药物分析杂志》2018年第3期477-484,共8页Chinese Journal of Pharmaceutical Analysis

基　　金："重大新药创制"国家科技重大专项(2012ZX09301002-001-019);2015年国家药品抽验计划

摘　　要：目的:建立门冬氨酸钾镁注射液中门冬氨酸有关物质含量测定的HPLC方法。方法:采用SPHERISORB NH_2柱(4.6 mm×250 mm,5μm);流动相为乙腈-0.05 mol·L^(-1)的磷酸二氢钾(60∶40);流速为1.0 mL·min^(-1);检测波长为210 nm;柱温为30℃,进样量为5μL;对最大单个杂质采用在线二维脱盐HPLC与MS联用进行初步推断。结果:在该选定色谱条件下,主峰与有关物质峰分离度良好;门冬氨酸在0.338 64~3.386 4 mg·mL^(-1)浓度范围内线性关系良好(r=0.999 8);平均回收率为99.6%(n=9),检测限为23.5 ng;初步推断最大单个杂质为富马酸。结论:本方法专属、灵敏、简便,可用于测定门冬氨酸钾镁注射液中门冬氨酸含量和有关物质。Objective： To establish an HPLC method for the determination of aspartate in potassium aspartate and magnesium aspartate injection and its related substances.Methods： The separation was performed on a Waters SPHERISORB NH2（4.6 mm×250 mm,5μm）column with the mobile phase consisting of acetonitrile-0.05 mol·L-1 phosphate solution（60：40） at the flow rate of 1.0 mL·min-1.The detection wavelength was set at 210 nm.The column temperature was 30℃.The volume of injection was 5 μL.On-line two-dimensional desalting HPLC/MS was applied to infer the maximum single impurity preliminarily.Results： Under above conditions,the main peak and the peaks of the related substances were well separated.Aspartate had a good linear relationship （r=0.999 8） within the range of 0.338 64-3.386 4 mg·mL-1.The average recovery （n=9） was 99.6%.The limit of the detection was 23.5 ng.The maximum single impurity in related substances was preliminarily inferred as fumaric acid.Conclusion： The method is sensitive,specific and simple.It can be used for determining aspartate in potassium aspartate and magnesium aspartate injection and its related substances.

关 键 词：门冬氨酸钾镁注射剂 有关物质 富马酸 含量测定 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]