柱前衍生化高效液相色谱法测定门冬氨酸洛美沙星中门冬氨酸  

Determination of aspartic acid in lomefloxacin aspartate by pre-column derivatization high performance liquid chromatography

作　　者：陈希 鄢雷娜 刘绪平 段和祥 CHEN Xi;YAN Lei-na;LIU Xu-ping;DUAN He-xiang(Jiangxi Institute For Drug Control,Jiangxi Provincial Engineering Research Center for Drug and Medical Device Quality,Nanchang 33002)

机构地区：[1]江西省药品检验检测研究院江西省药品与医疗器械质量工程技术研究中心,南昌330029

出　　处：《分析试验室》2018年第8期937-941,共5页Chinese Journal of Analysis Laboratory

摘　　要：建立了柱前衍生化高效液相色谱法测定门冬氨酸对映体。利用邻苯二甲醛、N-乙酰-L-半胱氨酸对门冬氨酸进行柱前衍生化,采用CAPCELL MGⅡC18色谱柱,流动相为磷酸盐溶液(pH 8.2)-甲醇,梯度洗脱,流速为1 m L/min,柱温为室温,检测波长为231 nm。门冬氨酸对映体分离度为1.7,L-门冬氨酸质量浓度在3.5~70.8μg/m L范围内线性关系良好(r2=0.9993),回收率在97%~101%之间。门冬氨酸洛美沙星中门冬氨酸均为L型。建立的手性分离测定门冬氨酸的方法可行,可用于门冬氨酸洛美沙星中门冬氨酸的构型鉴别和含量测定。This work establish a pre-column derivatization high performance liquid chromatography（HPLC） method for determination aspartic acid enantiomers. Aspartic acid was derivatized by ophthalaldehyde and N-phenacetin-L-cysteine. HPLC determination was performed on CAPCELL MGⅡC18（4. 6 × 250 mm,5 μm） at a column temperature of 25 ℃. Linear gradient elution was used with mobile phase consisted of phosphate solution（pH 8. 2）-methanolat the flow rate of 1 m L/min,and the detection wavelength was 231 nm. The resolution of aspartic acid enantiomers was 1. 7. L-aspartic acid showed a good linear relationship at a range of 3. 5-70. 8 μg/m L（r2= 0. 9993）. The recoveries was between 97 % and 101 %. Aspartate in lomefloxacin aspartate is L-aspartic acid. The method of chiral separation for determination of aspartate in the present study is feasible and can be used in the determination of the configuration and the content of aspartic acid in lomefloxacin aspartate.

关 键 词：门冬氨酸洛美沙星 门冬氨酸 柱前衍生化 手性分离 

分 类 号：R917[医药卫生—药物分析学]