高效液相色谱法测定左乙拉西坦中N-甲基苄胺含量  

Determination of N-methylbenzylamine in Levetiracetam by High Performance Liquid Chromatography

作　　者：李吉庆 刁玲玲 王帅 杨丽玲[3] Li Jiqing;Diao Lingling;Wang Shuai;Yang Liling(School of Environmental Science and Engineering,Qingdao University,Qingdao 266071,China;Chengyang Branch of Qingdao Ecological Environment Bureau,Qingdao 266109,China;Department of Ultrasound,The Eighth People's Hospital of Qingdao,Qingdao 266041,China)

机构地区：[1]青岛大学环境科学与工程学院,山东青岛266071 [2]青岛市生态环境局城阳分局,山东青岛266109 [3]青岛市第八人民医院超声科,山东青岛266041

出　　处：《山东化工》2021年第17期139-141,共3页Shandong Chemical Industry

摘　　要：建立了分析左乙拉西坦中N-甲基苄胺含量的高效液相色谱法。优化后液相色谱条件以安捷伦ZORBAX ODS C 18色谱柱(3.0×150 mm,5.0)为分析柱,甲醇与水为淋洗液,梯度洗脱,紫外检测器在244 nm波长下检测N-甲基苄胺。结果表明:本方法基质干扰低;专属性良好;在0.05~3μg/mL范围内线性关系良好(r=0.9991);检出限为0.05μg/mL,定量限为0.08μg/mL。优化前处理条件,考察二氯甲烷和乙酸乙酯作为水相提取剂的回收率,二氯甲烷作为萃取剂0.2,0.5,1μg/mL三个浓度的回收率从80.83%~84.83%,优于乙酸乙酯。该方法经济适用,重复性好,灵敏准确,适用于左乙拉西坦原料药中N-甲基苄胺的含量分析。A high performance liquid chromatography method was developed for the analysis of N-methylbenzylamine in levetiracetam.The optimized LC conditions were analyzed using an Agilent ZORBAX ODS C 18 column(3.0×150 mm,5.0)as the analytical column,methanol and water as the eluent,and gradient elution.The UV detector was used to detect N-methylbenzylamine at a wavelength of 244 nm.The results showed that:this method has low matrix interference;good specificity;good at 0.05;good linear relationship in the range of 3 mL to 3 mL(r=0.9991);detection limit is 0.05μg/mL and limit of quantification is 0.08μg/mL.The pretreatment conditions were optimized,and the recoveries of dichloromethane and ethyl acetate as aqueous extractants were investigated.The recoveries of dichloromethane as extractants of 0.2,0.5,and 1μg/mL were 80.83%~84.83%,which was better than acetic acid.Ethyl ester.This method is economical and applicable,has good reproducibility,sensitivity and accuracy,and is suitable for the analysis of N-methylbenzylamine in levetiracetam raw materials.

关 键 词：左乙拉西坦 N-甲基苄胺 高效液相色谱法 

分 类 号：O657.7[理学—分析化学]