胶束扫集毛细管电动色谱法测定药物中3种邻苯二甲酸酯  

Quick determination of three phthalate acid esters in medicine by capillary electrophoresis using sweeping micellar electrokinetic chromatography

作　　者：李斯光[1] 余娴陈[1] 刘展良[1] 

机构地区：[1]广东科贸职业学院实训中心,广州510430

出　　处：《分析试验室》2012年第5期99-103,共5页Chinese Journal of Analysis Laboratory

摘　　要：采用胶束扫集毛细管电动色谱技术,建立了测定药物中邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DZP)和邻苯二甲酸二丁酯(DBP)的方法。电泳缓冲体系含80 mmol/L SDS,20 mmol/L NaH2PO4(pH 2.20),5%甲醇(V/V),分离电压-18 kV,重力进样80s×15.0cm,检测波长225 nm,使用Φ50μm×62.0 cm石英毛细管,有效长度50.0 cm。讨论了磷酸盐浓度、有机改善剂、SDS浓度、分离电压、进样时间等因素的影响,并考察了胶束扫集法对DMP、DEP和DBP的富集能力。在优化条件下,线性关系良好,相关系数大于0.9986,DMP、DEP和DBP的线性范围分别为1.25～240,1.04～200和1.56～200 mg/L,检出限分别为0.26,0.26和0.39 mg/L。方法应用于肠溶片中DMP、DEP和DBP的测定,回收率在93.3%～108%之间,RSD≤5.2%。每次样品测定可在10 min内完成。Sweeping micellar electrokinetic chromatography（sweep-MEKC） was used in the determination of dimethyl phthalate（DIP）,diethyl phthalate（DEP） and dibutyl phthalate（DBP） in medicinal tablets.The buffer contained 80 mmol/L SDS,20 mmol/L NaH2PO4（pH 2.20） and 5% CH3OH（V/V）,the separation voltage was-18kV,injection time was 80s by 15.0 cm,and the detection was at 225 nm.During condition optimization,different organic solvents were compared,concentration of sodium dodecyl sulfa（SDS） and injection time were discussed.During sensitivity enrichment validation,a signal obtained by pushing single standards through detector window was used as the reference,and enrichment times of three analytes were found as 3.7 for DMP,6.5 for DEP and 3.6 for DBP.Under the optimum conditions,every determination was finished within 10 minutes.The linearities were 1.25-240 mg/L for DMP,1.04-200 for DEP,and 1.56-200 mg/L for DBP,The LODs were 0.26 mg/L for DEP and DMP,and 0.39 for DBP,all of the correlation coefficients were better than 0.9986.This method was used in determination of real samples with recoveries between 93.3% and 108%,and RSDs≤5.2%.

关 键 词：毛细管电泳 胶束扫集 电动色谱 邻苯二甲酸酯 

分 类 号：O658.1[理学—分析化学]