在线扫集-胶束毛细管电动色谱法测定金感胶囊中的绿原酸、脱水穿心莲内酯和马来酸氯苯那敏  

Determination of Chlorogenic Acid,Dehydroandrographolide and Chlorphenamine Maleate in Jingan Capsule by Sweeping-Micellar Electrokinetic Chromatography

作　　者：吴美艳[1] 李利军[1] 胡大春[1] 高文燕[2] 李彦青[1] 

机构地区：[1]广西工学院生物与化学工程系,广西柳州545006 [2]广西大学化学化工学院,广西南宁530004

出　　处：《分析科学学报》2011年第6期710-714,共5页Journal of Analytical Science

基　　金：广西自然科学基金(No.0832062)

摘　　要：建立了在线扫集-胶束毛细管电动色谱法(Sweeping-MEKC)测定金感胶囊中的绿原酸、脱水穿心莲内酯和马来酸氯苯那敏的新方法。考察了pH值、四硼酸钠浓度、硼酸浓度、十二烷基硫酸钠(SDS)浓度、电压、有机溶剂和进样时间对分离效果的影响。以12mmol/L四硼酸钠-50mmol/L硼酸-50mmol/L SDS为缓冲溶液(含10%甲醇,pH=9.1),进样时间60s,分离电压20kV,检测波长220nm,采用未涂层熔融石英毛细管(55cm×50μm,有效柱长42cm),环境温度25℃的条件下,达到最佳的分离效果。结果表明,方法富集能力强,对绿原酸、脱水穿心莲内酯和马来酸氯苯那敏的富集倍数分别为850、320和760以上。在优化条件下,3种有机物均在14min内出峰,峰面积的相对标准偏差(RSD)均小于4%。线性范围分别为2.91～46.56μg/mL、2.79～44.64μg/mL和3.98～63.68μg/mL;回收率分别为93%～103%,96%～110%和97%～111%;基于3倍信噪比(S/N=3)计算得到检出限分别为142、92和106μg/L。A sweeping-micellar electrokinetic chromatography（sweeping-MEKC） was used for the simultaneous separation and determination of chlorogenic acid,dehydroandrographolide and chlorphenamine maleate in Jingan capsule.The determination conditions including pH in background solution,concentration of sodium tetraborate,boric acid,sodium dodecylsulfate（SDS） and methanol were optimized.The result indicated that a best separation of the three organic compounds was obtained on a uncoated fused silica capillary column（55 cm×50 μm,effective length 42 cm） by using the background electrolyte containing 12 mmol/L sodium tetraborate,50 mmol/L boric acid,50 mmol/L SDS and 10%（by volume） methanol at pH=9.1 with a constant temperature of 25℃.The detection wavelength was set at 220 nm,sample injection voltage was 20 kV,and injection time was 60 s,respectively.The result showed that the enhancement of chlorogenic acid,dehydroandrographolide and chlorphenamine maleate was above 850,320 and 760 times by sweeping-MEKC.Under the optimum conditions,the separation of the three organic compounds was performed within 14 minutes with relative standard deviations（RSDs） of peak area less than 4%.The calibration curves showed good linearity in the range of 2.91～46.56 μg/mL for chlorogenic acid,2.79～44.64 μg/mL for dehydroandrographolide and 3.98～63.68 μg/mL for chlorphenamine maleate with detection limits（S/N=3） of 136 μg/L,71 μg/L and 93 μg/L,and the spiked recoveries were 93%～103%,96%～110% and 96%～110%,respectively.

关 键 词：胶束电动毛细管色谱 扫集法 绿原酸 脱水穿心莲内酯 马来酸氯苯那敏 

分 类 号：O657.8[理学—分析化学]