Separation of Hydrophobic Neutral Compounds by Microemulsion Electrokinetic Chromatography

Electrokineticchromatography(EKC)istheonlymodeofcapillaryelectrophoresisfOrtheseparationofelectricalneutralcompounds.Theseparationprincipleisbasedonthedifferentpartitionofsolutesbetweenthepseudostationaryphaseandthesurroundingaqueousphase.MicellarEKC(MEKC)provideshighspeedandhighefficiencyseparationforneutralcompoundswithsignificantsolubilityinaqueoussystem'.Theseparationofhydrophobiccompounds,however,givessomeproblems,becauseoftheirpoorsolubilityinaqueousphase.Inourpreviouswork"',somepol…     

蛋白质的微乳液毛细管电动色谱分离研究

考察了用微乳液毛细管电动色谱(MEEKC)分离蛋白质时微乳液组成等不同因素对分离的影响,并与胶束电动色谱进行对比,探讨了其分离机理,为蛋白质的分离鉴定提供了一种有力的工具.     

Optimized Separation of Nine Xanthones by Microemulsion Electrokinetic Chromatography

A microemulsion electrokinetic chromatography method has been firstly used for the separation of the therapeutically important xanthones from Securidaca inappendiculata. The separation of the nine xanthones was systematically optimized with respect to pH, composition of microemulsion,addition of cyclodextrins, applied voltage and column temperature. Baseline separation was successfully achieved for the nine xanthones, which was also compared with that by micellar electrokinetic chromtography.     

Chiral Separations by Ligand-Exchange Micellar Electrokinetic

The separation of enantiomers is of great importance in biology, pharmaceutics, agriculture and environment. The different separation modes ( i. e. capillary zone electrophoresis ( CZE ), micellar electrokinetic chromatography ( MEKC ), capillary electrochromatography ( CEC ), etc )     

Separation of Aniline Derivatives by Micellar Electrokinetic Capillary Chromatography

A micellar electrokinetic capillary chromatography (MECC) was developed for the determination of aniline and 6 substituted anilines. The seven components were separated within 25min in the buffer solution of 40mmol/L sodium borate and 100mmol/L SDS. It was found that the separation was dependent on operating voltage, pH value, borate and SDS concentrations.The analytical performance was examined in terms of linear response and reproducibility.Wastewater was determined by the established method.     

电中性物质的毛细管胶束电动色谱

在自制的高效毛细管电泳装置上,使用内径为0.05毫米,长为450毫米的熔融石英毛细管,十二烷基硫酸钠胶束溶液,254nm检测波长,进行了电中性化合物的毛细管胶束电动色谱研究。并将乙醇-水混合溶剂引入体系,成功地进行了多环芳烃的分离。考察了电场强度,SDS浓度及乙醇含量对柱效的影响。     

Separation of Felted Explosives by Pressurized Microemulsion Electrokinetic Chromatography

A new MEEKC method assisted with pressure-driven mobile phase was presented for the separation of felted explosives. Microemulsion solution was composed of 80 mmol/L heptane-120 mmol/L SDS (sodium dodecyl sulphate)-900 mmol/L butanol-10 mmol/L borate at pH 9.4 and a pressure-driven flow of 0.020 mL/min under 1.3 MPa was employed to manipulate the separation. Explosives HMX (1,3,5,7-tetranitro-1,3,5,7-tetrazacyclooctane) and TATB(triamino-trinitrobenzene), which were felted on fluorine rubber F2311 (polytrifluorochlorethylene and polyvinylidene fluoride 1/1 co-polymerization) and F2314 (polytrifluorochlorethylene and polyvinylidene fluoride 4/1 co-polymerization) were well separated with very good peak shapes.     

微乳电动色谱法的研究进展

微乳电动色谱(MEEKC)是一种以微乳为背景电解质,以电压为驱动力的分离技术。本文对MEEKC中的各调节参数进行了概述,重点归纳了MEEKC法在正辛醇-水分配系数测定、中药和手性化合物分离方面的应用,以及在操作技术上的新进展,如多路进样技术以及在线联用质谱检测技术等,并通过对相关文献的分析,对一直存有争议的MEEKC与胶束电动色谱(MEKC)的联系与区别进行了讨论,最后提出了MEEKC法未来的发展空间。     

微乳电动毛细管色谱分离分析氟喹诺酮类药物

建立了一种同时分离7种氟喹诺酮类药物(FQs)的微乳液电动毛细管色谱(MEEKC)。用十二烷基硫酸钠(SDS)作为表面活性剂,系统考察了缓冲溶液浓度和pH、SDS、助表面活性剂和油相的浓度、温度等对分离的影响。最佳分离条件为:1%正庚烷(V/V),100mmol/LSDS,10%正丁醇(V/V)和8mmol/L磷酸盐-四硼酸钠缓冲溶液(pH7.30)。以氧氟沙星(OF)作内标,FQs标准水溶液和标准血清溶液的线性范围分别为1.2×10-6~5.0×10-4mol/L和2.0×10-6~5.0×10-4mol/L,检出限(S/N=3)均为9.7×10-7mol/L。方法直接应用于滴眼液中环丙沙星(CPF)的测定,精密度和准确度高;应用于血液中加替沙星(GTF)的测定涉及固相萃取预处理样品,萃取平均回收率为90.6%,日内、日间精密度分别为3.3%和3.6%,结果满意。     

胶束电动毛细管色谱法拆分肾上腺素对映体

胶束电动毛细管色谱法拆分肾上腺素对映体;电化学检测;对映体拆分     

微乳液毛细管电动色谱法测定大鼠滑膜细胞中雷公藤甲素的含量

建立微乳液毛细管电动色谱法快速测定大鼠滑膜细胞内外液中雷公藤甲素含量的方法.在雷公藤甲素不同给药时间孵育条件下,将滑膜细胞分为空白对照组和给药组,测定滑膜细胞内外液中雷公藤甲素含量,并比较了细胞外液中雷公藤甲素在不同给药时间的含量变化.毛细管电泳运行缓冲液组成:1％(w/V)SDS,3％(V/V)正丁醇,1％(V/V)乙酸乙酯,96％(V/V)5 mmol/L硼砂-10 mmol/L磷酸盐溶液,pH 9.0;运行电压:25 kV;压力进样:0.5 psi×6 s;电泳操作温度:25℃;检测波长:214 nm.结果表明,细胞内外液中的雷公藤甲素所呈现的线性关系良好,相关系数分别为0.9995和0.9991.当给药24h时,细胞内外液中的雷公藤甲素浓度分别为0.736和20.745 μg/mL.本方法简单准确、灵敏度高、精密度好,可用于滑膜细胞内外液中雷公藤甲素浓度的动态变化规律研究,为进一步研究中药有效成分对滑膜细胞功能和活性的影响提供方法学基础.     

胶束电动毛细管色谱法分析手性化合物

对近年来胶束电动毛细管色谱法（ＭＥＣＣ）分析手性化合物方面的工作进行了评述,简述了ＭＥＣＣ分离手性化合物的原理,并探讨了几种ＭＥＣＣ手性分离体系的分离机理。     

用胶束毛细管电动色谱法分离三硝基甲苯异构体的研究

用胶束毛细管电动色谱法（ＭＥＫＣ）分离三硝基甲苯（ＴＮＴ）异构体。研究了背景电解质、十二烷基硫酸钠（ＳＤＳ）浓度、缓冲溶液添加剂Ｂｒｉｊ３５、ｐＨ等对分离的影响,找出了最佳分离条件,使三硝基甲苯的６种异构体在几分钟内达基线分离。     

微乳毛细管电动色谱快速分析脂溶性维生素

建立了一种新的微乳体系,成功地应用于微乳毛细管电动色谱(MEEKC)快速分析脂溶性维生素VA、VD3和VE.本微乳液的组成为:1.2%(m/m)十二烷基硫酸钠(SDS)-21%(V/V)正丁醇-18%(V/V )乙腈-0.8%(m/m)正己烷-20 mmol/L H3BO3-Na2B4O7缓冲液( pH 8.4 ).该微乳体系中,助表面活性剂正丁醇和有机溶剂乙腈对脂溶性维生素的分离起到了重要的作用.当分离电压为25 kV,柱温为25 ℃时,VA、VD3和VE在13 min内达到基线分离.3种脂溶性维生素的迁移时间和峰面积的RSD(n= 5)<2.5%和4.5%;VA、VD3和VE分别在20～1000、5～1000和5～1000 mg/L范围内与峰面积呈线性关系;检出限(S/N=3)分别为12、 0.72和0.29 mg/L.本体系应用于市售VE胶囊的测定,结果与标示值相符.     

Separation of Six Pyridoncarboylxic Acid Derivatives by Micellar and Microemulsion Electrokinetic Chromatography

Micellar electrokinetic chromatography (MEKC) and microemulsion electrokinetic chromatography (MEEKC) are two kinds of electrokinetic capillary chromatography (EKC), which are characterized of high solubilization capacity and separation efficiency. In our previous work, some polar organic compounds and hydrophobic neutral compounds were separated successfully by EKC1-3. In this paper, these methods were used for separating six pyridoncarboylxic acid derivatives with similar structures. T…     

微乳电动毛细管色谱分离山酮类化合物的影响因素

在优化微乳系统(如pH、缓冲液浓度、表面活性剂、助乳剂、油相及添加剂)的基础上,对影响微乳电动毛细管色谱(MEEKC)分离山酮类化合物的因素进行了系统研究。以正辛醇-水分配系数(疏水常数log P)、色谱峰对称因子和理论塔板数作为参数,研究了分离条件的改变对MEEKC分离性能的影响。结果表明,色谱条件的改变对疏水性山酮和亲水性山酮分离选择性的影响存在着显著差异,当微乳体系为50 mmol/L硼酸缓冲液(pH 9.5)、10%(体积分数)正丁醇、80 mmol/L正庚烷、120 mmol/L十二烷基硫酸钠和     

微乳电动毛细管色谱法分离检测酱油中的氯丙醇

建立了微乳电动毛细管色谱分离3种氯丙醇的方法。以十二烷基硫酸钠(SDS)作为表面活性剂,系统考察了pH值、缓冲溶液类型和浓度、SDS浓度、助表面活性剂浓度、油相浓度、温度和运行电压对3-氯-1,2-丙二醇(3-MCPD),1,3-二氯-2-丙醇(1,3-DCP),2,3-二氯-1-丙醇(2,3-DCP)分离的影响。结果表明,最佳微乳缓冲液为1%(V/V)正庚烷,100 mmol/L SDS,10%(V/V)正丁醇和8 mmol/L磷酸二氢钠-硼砂溶液(pH 8.50),检测波长为192 nm,温度20℃,分离电压为15 kV。3种氯丙醇的线性范围为2.0×10-6～3.2×10-5 mol/L,相关系数大于0.996,检出限(S/N=3)为0.95～1.9μmol/L。酱油样品经乙醚液液萃取,萃取平均回收率为93.2%～103.0%,相对标准偏差小于6.5%。本方法应用于实际样品和加标后样品中三氯丙醇的检测,结果满意。     

几种核苷的毛细管胶束电动色谱分离

在胶束电动色谱模式下,考察了影响核苷分离的缓冲溶液、SDS浓度、pH、表面活性剂、有机添加剂、分离温度及外加电压等重要因素,并优化了关键的分离条件,建立了一种简单快速的利用毛细管胶束电动色谱DAD检测器分离分析核苷的新方法。当缓冲溶液为36 mmol/L硼酸缓冲液(pH 9.0)、30 mmol/L SDS和3%(V/V)乙腈,分离电压为25 kV和分离温度为25℃时,5种核苷在6 m in内实现了令人满意的基线分离。在优化的条件下,对其线性范围、检出限和重现性进行了测定。结果表明,核苷的迁移时间的重现性<1%;面积的重现性<3%。所建立的分离方法的线性范围宽,检出限低,重现性好。     

The Retention Behaviors of Benzene and Its Alkyl Homologues in Microemulsion Electrokinetic Chromatography

MicroemulsioneIectrokineticchromatography(MEEKC)isonekindofelectrokineticchromatography(EKC),whoseseparationprincipIeisbasedonthedifferentpartitionofsolutesbetweenthepseudostationaryphaseandthesurroundingaqueousphase.Usingmicroemulsionsolutionasthepseudostationaryphase,MEEKCshowsahighsolubilizationcapacityandseparationefficiency"'.Inthiswork,theretentionbehaviorsofalkylbenzenesinbothanionicandcationicsurfactantMEEKCsystemswereinvestigated.Theeffectsofco-surfactantandsurfactantonseparat…     

鼠李糖脂应用于微乳毛细管电动色谱快速测定化妆品中激素类物质

采用生物表面活性剂鼠李糖脂建立了无需助表面活性剂的微乳体系,并应用于微乳毛细管电动色谱快速分析化妆品中皮质类激素泼尼松、泼尼松龙和氢化可的松。考察了pH值、鼠李糖脂浓度、离子强度、油相种类和浓度、分离温度、分离电压及进样电压和时间的影响,得出微乳体系最佳组成为0.1%(w/w)鼠李糖脂+0.8%(w/w)正庚烷+99.1%(w/w)硼砂缓冲液(80 mmol/L,pH 9.2)。分离温度20℃,分离电压20kV,电动进样10 kV×3 s,泼尼松、氢化可的松和泼尼松龙在9.4 min内可基线分离。重复进样7次,迁移时间和峰面积的RSD分别小于0.2%和5.0%。3种分析物线性范围均为5～100 mg/L;检出限分别为1.0,1.1和1.3 mg/L(S/N=3)。仅需简单萃取即可用于化妆品样品测定,回收率为81.6%～108%;RSD均小于4.8%。