毛细管电泳-间接紫外检测法测定蜂蜜中的氨基酸

采用毛细管电泳-间接紫外检测法同时分离测定蜂蜜中的赖氨酸、色氨酸、谷氨酸等9种氨基酸。考察了磷酸浓度、进样方式和缓冲液pH对分离效率和重现性的影响。在分离电压为-15 kV、检测波长为220 nm条件下,以含有0.5 mmol/L十六烷基三甲基溴化铵、20 mmol/L烟酸、10%甲醇的10 mmol/L磷酸二氢钠缓冲溶液(pH 10.2)为运行缓冲液,9种组分在11 min内达到基线分离;检出限最低可达到0.3 mg/L;线性范围为1.0~1000 mg/L;日间及日内精密度为0.64%~5.83%。实际样品中除甲硫氨酸外的8种氨基酸的加标回收率为60.00%~118.37%。将该方法应用于不同蜜源植物和产地的蜂蜜样品的测定,在市售的5种蜂蜜中均检测到脯氨酸、丝氨酸和天冬氨酸,而只在荔枝蜜中检测到苏氨酸。该方法可以为蜂蜜的蜜源鉴别及质量评估提供借鉴方法。     

高效毛细管电泳-紫外检测法快速分离测定三种抗肿瘤药物

肿瘤发生率近年呈明显升高趋势,建立快速、灵敏的抗肿瘤药物分离检测新方法,对指导临床用药,了解药物在体内的代谢等具有重要意义。建立了高效毛细管电泳-紫外检测法快速分离测定10-羟基喜树碱(10-Hydroxy camptothecin,10-HCPT)、6-巯基嘌呤(6-mercaptopurine,6-MP)、5-氟尿嘧啶(5-Fluorouracil,5-Fu)3种抗肿瘤药物的方法。考察了检测波长、分离电压、进样时间、缓冲液的pH值及离子强度对分离效果的影响。以未涂层熔融的石英毛细管(60.2cm×75μm,有效长度50cm)为分离柱,50.0 mmol·L~(-1)硼砂-200.0 mmol·L~(-1)硼酸(pH 8.4)为分离缓冲液,分离电压为21kV,柱温为25℃,0.5psi压力进样5s,于214 nm波长下检测,3种抗肿瘤药10min内能够完全分离。在最佳分析条件下,3类抗肿瘤药物分别在0.1～50.0μg·mL~(-1)、0.5～50.0μg·mL~(-1)、0.2～50.0μg·mL~(-1)范围内线性良好,相关系数r0.9990。对3种抗肿瘤药物平行测定7次,相对标准偏差(RSD)均低于0.85%,检出限(S/N)分别为0.05μg·mL~(-1)、0.2μg·mL~(-1)、0.1μg·mL~(-1),加标回收率为90.4%～103.8%。整个试验过程未使用有机溶剂,方法用于尿样、血样样品的测定,结果令人满意,为临床对10-HCPT、6-MP、5-Fu 3种抗肿瘤药物的用药监测提供了更加简单快速的分析方法。     

毛细管电泳-间接紫外检测法分离和测定食品中的有机酸

有机酸毛细管电泳（CE）分析是90年代初首先被报道的[1],近年来有了较大的发展[2]．采用CE法可进行不同基质样品如食品、饮料、尿液等样品中多种有机酸的同时分析[1,3,4]．该法采用CE的阴离子分离模式,在电解质溶液中加入电渗流改性剂,使电渗流方向逆向,从而与阴离子的电泳方向一致,以缩短分析时间．常见有机酸在200um以上大多无紫外吸收,一般采用间接紫外检测方法[1,3],也可采用低波长紫外检测[4]．低分子量阴离子的CE研究报道不多[5,6],有机酸的CE分离系统研究尚未见报道．本文系统地研究了毛细管电泳-间接紫外检测法分析…     

毛细管电泳-紫外检测法同时测定食品中的葡萄糖和多种糖醇

建立了食品中葡萄糖、半乳糖醇、甘露醇、山梨醇、赤藓糖醇、木糖醇和麦芽糖醇的毛细管电泳-紫外检测同时测定方法。食品中的葡萄糖和糖醇在硼砂碱性介质中与硼酸根结合形成阴离子配合物后,在添加了电渗流改性剂十六烷基三甲基溴化铵的硼砂缓冲液(pH 9.2)中进行快速电泳分离,紫外检测器于195 nm处检测。在优化的条件下,7种物质在12 min内基线分离,标准曲线线性良好(r>0.999),检出限均低于0.1g/L,加标回收率为81.6%~120%,相对标准偏差(RSD)小于6%。方法适用于食品中葡萄糖和多种常见糖醇的同时检测。     

非水体系毛细管电泳-紫外检测法测定苯甲酸和苯甲醛

建立了用非水相体系高效毛细管电泳-紫外检测法同时测定苯甲酸和苯甲醛的新方法，考察了运行电压、非水相介质和电解质等因素的影响，在25℃下，以V（乙腈）：V（碳酸丙烯酯）=1：1的混合液为溶剂，缓冲体系中含15mmol／L十六烷基三甲基溴化铵体积分数1％乙酸，重力进样30S，运行电压20kV，毛细管总长45cm有效长度30cm，φ75μm，检测波长285nm。苯甲酸线性范围为5～40μg／mL，线性方程为：Y=13．473ρ＋13．336，相关系数r=0．9985，检出限为0．92μg／mL，RSD为3．8％。苯甲醛的线性范围75～1125μg／mL线性方程为：Y=5．2449ρ＋564．01，相关系数r=0．9997，检出限为15．60μg／mL，RSD为3．5％。已用于经空气氧化后的苯甲醛中苯甲酸和苯甲醛的测定。     

高效毛细管电泳-二极管阵列检测法测定土壤中的苯酚

建立了高效毛细管电泳-二极管阵列检测器测定土壤样品中苯酚的方法,研究了检测波长、缓冲体系、缓冲体系的pH值及浓度、分离电压、进样时间及压力等因素。结果表明,在温度25℃、pH=10的30mmol/L K2HPO4+0.5mmol/L十四烷基三甲基溴化铵(TTAB)运行缓冲溶液、检测波长206nm、20kV运行电压、负电压模式、0.5psi进样10s条件下,苯酚在4.2到4.4min内出峰,迁移时间和峰面积的相对标准偏差(RSD)分别为0.11%、0.28%,检出限(3Sb/Sx)为0.01mg/L。该方法成功地应用于土壤中苯酚的测定,其回收率为98.4%。     

单糖的高效毛细管电泳间接紫外检测法研究

本文研究了单糖的毛细管电泳间接紫外检测法。实验发现选用β－哚吲乙酸－磷酸钠体系作为背景电解质比较理论想，用于９种未经衍生的单糖进行毛细管电泳分离和间接紫外检测可取得满意结果，对半乳糖，甘露糖和葡萄糖酸的检出极限为２－１０ｐｍｏｌ水平。本文还讨论了背景电解质浓度与样品响应值的关系以及各种操作条件的影响。     

毛细管电泳-电化学检测法测定饲料中的磺胺类药物

采用毛细管电泳-电化学检测法(CE-ED),对饲料中的6种磺胺类药物磺胺脒、磺胺二甲嘧啶、磺胺甲嘧啶、磺胺二甲氧嘧啶、磺胺嘧啶、磺胺甲恶唑进行了分离和测定。分别考察了工作电极电位、运行缓冲液的pH和浓度、分离电压和进样时间等实验参数对实验结果的影响。在优化的实验条件下,以直径300μm的碳圆盘电极为工作电极,检测电位为0.95 V(vs.SCE),在30 mmol/L硼砂-KH2PO4(pH7.6)的运行缓冲溶液中,6个分析物能够在16 min内实现很好的基线分离,被测物浓度与峰电流在3个数量级呈良好的线性,检出限(S/N=3)范围0.08～0.20μg/mL。该方法已应用于实际样品的分析。     

毛细管电泳-电化学检测法测定葡萄和葡萄酒中的白藜芦醇

采用毛细管电泳-电化学检测法测定了葡萄和葡萄酒中的白藜芦醇含量,实验发现白藜芦醇在红葡萄酒中的含量明显高于其在白葡萄酒中的含量,并验证原因为葡萄皮中白藜芦醇的含量显著高于葡萄肉中白藜芦醇的含量。考察了工作电极的工作电位、分离电压和进样时间对检测的影响。在优化条件下,以300μm直径的碳圆盘电极为工作电极,工作电位为+0.85V(vs.SCE),在100mmol/L硼酸盐(pH=9.2)的运行缓冲液中,被测物浓度与峰电流在3个数量级范围内呈良好线性,检出限为1×10-7g/mL。该法简单可靠,已成功地应用于实际样品中白藜芦醇含量的测定;样品处理简单,无须预富集,检测结果令人满意。     

毛细管电泳-激光干涉检测法测定饮料中蔗糖含量

本文将毛细管电泳-激光干涉检测法用于饮料中蔗糖的定量测定.结果表明,在样品浓度低于10mg/mL时,检测信号与样品浓度成正比.样品不需衍生化处理直接进行测定,分析结果较为满意.     

Determination of sulfate ester content in sulfated oligo‐ and poly‐saccharides by capillary electrophoresis with indirect UV detection

Carbohydrates having sulfate groups such as glycosaminoglycans and chemically synthesized sucrose sulfate show interesting and important biological activities. We adapted CE with indirect UV detection technique to the determination of sulfate ester in sulfated carbohydrates, which were previously hydrolyzed with HCl. The liberated sulfate ion was analyzed using a background electrolyte consisting of triethanolamine‐buffered chromate with hexamethonium bromide. Sulfate contents of glucose 3‐sulfate and sucrose octasulfate used as a model were in good agreement with theoretical values (accuracy, 95.9–96.7 and 97.4–101.9%, respectively), and relative standard deviation values run‐to‐run were 0.977 and 1.90%, respectively. We applied the method to the determination of the sulfate contents of some glycosaminoglycan samples and showed that the contents were in good agreement with those calculated from sulfur content. Copyright © 2010 John Wiley & Sons, Ltd.     

Separation of perfluorocarboxylic acids using capillary electrophoresis with UV detection

A capillary electrophoretic method with UV detection for separation and quantitation of perfluorocarboxylic acids (PFCAs) from C6-PFCA to C12-PFCA has been developed. The optimization of measurement conditions included the choice of the most appropriate type and concentration of buffer in the background electrolyte (BGE), as well as the type and the content of an organic modifier. The optimal separation of investigated PFCAs was achieved with 50 mM phosphate buffer and 40% isopropanol in the BGE using direct UV detection. The optimum wavelength for direct UV detection was optimized at 190 nm. For indirect detection, several chromophores were studied. Five mM 3,5-Dinitrobenzoic acid (3,5-DNBA) in 20 mM phosphate buffer BGE and indirect UV detection at 280 nm gave the optimal detection and separation performance for the investigated PFCAs. The possibility of on-line preconcentration of solutes by stacking has been examined for indirect detection. The detection limits (LODs) determined for direct UV detection ranged from 2 microg/mL for C6-PFCA to 33 microg/mL for C12-PFCA. The LODs obtained for indirect UV detection were comparable to those obtained for direct UV detection.     

Indirect UV detection of carbohydrates in capillary zone electrophoresis

Summary A new system for the rapid and sensitive analysis of underivatized carbohydrates has been established using capillary zone electrophoresis with indirect UV detection. At an applied potential of 28 kV, sugars and sugar acids could be separated by the combined effects of electroendosmosis and electrophoresis within 20 minutes in a fused silica capillary of 50 m internal diameter and an effective length of 100 cm using 6mM sorbic acid, pH 12.1, as both carrier electrolytie and chromophore. The alkaline pH ensured ionization of the sugars and, hence, their detection by means of charge displacement. Furthermore, the chosen concentration of sorbic acid allowed the smallest fractional change in the background signal to be measured. While the electrophoretic mobilities of the sugars were found to increase within a pH range of 11.9 to 12.3, those of the sugar acids were not affected. Due to the increasing competition of hydroxide ions in the displacement of the chromophore with rising pH, a significant loss of sensitivity is observed at pH values higher than 12.1 and this pH was found to provide sufficient resolution, optimum sensitivity, and a acceptably short analysis time. Under these conditions, a lower detection limit of 2 pmol was obtained for glucose.     

非水介质毛细管电泳电导检测罗红霉素及其制剂

采用甲醇为分离介质，三(羟甲基)氨基甲烷-硼酸(Tris—H3BO3)为支持电解质，采用负高压，使用电导检测，对罗红霉素及其制剂进行了毛细管电泳分离检测，对电泳介质的种类、浓度、表观pH、以及操作电压和进样时问对分离的影响进行了研讨，在选定的条件下，罗红霉素的线性范围为19．0—142．0mg/L，检出限为0．8mg/L(S／N≥3)，峰面积的相对标准偏差RSD(n=6)为4．3％。3种供试品中罗红霉素的平均加标回收率分别为97．7％、94．8％、93．6％。     

毛细管电泳-安培检测法测定女贞子中齐墩果酸的含量

女贞子又名冬青子,性凉,味甘、微苦,归肝、肾经,具有滋补肝肾、明目乌发的功能.女贞子主要有效成份为齐墩果酸Oleanolic Acid(OA)[1],其化学结构式如图1所示.OA是天然产物化学成分,毒性很低,具有多种生物活性如抗病毒、消炎、增强免疫和抑制免疫、抑制血小板凝集、降血脂、降糖、保肝、护肾、抗艾滋病毒等[2],故测定其含量可为药品的含量控制提供科学依据.     

高效毛细管电泳法测定二氢叶酸还原酶活力的研究

通过胶束电动毛细管电泳法研究分离二氢叶酸还原酶体系中二氢叶酸、四氢叶酸、 NADP、 NADPH和酶5种组分,在含0.002%Brij-35的pH 9.18 50 mmol/L 的硼砂缓冲溶液中,5种组分在18min内得到基线分离.通过对其产物四氢叶酸峰面积的定量测定,计算出二氢叶酸还原酶的米氏常数,建立了毛细管电泳法对二氢叶酸还原酶活力的测定方法.     

DNA fragment separations by on‐line combination of capillary isotachophoresis–capillary zone electrophoresis with UV detection

A high‐speed DNA fragment separation system based on an on‐line combination of capillary ITP with CZE (CITP‐CZE) and using UV detection at 260 nm was developed. A novel CITP‐CZE buffer system of pH 6.1 was designed for the separation of ten DNA fragments with sizes ranging from 100 to 1000 bp. An effect of underivatized α‐, β‐ and γ‐cyclodextrins on the resolution of DNA fragments in the CZE step of the CITP‐CZE combination was systematically investigated. Methylhydroxyethylcellulose present in the BGE was used to eliminate the EOF. DNA ladder fragments were separated within 10 min with LODs in the range of 1–5 ng/μL (S/N = 3). The RSDs of the migration time and peak area of individual DNA fragments were in the range of 1–3 and 3–9%, respectively. The developed CITP‐CZE system was further applied to the analysis of digest plasmid DNA samples.     

高效毛细管电泳分离及检测蛋氨酸对映体

蛋氨酸（Methionine）学名甲硫基丁氨酸,分子式C5H11NO2S,相对分子质量149．2。在蛋白质合成中,蛋氨酸是信息核糖核酸“翻译”成蛋白质过程中的第一步。无蛋氨酸的存在,蛋白质生物的合成就无法开始。适用于防治肝脏疾病和砷中毒,也用作食品的添加剂。蛋氨酸有D,L两种构型。目前尚未见用Cu^2＋做手性选择剂毛细管电泳电化学拆分D,L-蛋氨酸的报道。电化学检测（主要是安培检测和电导检测）具有操作简单、维护方便、无须衍生化处理等优点,     

Brompheniramine as a novel probe for indirect UV detection and its application for the capillary electrophoresis of adamantane drugs

Brompheniramine, an antihistamine drug, was employed as a novel UV probe for capillary electrophoresis with indirect UV detection of adamantane drugs (memantine, amantadine, and rimantadine). The probe possesses high molar absorptivity of 24 × 10³ L/mol cm at 6 mM, which enables the measurement of these nonchromophore analytes without derivatization. The simple background electrolyte (10 mM sodium dihydrogen phosphate (pH 5.0) containing 5 mM brompheniramine and 6 mM β‐cyclodextrin) provided the separation of the analytes in a short time (7.5 min). Under these conditions, brompheniramine had similar mobility to that of the analyte ions resulting in symmetric peaks with minimal electrodispersion. The analytes displace the probe at a one‐to‐one ratio with transfer values close to unity. β‐Cyclodextrin played a role in the resolution of the structurally similar adamantane derivatives. Method validation showed good linearity (r ² > 0.98), precision (%RSD ≤ 3.30), and accuracy (recoveries ranging from 98 to 109%). The proposed method was successfully applied to determine the adamantane content in pharmaceutical products.