等速电泳法同时检测无机和有机阴离子

本文介绍了利用自制的ＯＣＥＰ－１型离子分析仪,建立了以Ｃｌ－为前导,正丁酸很为尾随,８－羟基喹啉为缓冲配对离子的等速电泳分离系统的新分离分析方法,对ＮＯ＿３,ＮＯ＿２,Ｆ￣－,ＨＣＯＯ￣－及ＣＨ３ＣＯＯ￣－进行分离和同时检测,获得满意的结果。     

自由溶液和筛分介质条件下芯片DNA瞬间等速电泳预浓缩的比较

利用芯片电泳方法考察瞬间等速电泳-筛分电泳偶联分析的结果,比较了自由溶液和筛分介质中DNA瞬间等速电泳的预浓缩效果.结果显示,相比较于筛分介质条件,自由溶液瞬间等速电泳有利于改善预浓缩和后续筛分电泳分离效果.对此结果的解释是:自由溶液条件下DNA迁移速度的提高可以延长瞬间等速电泳持续时间,有利于提高预浓缩效率.此外,样品压缩区带在自由溶液-筛分介质界面的二次富集也是预浓缩效果得到改善的原因之一.     

毛细管电泳中样品在线预富集方法

本文对高效毛细管电泳中样品在线预富集方法作了评述，包括瞬间等速电泳，反流速电泳，场放大进样，场放大排除基体和固相萃取等技术，引用文献81篇。     

毛细管电泳中的样品在线富集技术及其应用

毛细管电泳作为一种快速、高效的分离分析技术,已应用于许多领域.该文就近年来毛细管电泳中的样品堆积、扫集、等速电泳、动态pH连接及固相萃取等样品富集方法的原理进行了简单介绍,并对它们的应用进行了总结和评述,引用文献161篇.     

强酸阴离子的等速电泳分析

等速电泳能同时分析多种离子,尤其可分析未经前处理的样品,仪器价格也相对低廉。等速电泳过程需要高迁移率的前导离子和低迁移率的终末离子作为电泳电解质,Cl~-是常用     

柱偶联装置在毛细管等速电泳中的应用

根据自制的ＯＣＥＰ－１型离子分析仪的特点，设计了一套新的住偶联装置。提高了分离容量，可以用来检测复杂混合物中的低浓度组分。用等速电泳法测定了高浓度Ｃｌ＾－，Ａｃ＾－存在时的Ｆ＾－。这个装置对于处理离子性组分，无论在研究工作还是实际分析工作中，都是很有用的。     

毛细管区带电泳

一、历史与现状 毛细管区带电泳(CZE)或高效毛细管电泳(RPCE)是继色谱之后的又一高效快速分析方法,近年来发展极快(图1)。CZE的研究热潮正在英国掀起,并向其他国家扩展。CZE是第六届国际等速电泳会议的主题之一,在88年的Pitts-burg会上受到高度重视。其首届专题国际会议也     

猪肝DFP酶催化水解反应产物的等速电泳分析

ＤＦＰ酶可催化水解二异丙基氰磷酸酯分子中的Ｐ－Ｆ键,使其断裂产生磷酸二异丙基酯和ＨＦ。根据电位滴定法和离子选择电极法对猪肝中发现的两种ＤＦＰ水解酶活力测定的结果,利用毛细管等速电泳分析仪对这两种酶催化ＤＦＰ水解的产物进行了定性分析。     

猪肝DFP酸催化水解反应产物的等速电泳分析

DFP酸可催化水解二异丙基氟磷酸酯（DFP）分子中的P－F键,使其断裂产生磷酸二异丙基酯和HF。根据电位滴定法和离子选择电极法对猪肝中发现的两种DFP水解酶活力测定的结果,利用毛细管等速电泳分析仪对这两种酶催化DFP水解的产物进行了定性分析。结果表明,猪肝中小分子质量的酸催化DFP水解反应时,并非水解P－F键．而是水解P－OR键,说明该酶是一种催化DFP分子中磷酯健水解的磷酯酶。     

新型无泵阀毛细管等速电泳仪的研制——Ⅰ.积木式分离管路结构及电位梯度检测器

本文介绍本实验室研制的新型无泵阀毛细管等速电泳仪的积木式分离管路结构及电位梯度检测器,该管路结构及检测器构造均较现有的仪器简单、合理,拆卸和组接方便,造价低廉,用其构成的无泵阀毛细管等速电泳仪分离分析阴、阳离子样品,结果表明该仪器的检测灵敏度及重现性等均良好。     

微波衍生-离子对高效液相-磺化四苯基卟啉光度法同时测定痕量镍、铜、锰和锌

 用磺化四苯基卟啉 (TPPS4 )作柱前衍生试剂 ,在微波作用下进行衍生反应 ,研究了衍生和分离Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的最佳条件。在 75 0W的微波作用下衍生反应 3min ,在C18柱上采用乙腈 水 (体积比为 2 2 5∶77 5 )体系作流动相 ,四乙基溴化铵 (TEABr)作离子对试剂 ,在 415nm处检测 ,建立了微波衍生 离子对高效液相快速分离、光度检测Ni2 + ,Mn2 + ,Zn2 + 和Cu2 + 的新方法。络合物和反应试剂在 15min内出峰完毕。Zn2 + ,Cu2 + ,Ni2 + 和Mn2 + 的检测限分别为 0 0 5 μg/L ,0 0 1μg/L ,0 10 μg/L和 0 40 μg/L。     

Direct determination of valproate in serum by zone electrophoresis–isotachophoresis on a column‐coupling chip

A feasibility study was performed using zone electrophoresis (ZE) coupled on‐line with isotachophoresis (ITP) sample pretreatment on a poly(methyl methacrylate) column‐coupling chip with integrated conductivity detection for direct determination of drugs in serum. Valproic acid (an antiepileptic drug), having a therapeutic range of 0.35–0.69 mmol/L (50–100 mg/L), was a test analyte while reference serum samples served as proteinaceous matrices. ITP provided in the ITP‐ZE combination a multitask sample pretreatment: (1) separation of the analyte from the serum matrix and its concentration into a narrow ITP band, (2) removal of the matrix constituents migrating in the ITP stack from the separation compartment of the chip, (3) ITP stacking of the drug released on a continuous electrophoretic decomposition of the drug‐protein complex. A high sample loadability, closely linked with the use of ITP in the first separation stage, made it possible to inject diluted serum samples with the aid of a 0.95 μL sample channel of the chip. Consequently, a 1–2 μmol/L concentration limit of quantitation for valproate from the response of the conductivity detector in the ZE stage of the combination was reached. The drug could be reliably determined in less than 10 minutes also in instances when its concentration in serum was below the lower value of the therapeutic range. 90–94% recoveries of valproate from serum samples were obtained in its direct ITP‐ZE determination when the filtration of the diluted serum (a 0.45 μm pore size filter) was the only pre‐column sample handling operation. No disturbances attributable to the precipitation of proteins from the loaded samples in the chip channels were detected.     

阳离子交换色谱中色谱柱温度对碱金属与碱土金属离子保留的影响

研究了非抑制型阳离子交换色谱中色谱柱温度(25~50℃)对碱金属离子(Li+、Na+、K+、Rb+)和碱土金属离子(Mg2+、Ca2+、Sr2+)以及NH4+保留的影响。在Shim-pack IC-C1磺酸型阳离子交换柱上,以硝酸为流动相分离碱金属离子,以乙二胺或乙二胺-草酸(柠檬酸)为流动相分离碱土金属离子,随着色谱柱温度的升高,碱金属和碱土金属离子的保留时间均增长,其范特霍夫曲线具有良好的线性关系,斜率为负值,表明在此条件下碱金属和碱土金属离子的保留为吸热过程。在Shim-pack IC-SC1羧酸型阳离子交换柱上,以硫酸为流动相同时分离碱金属和碱土金属离子,随着色谱柱温度的升高,Mg2+、Ca2+的保留时间增长,而K+、Rb+的保留时间缩短,Li+、Na+、NH4+的保留时间基本不变。在此条件下,Mg2+、Ca2+、K+和Rb+的范特霍夫曲线具有良好的线性关系,其中Mg2+和Ca2+的曲线斜率为负值,K+和Rb+的曲线斜率为正值,表明Mg2+和Ca2+的保留表现为吸热过程,K+和Rb+的保留表现为放热过程。研究表明在不同固定相和流动相条件下,色谱柱温度对碱金属和碱土金属离子保留行为的影响不同。     

4-(5-溴-2-噻唑偶氮)间苯二酚反相阳离子对HPLC测定痕量铌、钒、铑、铬

本文报道新试剂4-(5-溴-2-噻唑偶氮)间苯二酚(5-Br-TAR)为柱前衍生试剂,以阳离子表面活性剂作为对离子试剂,用含15 mmol／L的pH 5.8的乙酸-乙酸钠缓冲溶液、0.05 mmol／L溴化钠、10 mmol／L TBA·Br的乙腈-甲醇-水(42 : 13：45,V／V／V)三元体系为流动相,在C8柱上25min内HPLC测定了Nb(V)、V(V)、Rh(Ⅲ)和Cr(Ⅵ)的5-BR-TAR螯合物。当SNR=2时,检出限分别为Nb(V)1.0、V(V)1.6、Rh(Ⅲ)0.9和Cr(Ⅵ)1.9μg／L。该方法用于测定污水中的铬和钒,结果良好。     

高效液相色谱与电感耦合等离子体质谱联用技术用于胁迫富硒海带硒形态研究

通过对海带胁迫富硒培养, 研究了海带对硒的富集总量及硒化学形态转变. 建立了反相离子对缓冲盐等3个色谱系统的高效液相色谱与电感耦合等离子体质谱联用(RP-HPLC-ICP-MS)技术测定亚硒酸钠、硒甲基半胱氨酸(MeSeCys)、硒代蛋氨酸(SeMet)三种硒形态. 采用3种提取溶剂, 超声提取缩短提取时间, 分离检测富硒海带的主要硒形态为亚硒酸钠、硒甲基半胱氨酸和硒代蛋氨酸.     

亲水作用色谱柱与阳离子交换树脂柱结合分离无机离子（英文）

A combination of hydrophilic interaction chromatographic(HILIC) column and a weakly acidic cation-exchange resin(WCX) column was used for simultaneous separation of inorganic anions and cations by ion chromatography(IC).Firstly,the capability of HILIC column for the separation of analyte ions was evaluated under acidic eluent conditions.The columns used were SeQuant ZIC-HILIC(ZIC-HILIC) with a sulfobetaine-zwitterion stationary phase(ZIC-HILIC) and Acclaim HILIC-10 with a diol stationary phase(HILIC-10).When using tartaric acid as the eluent,the HILIC columns indicated strong retentions for anions,based on ion-pair interaction.Especially,HILIC-10 could strongly retain anions compared with ZIC-HILIC.The selectivity for analyte anions of HILIC-10 with 5 mmol/L tartaric acid eluent was in the order of I-> NO-3 > Br-> Cl-> H2PO-4.However,since HILIC-10 could not separate analyte cations,a WCX column(TSKgel Super IC-A/C) was connected after the HILIC column in series.The combination column system of HILIC and WCX columns could successfully separate ten ions(Na+,NH+4,K+,Mg2+,Ca2+,H2PO-4,Cl-,Br-,NO-3 and I-) with elution of 4 mmol/L tartaric acid plus 8 mmol/L 18-crown-6.The relative standard deviations(RSDs) of analyte ions by the system were in the ranges of 0.02%-0.05% in retention times and 0.18%-5.3% in peak areas through three-time successive injections.The limits of detection at signal-to-noise ratio of 3 were 0.24-0.30 μmol/L for the cations and 0.31-1.2 μmol/L for the anions.This system was applied for the simultaneous determination of the cations and the anions in a vegetable juice sample with satisfactory results.     

Simultaneous separation and determination of thallium in water samples by high‐performance liquid chromatography with inductively coupled plasma mass spectrometry

An analytical method for separation and determination of thallium species in water using high‐performance liquid chromatography with inductively coupled plasma mass spectrometry was developed. The composition and concentration of mobile phase, injection volume, and pH value were optimized respectively with an anion or cation exchange column. The results showed that Tl(I) and Tl(III) were effectively separated using anion exchange column Hamilton PRP‐X100, with the mobile phase consisting of 200 mmol/L ammonium acetate and 10 mmol/L diethylenetriaminepentaacetic acid (pH = 4.2). When using a Dionex cation exchange guard column, CS12A, 15 mmol/L HNO₃, and 3 mmol/L diethylenetriaminepentaacetic acid as the mobile phase, Tl(I) and Tl(III) could be effectively separated. The detection limits of the methods were 3–6 and 9–12 ng/L, respectively. In a solution containing Fe ions and oxalic acid, a significant quantity of Tl(I) was oxidized. Fe ions and oxalic acid in the water samples did not interfere with high‐performance liquid chromatography‐inductively coupled plasma mass spectrometry measurement results.     

Focusing of alkali earth metals in ligand step gradient

A capillary electroseparation technique for focusing and selective pre-concentration of metal chelates with subsequent on-line isotachophoresis (ITP) analysis was developed and verified. The ions of alkali earth metals (Mg, Ca, Sr, and Ba) were pre-concentrated from the mixture and analyzed. The focusing of the metals was carried out in a ligand step gradient, which was created by the addition of a convenient ligand agent to the regular stationary pH step gradient. The analytical procedure consisted of three steps. During the first step, the metal ions were electrokinetically continuously dosed into the column where they were selectively trapped on the stationary ligand step gradient in the form of unmoving zones of chelate complexes with effectively zero charge. After a detectable amount of analyte was accumulated, the dosing was stopped. The accumulated zones were mobilized to the analytical column, where they were analyzed by the ITP method with conductivity or photometric detection. The proper electrolyte systems for dosing, mobilizing, and analyzing in isoelectric focusing (IEF), moving boundary electrophoresis (MBE), and ITP modes were consequently developed and put into practice. The trapping selectivity can be regulated by the choice of pH and convenient complexing agents. A mixture of alkali earth metals were used as model analytes. Using a 3000 s dosing time, the proposed method improved the detection limit by 5-29 times in comparison to analysis by ITP with classical injection.     

反相高效液相色谱法测定罐头食品中乙二胺四乙酸的残留量

 将罐头食品捣碎后用水稀释,加氯化铜溶液和抗坏血酸,用水定容,过0.45 μm滤膜后立即供液相色谱分析,在254 nm波长处测定。色谱柱：Hypersil ODS(125 mm×4 mm i.d., 5 μm);流动相：水-甲醇（体积比为80∶20）,含有20 mmol/L四丁基溴化铵,0.03 mol/L 醋酸钠缓冲液（pH 4） ,流速：0.8 mL/min;进样量：20 μL。EDTA在10 mg/L～400 mg/L范围内呈线性。方法回收率为95.5%～98.9%,其RSD为0.82%～1.32%。     

火锅底料中罂粟壳的高效液相色谱法测定

采用高效液相色谱法,以C18柱为分析柱,V（甲醇）：V（25mmol／LKH2PO4）＝90：10为流动相,检测波长254mm,分析了火锅底料中的罂粟壳。同时以空白火锅底料及空白底料添加罂粟壳做阴性及阳性对照。实验证实该方法灵敏、准确、可靠。