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1.
李霞  温志渝  温中泉 《色谱》2004,22(5):469-471
目前电泳芯片大多数采用的是光学检测的方法,这为电泳芯片的微型化、一体化集成带来了一定的难度。为此,设计了一种新的电泳芯片高频无接触电导检测器,并对这种新型的检测器进行了理论研究和分析,建立了高频电导检测器等效电路模型,对高频电导检测器的结构进行了设计;综合考虑区带展宽等因素,确定了检测器的结构尺寸。该检测器具有应用范围广、结构简单、易于一体化集成的特点。  相似文献   

2.
毛细管电泳-荧光/非接触电导组合型检测器的研制   总被引:3,自引:0,他引:3  
杨丙成  谭峰  关亚风 《分析化学》2005,33(5):740-742
报道了一种毛细管电泳-荧光/非接触电导组合型检测器。该检测器共用非接触电导检测池,实现了双检测器响应同步。优化了非接触电导检测系统中激发电压信号及其频率;荧光检测是用发光二极管作为激发光源,用光纤收集并传输荧光信号至光电倍增管。用无机金属离子和异硫氰酸荧光素评价该体系,结果表明,该检测器达到了任一单类型检测器性能指标。  相似文献   

3.
毛细管电泳法快速测定琥乙红霉素的含量   总被引:2,自引:0,他引:2  
建立了毛细管电泳高频电导法测定琥乙红霉素的方法。探讨了缓冲溶液、有机溶剂添加剂以及分离电压和进样条件等因素对分离检测的影响。在电泳介质为2.0mmol/L柠檬酸-20.0?H5OH,分离电压20.0kV的优化条件下,在7min内即可实现琥乙红霉素的分离检测,线性范围为3.0μg/mL-150.0μg/mL,检出限为1.0μg/mL。方法简便、快速,可检测制剂中琥乙红霉素的含量。  相似文献   

4.
谭峰  关亚风 《色谱》2005,23(2):152-157
介绍了电容耦合非接触电导检测(C4D)的检测原理及其最新的研究进展,引用文献50篇。C4D是近几年发展起来的一种用于毛细管电泳和微流控芯片电泳的新检测技术。C4D检测器的原理清楚,结构简单,易于微型化、集成化,不污染检测电极,因而很有应用价值。  相似文献   

5.
    
An axial design of a capacitively coupled contactless conductivity detector was tested in combination with fused‐silica capillaries with internal diameters of 10, 15, and 25 μm, which are used for high‐efficiency electrophoretic separation. The transmission of the signal in the detection probe dependent on the specific conductivity of the solution in the capillary in the range 0–278 mS.m−1 has a complex character and a minimum appears on the curve at very low conductivities. The position of the minimum of the calibration dependence gradually shifts with decreasing frequency of the exciting signal from 1.0 to 0.25 MHz toward lower specific conductivity values. The presence of a minimum on the calibration curves is a natural property of the axial design of contactless conductivity detector, demonstrated by solution of the equivalent electrical circuit of the detection probe, and is specifically caused by the use of shielding foil. The behavior of contactless conductivity detector in the vicinity of the minimum was documented for practical separations of amino acids in solutions of 3.2 M acetic acid with addition of 0–50% v/v methanol.  相似文献   

6.
毛细管电泳高频电导法测定虫草中的有效成份   总被引:1,自引:0,他引:1  
建立了毛细管电泳高频电导法同时测定腺苷和虫草素的方法。实验对电泳介质的种类、浓度以及操作电压和进样时间等因素进行了优化,在4mmol/L乳酸+10%异丙醇+80μg/mL羟甲基纤维素钠(pH=4.0),分离电压20.OkV的条下测定了天然虫草和人工虫草菌丝制品中的腺苷和虫草素的含量,线性范围分别为2.0μg/mL~120μg/mL和3.0μg/mL~110μg/mL,检出限分别为0.5μg/mL和1.0μg/mL。  相似文献   

7.
A study on the separation of lipophilic quaternary ammonium cations in NACE coupled with contactless conductivity detection (NACE‐C4D) is presented. The suitability of different salts dissolved in various organic solvents as running electrolytes in NACE‐C4D was investigated. A solvent mixture of methanol/acetonitrile at a ratio of 90%:10% v/v showed the best results. Deoxycholic acid sodium salt as BGE was found to provide exceptional high stability with low baseline noise that leads to highest S/N ratios for the target analytes among all BGEs tested. Under the optimum conditions, capillaries with different internal diameters were examined and an id of 50 μm was found to give best detection sensitivity. The proposed method was validated and showed good linearity in the range from 2.5 to 200 μM, low limits of detection (0.1–0.7 μM) and acceptable reproducibility of peak area (intraday RSD 0.1–0.7%, n = 3; interday RSD 5.9–9.4%, n = 3).  相似文献   

8.
毛细管电泳高频电导法同时测定阿莫西林和克拉维酸钾含量;毛细管电泳; 高频电导检测; 非接触式电导检测; 阿莫西林; 克拉维酸  相似文献   

9.
    
Saccharides form one of the major constituents of biological macromolecules in living organisms. Many biological processes including protein folding, stability, immune response and receptor activation are regulated by glycosylation. In this work, we optimized a capillary electrophoresis method with capacitively coupled contactless conductivity detection for the separation of eight monosaccharides commonly found in glycoproteins, namely D-glucose, D-galactose, D-mannose, N-acetyl-D-glucosamine, N-acetyl-D-galactosamine, D-fucose, N-acetylneuraminic acid, and D-xylose. A highly alkaline solution of 50 mM sodium hydroxide, 22.5 mM disodium phosphate, and 0.2 mM CTAB (pH 12.4) was used as a background electrolyte in a 10 µm id capillary. To achieve baseline separation of all analytes, a counter-directional pressure of –270 kPa was applied during the separation. The limits of detection of our method were below 7 µg/ml (i.e., 1.5 pg or 1 mg/g protein) and the limits of quantification were below 22 µg/ml (i.e., 5 pg or 3 mg/g protein). As a proof of concept of our methodology, we performed an analysis of monosaccharides released from fetuin glycoprotein by acid hydrolysis. The results show that, when combined with an appropriate pre-concentration technique, the developed method can be used as a monosaccharide profiling tool in glycoproteomics and complement the routinely used LC-MS/MS analysis.  相似文献   

10.
Law WS  Kubán P  Zhao JH  Li SF  Hauser PC 《Electrophoresis》2005,26(24):4648-4655
The separation and detection of commonly used preservatives (benzoate, sorbate) and vitamin C by both conventional CE and microchip electrophoresis with capacitively coupled contactless conductivity detection is presented. The separation was optimized by adjusting the pH-value of the buffer and the use of hydroxypropyl-beta-CD (HP-beta-CD) and CTAB as additives. For conventional CE, optimal separation conditions were achieved in a histidine/tartrate buffer at pH 6.5, containing 0.025% HP-beta-CD and 0.1 mM CTAB. LOD ranged from 0.5 to 3 mg/L (S/N = 3) and the RSDs for migration time and peak area were less than 0.1 and 2%, respectively. A considerable reduction of analysis time can be accomplished by using microchip electrophoresis without significant loss in sensitivity under optimal separation conditions. A histidine/tartrate buffer at pH 6.5, incorporating 0.06% HP-beta-CD and 0.25 mM CTAB, gave detection limits ranging between 3 and 10 mg/L and satisfactory reproducibilities of < or =0.4% for the migration time and < or =3.5% for the peak area. The methods developed are useful for the quantitative determination of food additives in real samples such as soft drinks and vitamin C tablets.  相似文献   

11.
毛细管电泳;高频电导检测;非接触式电导检测;硝酸咪康唑;复方制剂  相似文献   

12.
    
A method of capillary electrophoresis with contactless conductivity detection has been developed for non‐enantioselective monitoring the anaesthetic ketamine and its main metabolite norketamine. The separation is performed in a 15 μm capillary with an overall length of 31.5 cm and length to detector of 18 cm; inner surface of the capillary is covered with a commercial coating solution to reduce the electroosmotic flow. In an optimised background electrolyte with composition 2 M acetic acid + 1% v/v coating solution under application of a high voltage of 30 kV, the migration time is 97.1 s for ketamine and 95.8 s for norketamine, with an electrophoretic resolution of 1.2. The attained detection limit was 83 ng/mL (0.3 μmol/L) for ketamine and 75 ng/mL (0.3 μmol/L) for norketamine; the number of theoretic plates for separation of an equimolar model mixture with a concentration of 2 μg/mL was 683 500 plates/m for ketamine and 695 400 plates/m for norketamine. Laboratory preparation of rat blood plasma is based on mixing 10 μL of plasma with 30 μL of acidified acetonitrile, followed by centrifugation. A pharmacokinetic study demonstrated an exponential decrease in the plasma concentration of ketamine after intravenous application and much slower kinetics for intraperitoneal application.  相似文献   

13.
报道了一种芯片毛细管电泳-非接触电导法,用于快速测定葡萄糖氯化钠注射液中两种药物的含量。实验考察了运行缓冲液pH值和分离电压对组分分离的影响,以及检测器激励频率对组分信号响应和灵敏度的影响。确定以20mmol/L硼酸缓冲液(pH9.6)为分离介质,分离电压为1200V;最佳激励频率为70kHz。在上述条件下,两种成分(葡萄糖和Na+)可在60s内实现有效分离。Na+和葡萄糖的线性响应范围分别为20~1000μmol/L和50~5000μmol/L(r≥0.992);按信噪比(S/N)为3∶1计算检出限分别为8.2μmol/L和26.7μmol/L。两个组分的回收率分别为95%~99%和97%~104%,相对标准偏差(RSDs)均小于4.0%。该文首次报道了葡萄糖和氯化钠两种常见药物成分的同时测定。方法简便、快速、准确度高、稳定性好,用于注射剂含量的测定,结果满意。  相似文献   

14.
综述了毛细管电泳(CE)及芯片毛细管电泳(MCE)的电容耦合非接触电导检测(Capacitively Coupled Contactless Conductivity detection,C4D)的研究状况;并分别对其装置、检测的影响因素及其应用进行了评述。引用文献81篇。  相似文献   

15.
体液中卡托普利的乙醚提取毛细管电泳法测定;毛细管电泳;高频电导检测;非接触式电导检测;卡托普利;体液  相似文献   

16.
盐酸二甲双胍的毛细管电泳法快速测定   总被引:2,自引:0,他引:2  
建立了毛细管电泳高频电导法快速测定片剂中盐酸二甲双胍的方法。考察了缓冲溶液、有机溶剂添加剂、毛细管长度以及分离电压和进样条件等因素对分离检测的影响。在最佳条件下5.0 min内即可实现盐酸二甲双胍分离检测,盐酸二甲双胍的线性范围为1.50μg/mL~130μg/mL,检出限为1.0μg/mL。该方法成功地测定了盐酸二甲双胍片剂中的盐酸二甲双胍。  相似文献   

17.
    
Capillary electrophoresis (CE) systems have undergone extensive development for spaceflight applications. A flight-compatible high voltage power supply and the necessary voltage isolation for other energized components can be large contributors to both the volume and mass of a CE system, especially if typical high voltage levels of 25–30 kV are used. Here, we took advantage of our custom CE hardware to perform a trade study for simultaneous optimization of capillary length, high voltage level, and separation time, without sacrificing method performance. A capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C4D) method recently developed by our group to target inorganic cations and amino acids relevant to astrobiology was used as a test case. The results indicate that a 50 cm long capillary with 15 kV applied voltage (half of that used in the original method) can be used to achieve measurement goals while minimizing instrument size.  相似文献   

18.
    
A capillary electrophoresis with capacitively coupled contactless conductivity detection based method for the assay of azithromycin, clarithromycin and clindamycin was optimized and validated in this study. A buffer solution of 20 mM 2‐(N‐morpholino) ethane sulfonic acid, 40 mM l ‐histidine and 0.6 mM cetyltrimethylammonium bromide (pH 6.39) was used for the electrophoresis. An uncoated, bare‐fused silica capillary (total length 60 cm, effective length 32 cm, 75 μm id) was used at 25°C. The sample was injected hydrodynamically at 0.5 psi for 5 s. The electrophoresis was conducted at 30 kV in reverse polarity for 6 min with 3 and 2 min of in‐between sodium hydroxide (0.1 M) and background electrolyte rinsing, respectively. Ammonium acetate was used as internal standard. This simple and robust method showed reasonable limit of detection and limit of quantitation for azithromycin (0.0125/0.03 mg/mL), clarithromycin (0.017/0.03 mg/mL), and clindamycin (0.038/0.06 mg/mL), with good selectivity, precision both intraday (relative standard deviation ≤ 1.0%) and interday (relative standard deviation < 3.7%), linearity (R 2 > 0.999) and recovery (99 – 101.7%). The method was successfully applied for the determination of azithromycin, clarithromycin and clindamycin in formulations.  相似文献   

19.
采用微芯片毛细管电泳非接触电导检测法快速测定了盐酸洛美沙星胶囊中盐酸洛美沙星的含量。探讨了缓冲液类型、浓度,添加剂种类、浓度及分离电压、进样时间等因素对分离检测的影响。实验采用5.0mmol/L HAc(pH=2.5)+5%乙醇为缓冲溶液,分离电压3.0 kV,在1 min内实现了盐酸洛美沙星的快速分离测定。优化条件下盐酸洛美沙星的线性范围为20.0~250.0μg/mL,检出限为10.0μg/mL(S/N=3),RSD=2.0%,加标回收率为98.6%~103%。  相似文献   

20.
    
The search for chemical indicators of life is a fundamental component of potential future spaceflight missions to ocean worlds. Capillary electrophoresis (CE) is a useful separation method for the determination of the small organic molecules, such as amino acids and nucleobases, that could be used to help determine whether or not life is present in a sample collected during such missions. CE is under development for spaceflight applications using multiple detection systems, such as laser induced fluorescence (LIF) and mass spectrometry (MS). Here we report CE-based methods for separation and detection of major polar metabolites in cells, such as amino acids, nucleobases/sides, and oxidized and reduced glutathione using detectors that are less expensive alternatives to LIF and MS. Direct UV detection, indirect UV detection, and capacitvely coupled contactless conductivity detection (C4D) were tested with CE, and a combination of direct UV and C4D allowed the detection of the widest variety of metabolites. The optimized method was used to profile metabolites found in samples of Escherichia coli and Pseudoalteromonas haloplanktis and showed distinct differences between the species.  相似文献   

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