Coupling of capillary electrophoresis (CE) with mass spectrometry (MS) represents a powerful combination for performing rapid, efficient, and sensitive analysis of a variety of compounds. Here we describe a construction, operation, and application of a microfabricated liquid junction CE-MS interface. The interface is designed as a microfabricated unit with an integrated liquid junction and electrospray tip made from polyimide, which is positioned in a plastic connection block securing the separation CE capillary and attachable to the CE instrument. The application was demonstrated by CE-MS analysis of dextran oligomers labeled by (2-aminoethyl)trimethylammonium (AETMA) salt.

• Klíčová slova
• CE-MS interface, Capillary electrophoresis, Liquid junction, Mass spectrometry,
• MeSH
• elektroforéza kapilární * metody   MeSH
• hmotnostní spektrometrie s elektrosprejovou ionizací * MeSH
• hmotnostní spektrometrie metody   MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH

A miniaturized electrospray interface consisting of a microfluidic nanosprayer and nanospray module is reported in the presented short communication. The nanosprayer was fabricated using silicon (Si) technology suitable for cost-efficient high-volume mass production. The nanospray module enabled the positioning of the nanosprayer in front of a mass spectrometry entrance and its coupling with capillary electrophoresis based on the liquid junction principle. A case study of top-down and bottom-up proteomic analyses of intact cytochrome c and its tryptic digest demonstrates the practical applicability of the developed interface.

• Klíčová slova
• capillary electrophoresis, electrospray ionization, mass spectrometry, microfabrication, proteomics,
• MeSH
• cytochromy c * analýza   chemie   MeSH
• design vybavení MeSH
• elektroforéza kapilární * metody   přístrojové vybavení   MeSH
• hmotnostní spektrometrie s elektrosprejovou ionizací * metody   přístrojové vybavení   MeSH
• miniaturizace * přístrojové vybavení   MeSH
• nanotechnologie * přístrojové vybavení   MeSH
• proteomika metody   MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• cytochromy c * MeSH

A pilot study using capillary electrophoresis with mass spectrometry for the analysis of nucleotides in human erythrocytes is presented. Erythrocytes were incubated with 5-amino-4-imidazolecarboxamide riboside in order to mimic situation in defect of purine metabolism--AICA-ribosiduria. Characteristic AICA-ribotides together with normal nucleotides were separated by capillary electrophoresis in acetate buffer (20 mmol/L, pH 4.4) and identified on line by mass spectrometry.

• MeSH
• aminoimidazolkarboxamid analogy a deriváty   chemie   farmakologie   MeSH
• elektroforéza kapilární přístrojové vybavení   metody   MeSH
• erytrocyty cytologie   metabolismus   MeSH
• hmotnostní spektrometrie metody   MeSH
• koncentrace vodíkových iontů MeSH
• lidé MeSH
• nukleotidy analýza   chemie   izolace a purifikace   MeSH
• puriny chemie   MeSH
• ribonukleosidy chemie   farmakologie   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• acadesine MeSH Prohlížeč
• aminoimidazolkarboxamid MeSH
• nukleotidy MeSH
• puriny MeSH
• ribonukleosidy MeSH

A new analytical method based on capillary zone electrophoresis-tandem mass spectrometry is proposed and validated for the identification and simultaneous quantification of nine aminoglycosides in honey samples. Detection using an ion trap mass analyzer operating in the multiple reaction monitoring mode was used. Different parameters were optimized in order to obtain an adequate separation combined with the highest sensitivity. In order to achieve high selectivity in the sample treatment, a commercially-available molecularly imprinted polymer has been used for the solid phase extraction of the analytes. Under optimum conditions, recoveries for fortified samples ranged from 88.2 to 99.8%, with relative standard deviations lower than 8%. The limits of detection ranged from 0.4 to 28.5 μg kg(-1). Furthermore, the decision limit and the detection capability were evaluated, ranging from 3.5 to 60.5 μg kg(-1) and from 6.0 to 103.1 μg kg(-1), respectively, demonstrating the sensitivity and applicability of this fast and simple method.

• Klíčová slova
• Aminoglycosides, Capillary zone electrophoresis, Honey, Molecularly imprinted polymers, Stacking, Tandem mass spectrometry,
• MeSH
• aminoglykosidy analýza   MeSH
• elektroforéza kapilární metody   MeSH
• extrakce na pevné fázi metody   MeSH
• limita detekce MeSH
• med analýza   MeSH
• molekulový imprinting * metody   MeSH
• polymery chemie   MeSH
• tandemová hmotnostní spektrometrie metody   MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• validační studie MeSH
• Názvy látek
• aminoglykosidy MeSH
• polymery MeSH

Alzheimer's disease is the most common cause of dementia, currently afflicting almost 40 million patients worldwide. According to the amyloid cascade hypothesis, the pathogenesis of the disease could be slowed down or even stopped by the inhibition of beta-secretase, making this aspartic acid protease a potentially important drug target site. Capillary electrophoresis is a promising technique for screening putative enzyme inhibitors due to highly effective separations, minuscule sample and other chemicals consumption, compatibility with a variety of detection techniques, and high throughput via automation. This chapter presents a method based on capillary electrophoresis coupled to mass spectrometry detection for kinetic and inhibition assays of the beta-secretase reaction with a decapeptide derived from an amyloid precursor protein.

• Klíčová slova
• Alzheimer’s disease, Beta-secretase, Capillary electrophoresis, Enzyme inhibition, Mass spectrometry, Screening,
• MeSH
• Alzheimerova nemoc farmakoterapie   metabolismus   MeSH
• amyloidový prekurzorový protein beta metabolismus   MeSH
• aspartátové endopeptidasy metabolismus   MeSH
• elektroforéza kapilární metody   MeSH
• hmotnostní spektrometrie metody   MeSH
• inhibitory enzymů farmakologie   MeSH
• inhibitory proteas farmakologie   MeSH
• kinetika MeSH
• lidé MeSH
• plošný screening metody   MeSH
• sekretasy antagonisté a inhibitory   MeSH
• Check Tag
• lidé MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• Názvy látek
• amyloidový prekurzorový protein beta MeSH
• aspartátové endopeptidasy MeSH
• inhibitory enzymů MeSH
• inhibitory proteas MeSH
• sekretasy MeSH

Clinical analyses always represent a challenge for the sensitivity and selectivity of the analytical techniques. Of the most critical are the techniques required for the quick determination of the disease state and application of the proper treatment in newborns. This short critical review overviews the present state of the art of the use of mass spectrometry and capillary electrophoresis for screening of metabolic disorders in newborns.

• MeSH
• elektroforéza kapilární metody   MeSH
• hmotnostní spektrometrie metody   MeSH
• lidé MeSH
• metabolické nemoci * MeSH
• novorozenec MeSH
• plošný screening * MeSH
• Check Tag
• lidé MeSH
• novorozenec MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• přehledy MeSH

The biology of hyaluronidase activity on age related turnover of the hyaluronic acid (HA) in skin dermis and epidermis has not been established. Elucidation of this phenomenon enables discovery of novel compounds for skin health. As a simple and green technique, capillary electrophoresis (CE) was used for the first time for the determination of the kinetic constants (Km, Vmax and IC50) of the enzymatic degradation of HA. Reaction products were identified using CE/high-resolution mass spectrometry (HRMS) after appropriate optimization. Best results in terms of signal sensitivity were obtained using 10 mM ammonium acetate (pH 9.0) BGE, a sheath liquid composed of methanol-water (80:20, v/v) with 0.02% (v/v) formic acid at 10 μL min-1 and an ESI voltage at -4 kV. Km and Vmax were determined (n = 3) using CE/UV at 200 nm as 0.24 ± 0.02 mg mL-1 and 150.4 ± 0.1 nM s-1, respectively. They were also successfully obtained by CE/HRMS (n = 3) with Km of 0.49 ± 0.02 mg mL-1 and Vmax of 155.7 ± 0.2 nM s-1. IC50 of a standard natural inhibitor, epigallocatechin gallate, was also determined by CE-UV/HRMS. Kinetic constant values obtained by CE compared well with literature which validated the developed CE-based assay. In addition, the activity of homemade tetrasaccharides of biotinylated chondroitin sulfate CS-A or CS-C (4- or 6- sulfated in a homogeneous or heterogeneous way) on the hydrolysis reaction of hyaluronidase was evaluated. Hyaluronidase was mostly dose-dependently inhibited by CS-A tetrasaccharides sulfated in a homogeneous way. Two trisaccharides from truncated linkage region of proteoglycans were also tested as inhibitors or activators. CE-based assay showed that even a small modification of one hydroxyl group changes the influence on hyaluronidase activity. CE-based assay can be used for the screening of natural and synthetic inhibitors of hyaluronidase activity for cosmetic and therapeutic applications.

• Klíčová slova
• Capillary electrophoresis, Chondroitin sulfate, Enzyme, High-resolution mass spectrometry, Hyaluronidase,
• MeSH
• elektroforéza kapilární * MeSH
• hmotnostní spektrometrie * MeSH
• hyaluronoglukosaminidasa chemie   MeSH
• kinetika MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• hyaluronoglukosaminidasa MeSH

This review focuses on the latest development of microseparation electromigration methods in capillaries and microfluidic devices with MS detection and identification. A wide selection of 183 relevant articles covers the literature published from June 2012 till May 2014 as a continuation of the review article on the same topic by Kleparnik [Electrophoresis 2013, 34, 70-86]. Special attention is paid to the new improvements in the theory of instrumentation and methodology of MS interfacing with capillary versions of zone electrophoresis, ITP, and IEF. Ionization methods in MS include ESI, MALDI, and ICP. Although the main attention is paid to the development of instrumentation and methodology, representative examples illustrate also applications in the proteomics, glycomics, metabolomics, biomarker research, forensics, pharmacology, food analysis, and single-cell analysis. The combinations of MS with capillary versions of electrochromatography and micellar electrokinetic chromatography are not included.

• Klíčová slova
• Capillary electrophoresis, Electrospray, Mass spectrometry, Microfluidic devices,
• MeSH
• analýza jednotlivých buněk přístrojové vybavení   metody   MeSH
• analýza potravin přístrojové vybavení   metody   MeSH
• design vybavení MeSH
• elektroforéza kapilární přístrojové vybavení   metody   MeSH
• hmotnostní spektrometrie přístrojové vybavení   metody   MeSH
• lidé MeSH
• metabolomika přístrojové vybavení   metody   MeSH
• mikrofluidní analytické techniky přístrojové vybavení   metody   MeSH
• polysacharidy analýza   MeSH
• proteiny analýza   MeSH
• zvířata MeSH
• Check Tag
• lidé MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• práce podpořená grantem MeSH
• přehledy MeSH
• Názvy látek
• polysacharidy MeSH
• proteiny MeSH

Capillary electrophoresis coupled online with mass detection is a modern tool for analyzing wide ranges of compounds in complex samples, including urine. Capillary electrophoresis with mass spectrometry allows the separation and identification of various analytes spanning from small ions to high molecular weight protein complexes. Similarly to the much more common liquid chromatography-mass spectrometry techniques, the capillary electrophoresis separation reduces the complexity of the mixture of analytes entering the mass spectrometer resulting in reduced ion suppression and a more straightforward interpretation of the mass spectrometry data. This review summarizes capillary electrophoresis with mass spectrometry studies published between the years 2017 and 2021, aiming at the determination of various compounds excreted in urine. The properties of the urine, including its diagnostical and analytical features and chemical composition, are also discussed including general protocols for the urine sample preparation. The mechanism of the electrophoretic separation and the instrumentation for capillary electrophoresis with mass spectrometry coupling is also included. This review shows the potential of the capillary electrophoresis with mass spectrometry technique for the analyses of different kinds of analytes in a complex biological matrix. The discussed applications are divided into two main groups (capillary electrophoresis with mass spectrometry for the determination of drugs and drugs of abuse in urine and capillary electrophoresis with mass spectrometry for the studies of urinary metabolome).

• Klíčová slova
• capillary electrophoresis, drugs, mass spectrometry, metabolome, urine analysis,
• MeSH
• elektroforéza kapilární metody   trendy   MeSH
• hmotnostní spektrometrie metody   trendy   MeSH
• léčivé přípravky moč   MeSH
• lidé MeSH
• metabolomika MeSH
• moč chemie   MeSH
• odhalování abúzu drog metody   MeSH
• zvířata MeSH
• Check Tag
• lidé MeSH
• zvířata MeSH
• Publikační typ
• časopisecké články MeSH
• přehledy MeSH
• Názvy látek
• léčivé přípravky MeSH

The newly developed interface-free capillary electrophoresis-nanospray/mass spectrometry system (CE-nESI/MS) was applied for rapid analysis of the cardioprotective drug dexrazoxane and its hydrolysed form ADR-925 in deproteinized blood plasma samples. The aim of this study was to test the simplest possible CE-nESI/MS instrumentation for analyses of real samples. This interface-free system, utilizing single piece of a narrow bore capillary as both the electrophoretic separation column and the nanospray emitter, was operated at a flow rate of 30nL/min. Excellent electrophoretic separation and sensitive nanospray ionization was achieved with the use of only one high voltage power supply. In addition, hydrophobic external coating was developed and tested for additional stability of the nanospray ionization. To our knowledge this is the first study devoted to the analysis of dexrazoxane and ADR-925 by capillary electrophoresis-mass spectrometry.

• Klíčová slova
• Capillary electrophoresis, Dexrazoxane, Hydrophobic coating, Interface, Mass spectrometry, Nanospray,
• MeSH
• biochemická analýza krve metody   MeSH
• dexrazoxan krev   MeSH
• elektroforéza kapilární * MeSH
• ethylendiaminy krev   MeSH
• glycin analogy a deriváty   krev   MeSH
• hmotnostní spektrometrie s elektrosprejovou ionizací * MeSH
• Publikační typ
• časopisecké články MeSH
• Názvy látek
• dexrazoxan MeSH
• ethylendiaminy MeSH
• glycin MeSH
• ICRF 198 MeSH Prohlížeč