Phosphate Background Electrolyte Research Articles

Competition between fulvic acid and phosphate-mediated surface properties and transport of titanium dioxide nanoparticles in sand porous media

Fulvic acid (FA) is a series of organic macromolecular compounds with many oxygen-containing functional groups and is easy to complex with nanoparticles (NPs) in the environment, thus affecting the stability and mobility of NPs in the water environment. Therefore, it is necessary to investigate the transport behavior of nano titanium dioxide (nTiO2) particles with FA in the presence of phosphate (P). A series of transport experiments were conducted by using nTiO2 suspended in phosphate background electrolyte with and without the addition of FA passing through water-saturated sand columns. The zeta potentials, hydrodynamic radii, and aggregation kinetics were measured, and the extended Derjaguin-Landau-Verwey-Overbeek (DLVO) theory and two-site kinetic attachment model (TSKAM) were employed to explain the underlying mechanism. The experimental results showed that the presence of FA compressed the transport of nTiO2 in phosphate electrolyte due to formation of larger complex via the adsorption of organic FA molecules onto nTiO2, which can strongly compete with phosphate adsorption, leading to reduced electrostatic repulsive forces between nTiO2 and sand. In the absence of FA at low pH (6.0), transport of individual nTiO2 was increased by low phosphate adsorption in response to increased phosphate levels, and then, transport was decreased with the increased number of cations (Na+) from the phosphate (P ≥ 1.0 mM) electrolyte due to the compressed electric double layer. From the goodness-of-fit of the modeling results, the TSKAM provided a good prediction for the retention and transport of nTiO2 in the copresence of FA and phosphate. The compressed transport of nTiO2 in the copresence of FA and phosphate was distinct from the synergistic transport in the copresence of humic acid.

Development of a generic method for the determination of proton-pump inhibitors by capillary zoneelectrophoresis

A generic capillary zone electrophoresis method was developed for the analysis of four proton pump inhibitors: omeprazole, pantoprazole, lansoprazole and rabeprazole. During preliminary analysis screening of phosphate buffers at different pH levels was performed, in order to determine the optimum pH domain suitable for the simultaneous determination of all studied compounds. A face centered central composite design was employed for the optimization of separation conditions. The effect of buffer concentration, pH and applied voltage was studied; resolution between peaks and migration time of the last compound were considered as responses. Other factors as system temperature, injection parameters, capillary length, were held constant during the optimization process. The optimized conditions consisted of 40mM phosphate background electrolyte at pH 5.0, +25 kV applied voltage and 20 °C temperature. The migration order of the analytes was as follows: rabeprazole, omeprazole, lansoprazole and pantoprazole. Full resolution of all analytes was achieved within 9 minutes. The method was validated and proved to be suitable in terms of repeatability, sensitivity, linearity, accuracy and robustness. Determinations from commercially available pharmaceutical formulation were performed for omeprazole; good reproducibility and recovery were obtained.

Separation of hydroxynorketamine stereoisomers using capillary electrophoresis with sulfated β‐cyclodextrin and highly sulfated γ‐cyclodextrin

The racemic N-methyl-d-aspartate receptor antagonist ketamine is used in anesthesia, analgesia and the treatment of depressive disorders. It is known that interactions of hydroxylated norketamine metabolites and 5,6-dehydronorketamine (DHNK) with the α7 -nicotinic acetylcholine receptor and the α-amino-3-hydroxy-5-methyl-4-isoxazolepropionic acid receptor are responsible for the antidepressive effects. Ketamine and its first metabolite norketamine are not active on these receptors. As stereoselectivity plays a role in ketamine metabolism, a cationic capillary electrophoresis based method capable of resolving and analyzing the stereoisomers of four hydroxylated norketamine metabolites, norketamine and DHNK was developed. The assay is based on liquid/liquid extraction of the analytes from the biological matrix, electrokinetic sample injection across a buffer plug and analysis of the stereoisomers in a phosphate background electrolyte (BGE) at pH 3 comprising a mixture of sulfated β-cyclodextrin (5 mg/mL) and highly sulfated γ-cyclodextrin (0.1%). The method was used to analyze samples of an in vitro study in which ketamine was incubated with equine liver microsomes and in plasma samples of dogs and horses that were collected after an i.v. bolus injection of racemic ketamine.

Chiral separation of benzothiazole derivatives of amino acids using capillary zone electrophoresis.

A method for the separation of enantiomers of leucine and phenylalanine benzothiazole derivatives as potential antimicrobial agents was developed using capillary zone electrophoresis with a dual cyclodextrin (CD) system. The best resolution of enantiomers was achieved in 100 mmol/L phosphate background electrolyte (pH 3.5) with the dual CD system consisting of 10mmol/L of β-CD with 10 mmol/L of 2-hydroxypropyl-β-cyclodextrin for leucine derivative and 10 mmol/L of 2-hydroxypropyl-γ-cyclodextrin for phenylalanine derivative, respectively. Under the optimal conditions, the highest enantioresolution of 1.25 was achieved in a noncoated-fused silica capillary at 17°C and 24 kV applied voltage.

Simultaneous Chiral Separation of Four H1-Antihistamines by Capillary Zone Electrophoresis Using a Dual Cyclodextrin System

Capillary zone electrophoresis employing a dual cyclodextrin (CD) system, consisting of anionic sulfobutylether-β-CD and native β-CD, was developed for the simultaneous chiral separation of four H1-antihistamine racemates (brompheniramine, chlorpheniramine, cetirizine and promethazine). A cost-effective screening using different native and derivatized, neutral and ionized CDs as chiral selectors was performed to find suitable derivatives for the dual CD system. Under the optimized conditions consisting of 25 mM phosphate background electrolyte at pH 7.0, a combination of 15 mM SBE-β-CD and 10 mM β-CD as chiral selectors, +25 kV applied voltage and 20 °C system temperature, the baseline chiral separation of all racemates was accomplished in less than 8 min. The method proved to be suitable for routine analysis, since it provided satisfactory results during sensitivity, linearity and repeatability studies.

CHARACTERIZING EFFECTS OF CATIONIC SURFACTANT ON ELECTRO-OSMOTIC MOBILITY AND ANION MIGRATION IN CAPILLARY ELECTROPHORESIS

The analysis of anions by capillary electrophoresis (CE) with bare silica capillary often uses cationic surfactant to modify the electro-osmotic mobility (EOM) to ensure anions migrating to anode and being detected. The effect of cetyltrimethylammonium bromide (CTAB) concentration in phosphate background electrolyte (BGE) with various ionic strength and pH on the migration of analytes was investigated and reported. A concentration of 0.08 mM CTAB in the BGE starts to reverse cathodic EOM into anodic EOM, and a concentration of 0.30 mM CTAB in the BGE maximizes anodic EOM. Lower EOM is obtained in BGE of higher phosphate concentration while the CTAB concentration and pH are kept constant. Under conditions of constant CTAB and phosphate concentration, higher cathodic EOM was obtained in the BGE of higher pH and lower anodic EOM was obtained in the BGE of higher pH. Although the effect of CTAB concentration, pH, and phosphate concentration on the migration of aromatic anions is complex, the result indicates that the most rapid and effective separation for the anions can be achieved by using a BGE with 0.20 mM CTAB. Furthermore, the relationship between the electrophoretic mobility of anions and the CTAB concentration can be used to determine the critical micelle concentration of cationic surfactant.

Capillary electrophoresis study of iron(II) and iron(III) polyaminocarboxylate complex speciation

Environmental contextMethods for determining iron species are integral to investigations of iron cycling processes in the environment. Capillary electrophoresis is an effective tool for determining the concentrations of various iron species in solution, but the separations are highly dependent on the electrolyte composition. This study reports the use of capillary electrophoresis to separate and quantify distinct FeII and FeIII complexes with polyaminocarboxylates. AbstractThe purpose of this study was to use capillary electrophoresis to (i) separate and quantify distinct FeII and FeIII complexes with polyaminocarboxylates and (ii) develop new methods for distinguishing between FeII and FeIII in aqueous media. A 25 mM phosphate and a 50 mM 3-(N-morpholino)propanesulfonic acid (MOPS) background electrolyte (BGE), both buffered at pH 7.1, were each tested with 6 polyaminocarboxylate complexes with FeII and FeIII. Adequate separation of all FeIII-chelating agent complexes was observed with the MOPS BGE. With the phosphate BGE, sharp peaks were obtained for FeIII complexes with EDTA, HEDTA, DTPA and CDTA, however FeIII–EGTA showed excessive peak broadening, and FeIII–TMDTA showed no discernable peak. Mobilities of FeIII–EGTA, FeIII–EDTA and FeIII–HEDTA were much larger when the phosphate BGE was employed, providing evidence for ternary complex formation with phosphate during electromigration. For FeII, complexes with TMDTA and EGTA were adequately separated with either BGE, but separations of the other chelating agents resulted in their corresponding FeIII complexes due to rapid oxidation by molecular oxygen. These chelating agents may be used as preservatives and derivatising agents for the analysis of ferrous and ferric iron in environmental samples.

Analysis of Non-Aromatic Organic Acids in Beer by CE and Direct Detection Mode with Diode Array Detection

A method for the analysis of the main non-aromatic organic acids in beer using capillary electrophoresis is presented. In this work, malic, citric, succinic, pyruvic, acetic and lactic acids are separated using a sodium hydrogen phosphate background electrolyte with direct detection mode with a diode array detector. The separation exhibits lower sensitivity than equivalent methods with indirect detection mode, however, the risk of co-migration with unknown compounds in beer matrixes is significantly reduced. This is due to (i) a higher efficiency (250,000–400,000 theoretical plates), (ii) a higher selectivity than any equivalent method using an indirect detection mode, and (iii) the possibility to monitor other wavelengths in parallel (260 nm for example) to check for possible co-migration with phenolic or benzoic acids. This was critical when working with beer samples as an unknown compound absorbing at 200 and 260 nm was detected in the neighbourhood of malic, citric and succinic acids. Such co-migration will not have been detected using single wavelength detection below 200 nm or indirect detection mode.

The Quantitative Structure–Retention Relationship (QSRR) Analysis of Some Centrally Acting Antihypertensives and Diuretics

AbstractThe complete separation of 15 guanidine/imidazoline derivatives, acting as antihypertensive drugs, was achieved by capillary electrophoresis employing 30 mM phosphate background electrolyte (pH 1.5) containing 15 mM β‐Cyclodextrin (BCD). Here the Quantitative Structure–Retention Relationship (QSRR) models of the inclusion complexes between the analyzed compounds (ligands) and BCD were performed to investigate the correlations between electrophoresis migration order and the constitutional, geometrical, physico‐chemical, and electronical properties of the molecular models. The ChemPro, Marvin 4.0.5 ChemAxon, and CS Gaussian 98 [B3LYP/6–31G+(d,p) and HF/3–21G(d) basis sets] programs were applied for molecular parameters computation of the optimized ligands and ligand–BCD complexes. Total charge of the analyzed compounds at experimental pH 1.5, HOMO (BCD–ligand) energy, and Solvent‐Accessible Surface (SAS) (BCD–ligand) area account for the electrophoresis retention parameter log(t). The multiple linear regression models with three variables, log(t)=f [Total Charge (ligand), SAS (BCD–ligand), HOMO (BCD–ligand)], were obtained with R2=0.914 and crossvalidation parameter of prediction $\rm{ q_{{\rm{pre}}}^{\rm{2}} }$=0.778. The developed QSRR approach can help in understanding the structural features that contribute to the electrophoresis retention parameter [log(t)] of the investigated antihypertensives. Therefore, the theoretical method presented could be used as a fast, easy, and reliable tool for electrophoretic migration parameters prediction of other related antihypertensives.

Characterization of anacardic acids by micellar electrokinetic chromatography and mass spectrometry

A possibility of using capillary electrophoresis for separation of anacardic acids (6-alkylsalicylic acids) has been studied. Conventional micellar electrokinetic chromatography (MEKC) in non-coated fused silica capillaries and reversed-flow micellar electrokinetic chromatography (RF-MEKC) in capillaries coated with polydimethylacrylamide was applied for separation of anacardic acids extracted from cashew nuts. Influence of the composition of background electrolyte on the resolution of anacardic acid isomers was evaluated. Separations were performed using sodium dodecyl sulphate (SDS) micelles and mixed micelles of SDS and polyoxyethylene lauryl ether as a pseudostationary phase. To further improve the separation in RF-MEKC, β-cyclodextrin and a dual cyclodextrin system of β-cyclodextrin with heptakis-6-sulphato-β-cyclodextrin was added to the working electrolyte. Best separation of anacardic acids were achieved in the polydimethylacrylamide-coated capillary using 10 mM phosphate background electrolyte pH 6.5 with addition of 1 M urea, 20% acetonitrile, 10 mM of β-cyclodextrin and 1 mM of heptakis-6-sulfo-β-cyclodextrin. Mass spectrometry was used for the identification of anacardic acids in the extract from cashew nuts in single and tandem mode using Q-TOF instrument. Nine anacardic acids were identified in the extract form the cashew nuts.

Enantioseparations of hydrobenzoin and structurally related compounds in capillary zone electrophoresis using heptakis(2,3-dihydroxy-6-O-sulfo)-beta-cyclodextrin as chiral selector and enantiomer migration reversal of hydrobenzoin with a dual cyclodextrin system in the presence of borate complexation.

We investigated the enantioseparations of racemic hydrobenzoin, together with benzoin and benzoin methyl ether, in capillary electrophoresis (CE) using the single-isomer heptakis(2,3-dihydroxy-6-O-sulfo)-beta-cyclodextrin (SI-S-beta-CD) as a chiral selector in the presence and absence of borate complexation and enantiomer migration reversal of hydrobenzoin with a dual CD system consisting of SI-S-beta-CD and beta-CD in the presence of borate complexation at pH 9.0 in a borate buffer. The enantioselectivity of hydrobenzoin increased remarkably with increasing SI-S-beta-CD concentration and the enantioseparation depended on CD complexation between hydrobenzoin-borate and SI-S-beta-CD. The (S,S)-enantiomer of hydrobenzoin-borate complexes interacted more strongly than the (R,R)-enantiomer with SI-S-beta-CD. The enantiomers of hydrobenzoin could be baseline-resolved in the presence of SI-S-beta-CD at a concentration as low as 0.1% w/v, whereas the three test analytes were simultaneously enantioseparated with addition of 0.3% w/v SI-S-beta-CD or at concentrations >2.0% w/v in a borate buffer and 0.5% w/v in a phosphate background electrolyte at pH 9.0. Compared with the results obtained previously using randomly sulfated beta-CD (MI-S-beta-CD) in a borate buffer, enantioseparation of these three benzoin compounds is more advantageously aided by SI-S-beta-CD as the chiral selector. The enantioselectivity of hydrobenzoin depended greatly on the degree of substitution of sulfated beta-CD. Moreover, binding constants of the enantiomers of benzoin compounds to SI-S-beta-CD and those of hydrobenzoin-borate complexes to SI-S-beta-CD were evaluated for a better understanding of the role of CD complexation in the enantioseparation and chiral recognition. Enantiomer migration reversal of hydrobenzoin could be observed by varying the concentration of beta-CD, while keeping SI-S-beta-CD at a relatively low concentration. SI-S-beta-CD and beta-CD showed the same chiral recognition pattern but they exhibited opposite effects on the mobility of the enantiomers.

Enantioseparation of benzoins and enantiomer migration reversal of hydrobenzoin in capillary zone electrophoresis with dual cyclodextrin systems and borate complexation

Enantioseparations of racemic hydrobenzoin and structurally related compounds, including benzoin and benzoin methyl ether, in capillary zone electrophoresis (CZE) with dual cyclodextrin (CD) systems consisting of S-β-CD (mixed isomers) and a neutral CD, including β-CD and hydroxypropyl-β-CD (HP-β-CD), as chiral selectors in the presence of borate complexation at pH 9.0 were investigated. Effective enantioseparations of hydrobenzoin were achieved with addition of dual CD systems and also with neutral CDs in a borate buffer. The enantioseparation and migration behavior of hydrobenzoin in such an electrophoretic system are primarily governed by the interaction of the borate complex of hydrobenzoin with β-CDs. The CD complexations of both hydrobenzoin and the borate complexes of hydrobenzoin with β-CDs increase in the order S-β-CD<HP-β-CD<β-CD. As a result, enantioseparations of hydrobenzoin with the use of dual CD systems consisting of S-β-CD/β-CD and S-β-CD/HP-β-CD as chiral selectors are more advantageous than that with the use of S-β-CD alone. With these dual CD systems in the presence of borate complexation, the enantiomer migration reversal was observed for hydrobenzoin. The interactions of hydrobenzoin with neutral CDs and with S-β-CD exhibit the same chiral recognition pattern, but opposite effect on the mobility of the enantiomers. The ( S, S)-enantiomer of hydrobenzoin was found to interact more strongly than the ( R, R)-enantiomer with neutral CDs. For comparison, enantioseparation of hydrobenzoin, together with benzoin and benzoin methyl ether, with dual CD systems in a phosphate background electrolyte at pH 9.0 was also examined. The migration order and enantioselectivity of these three benzoins depend on the degree of CD complexations between benzoins and both S-β-CD and neutral CD in a phosphate background electrolyte. In addition, effective enantioseparations of hydrobenzoin were also achievable with addition of either β-CD at concentrations greater than 1.0 mM or HP-β-CD at concentrations exceeding 2.0 mM in a borate buffer at pH 9.0.

Experimental Design Optimization of a Capillary Zone Electrophoresis Method for the Screening of Several Diuretics and ACE Inhibitors

Experimental design methodologies are applied to the development of a capillary zone electrophoretic method for the separation of the angiotensin-converting enzyme inhibitor enalapril and its derivative enalaprilat and the diuretics xipamide and hydrochlorothiazide. The effects of pH, buffer concentration, proportion of boric acid in the mixed boric acid-potassium dihydrogen phosphate background electrolyte, temperature, applied voltage, and percentage of organic modifier are studied. Critical factors are identified in a screening design (a 2(6-2) fractional factorial design), and afterwards, optimal conditions for the separation are reached by means of an optimization design (a 2(2) + 2 x 2 + k central composite design). The studied response is the resolution between peaks. The four studied compounds can be separated in less than 3.5 min using an electrolyte of 20mM boric acid-potassium dihydrogen phosphate (75:25, v/v) with 5% MeOH adjusted to pH 8.0 with KOH, at a potential of 30 kV. The detection wavelength and temperature are 206 nm and 35 degrees C, respectively.

Comparative studies on the enantioseparation of hydrobenzoin and structurally related compounds by capillary zone electrophoresis with sulfated β-cyclodextrin as the chiral selector in the presence and absence of borate complexation

Comparative studies on the enantioseparations of racemic hydrobenzoin, together with benzoin and benzoin methyl ether, in capillary zone electrophoresis using sulfated β-cyclodextrin (S-β-CD) as a chiral selector in the presence and absence of borate complexation were investigated. The influences of S-β-CD concentration on the enantioseparation of benzoins in a borate buffer and a phosphate background electrolyte and the influences of the concentration and the pH of borate buffer containing S-β-CD on the enantioseparation of hydrobenzoin were examined. The results indicate that, depending on the degree of strong borate complexation and comparatively weak CD complexation, the selectivity of the enantiomers of hydrobenzoin can be greatly reduced in a buffer system containing borate ions. Enantioseparation of hydrobenzoin is mainly governed by the interaction between hydrobenzoin–borate complexes and S-β-CD in a borate buffer, whereas enantioseparation of benzoins is primarily determined by CD complexation in a phosphate background electrolyte. Effective enantioseparations of benzoins were simultaneously achieved with addition of S-β-CD at a concentration greater than 3.0% (w/v) in a borate buffer and at a concentration greater than 2.5% (w/v) in a phosphate background electrolyte at pH 9.0.

Separation and migration behavior of structurally related phenothiazines in cyclodextrin-modified capillary zone electrophoresis.

The influences of buffer pH and the concentration of beta-cyclodextrins (beta-CDs) on the separation and migration behavior of 13 structurally related phenothiazines in CD-modified capillary zone electrophoresis (CD-CZE) using a phosphate background electrolyte at low pH were investigated. We focused on the separation of these phenothiazines, including the enantiomers of chiral analytes, with the use of beta-CD and hydroxypropyl-beta-CD (HP-beta-CD) as electrolyte modifiers or chiral selectors at concentrations less than 8 mM. The results indicate that the interactions of phenothiazines with beta-CDs are very strong and that effective separations of 13 analytes can be achieved with addition of 0.3 mM beta-CD or 0.5 mM HP-beta-CD in a phosphate buffer at pH 3.0. Binding constants of phenothiazines to beta-CDs were evaluated for a better understanding of the interactions of phenothiazines with beta-CDs.

The use of a highly sulfated cyclodextrin for the simultaneous chiral separation of amphetamine-type stimulants by capillary electrophoresis.

We investigated the simultaneous chiral separation of nine amphetamine type stimulants (dl-norephedrine, dl-norpseudoephedrine, dl-ephedrine, dl-pseudoephedrine, dl-amphetamine, dl-methamphetamine, dl-methylenedioxyamphetamine (MDA), dl-methylenedioxymethamphetamine (MDMA), and dl-methylenedioxyethylamphetamine (MDEA)) by capillary electrophoresis using highly sulfated gamma-cyclodextrin (SU(XIII)-gamma-CD) as a chiral selector. Three different approaches using SU(XIII)-gamma-CD with 50 mM phosphate background electrolyte were designed; (I) high CD concentration (10 mM SU(XIII)-gamma-CD) at neutral pH (pH 7.0) in the normal polarity mode, (II) low CD concentration (1.0 mM) at low pH (pH 2.6) in the normal polarity mode and (III) high CD concentration at low pH (pH 2.6) in the reversed-polarity mode. In mode (II), the effects of adding three neutral CDs (beta-CD, dimethyl-beta-CD and hydroxypropyl-beta-CD) were also investigated. The best separation was obtained after optimizing mode (III) as follows: run buffer of 10 mM SU(XIII)-gamma-CD with 50 mM phosphate background electrolyte at pH 2.6, applied voltage of -12 kV and capillary temperature of 15 degrees C.

Evaluation of the efficiency of extraction of ultraviolet-absorbing pollen allergens and organic pollutants from airborne dust samples by capillary electromigration methods

Capillary electromigration methods, zone electrophoresis (CZE) and micellar electrokinetic chromatography (MEKC), have been used for evaluation of the efficiency of different extraction agents applied to the extraction of pollen allergens and organic pollutants from dust samples collected during different periods (before, during and after pollen seasons) and in different locations in air-filtration devices (car-traffic tunnel in Prague and a metro station in Paris). Water and acetic acid extracts were analyzed by CZE using acetic acid as background electrolyte (BGE). Water and alkaline water–SDS–buffer extracts were analyzed by MEKC in Tris–phosphate BGE with anionic detergent sodium dodecylsulfate (SDS) micellar pseudophase. More material was extracted and more components were found in the water–buffer extracts than in the water extracts, and better resolution of the components was achieved by MEKC than by CZE. Significant differences have been found in the analyses of dust extracts of different origin. More material and more components have been found in the extracts of the dust collected in the pollen-rich period (March, April) than in the pollen-free period (December, January).

Separation of the high-ceiling diuretic Torasemide and its metabolites by capillary zone electrophoresis with diode-array detection.

A capillary zone electrophoretic method was developed for the separation of the high-ceiling loop diuretic Torasemide and three of its metabolites (M1, M3 and M5) using an experimental design approach. Two different experimental designs were employed to optimize the developed method: (i) a fractional factorial design examining six factors at two levels (2(6-2)) and (ii) a central composite design examining two factors at two levels (2(2)+2x2+p). The factors studied were: pH, buffer concentration, proportion of boric acid in the mixed boric acid:potassium dihydrogen phosphate background electrolyte, temperature, applied voltage and percentage of organic modifier. Resolution between peaks was established as response. Separation of the four studied compounds was achieved in less than 8 min, using an electrolyte of 20 mM boric acid:potassium dihydrogen phosphate (75:25 v/v) with 15% MeOH adjusted to pH 9.7 with KOH, at a potential of 28 kV. Detection wavelength and temperature were 206 nm and 35 degrees C, respectively.

Capillary electrophoresis studies of pectins

Capillary electrophoresis (CE) has been used to study a variety of pectins that originate from different sources (citrus, apple and beet) and have different anhydrogalacturonic acid (AGU) contents (86.2–63.2%). This CE method can be used for the quantitative detection of aqueous solutions of pectins in the concentration range 0.5–5 mg mL −1 using a 50 mM pH 7.0 phosphate background electrolyte and UV detection at 192 nm. Using lemon pectin calibration standards in the degree of esterification (DE) range 31.1–75.8%, the technique was used to determine the DE of a further 11 pectin samples. Results are shown to be in excellent agreement with those obtained by titration, irrespective of the pectin type and neutral sugar content. The method also allows determination of the intermolecular DE distribution (variation in DE between molecules), from the CE peak shape. Results for the DE distribution are compared with those obtained by ion-exchange chromatography in combination with size-exclusion chromatography (IEC-SEC). Both DE and DE distribution are obtained from CE in approximately 2 h, inclusive of sample preparation and calibration, in contrast to 2 days for the IEC-SEC method.

Separation and quantification of pectins using capillary electrophoresis: a preliminary study

A rapid method for the analysis of the degree of esterification (DE) of pectin is presented. The migration time of pectin in capillary electrophoresis (CE) is a function of the DE, and separation of pectins with different DE values has been demonstrated. Using the average charge per residue, z = −(100−DE) 100 , a linear relationship is found between pectin charge and mobility. For a fixed charge mobility increases with decreasing ionic strength, but does not depend significantly on whether the pectin charge distribution is blockwise or random. This CE method can be used for the quantitative detection of aqueous solutions of pectins in the concentration range 0.5–5 mg ml −1 using a 50 mM, pH 7.0 phosphate background electrolyte and u.v. detection at 192 nm.