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PubMed2003

Behavioral and adrenocortical responses to mate separation and reunion in the zebra finch.

The adaptive value of social affiliation has been well established. It is unclear, however, what endogenous mechanisms may mediate affiliative behavior. The Australian zebra finch (Taeniopygia guttata) breeds colonially and adults maintain lifelong pair bonds that may be disrupted in the wild due to high mortality rates. Many of its natural, social behaviors are maintained in laboratory conditions, making this species well suited for studying the mechanisms of affiliation. This study examines the behavioral and neuroendocrine responses to pair mate separation and reunion in zebra finches. We measured plasma corticosterone (CORT) and behavioral changes following separation from a pair bonded mate, and again upon reintroducing the mate or an opposite-sex cagemate. Plasma CORT concentrations were: (1). elevated during pair mate separation, even in the presence of other same-sex individuals, and (2). reduced to baseline upon reunion with the pair mate but not upon re-pairing with a new opposite-sex partner. These findings show that zebra finches exhibit hormonal responses to separation and reunion specifically with a bonded pair mate and not with other familiar conspecifics. In addition, alterations in behavior during separation and reunion are consistent with monogamous pair bond maintenance. This study presents evidence for adrenocortical involvement in avian pair bonding, and for hypothalamic-pituitary-adrenal activation in response to an ecologically relevant social stressor.

Acoustic Stimulation↗
PubMed2001

"In vivo" determination of hip joint separation and the forces generated due to impact loading conditions.

Numerous supporting structures assist in the retention of the femoral head within the acetabulum of the normal hip joint including the capsule, labrum, and ligament of the femoral head (LHF). During total hip arthroplasty (THA), the LHF is often disrupted or degenerative and is surgically removed. In addition, a portion of the remaining supporting structures is transected or resected to facilitate surgical exposure. The present study analyzes the effects of LHF absence and surgical dissection in THA patients. Twenty subjects (5 normal hip joints, 10 nonconstrained THA, and 5 constrained THA) were evaluated using fluoroscopy while performing active hip abduction. All THA subjects were considered clinically successful. Fluoroscopic videos of the normal hips were analyzed using digitization, while those with THA were assessed using a computerized interactive model-fitting technique. The distance between the femoral head and acetabulum was measured to determine if femoral head separation occurred. Error analysis revealed measurements to be accurate within 0.75mm. No separation was observed in normal hips or those subjects implanted with constrained THA, while all 10 (100%) with unconstrained THA demonstrated femoral head separation, averaging 3.3mm (range 1.9-5.2mm). This study has shown that separation of the prosthetic femoral head from the acetabular component can occur. The normal hip joint has surrounding capsuloligamentous structures and a ligament attaching the femoral head to the acetabulum. We hypothesize that these soft tissue supports create a passive, resistant force at the hip, preventing femoral head separation. The absence of these supporting structures after THA may allow increased hip joint forces, which may play a role in premature polyethylene wear or prosthetic loosening.

Biomechanical Phenomena↗
PubMed2000

Micellar electrokinetic capillary chromatographic separation and fluorescent detection of amino acids derivatized with 4-fluoro-7-nitro-2,1,3-benzoxadiazole.

Another method has been developed for the separation of amino acids (1 min derivatization plus 22 min separation) by micellar electrokinetic capillary chromatography (MECC) with laser-induced fluorescence detection. Interestingly enough, such work has never been performed on essential amino acids derivatized by 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F). Fifteen L-amino acid standards were labelled with NBD-F at 60 degrees C for 1 min, and separated in a buffer system containing 20 mM borate, 25 mM sodium cholate, 10 mM Brij 35 and 2.5% methanol. Methanol was employed to expand the MECC migration time window; whereas Brij 35 was used to improve the fluorescence intensity of amino acid derivatives. This method also indicates that bile salt is effective for MECC separation of ionic analytes. Surprising though, improvements in resolution, sensitivity and speed for amino acids analysis are obtained in this work, which are not initially apparent in just employing another derivatizing reagent. Under optimal conditions, 15 amino acids were separated in a short 22 min analysis time, the shortest ever reported, and detection limits of nanomolar concentration and attomole mass were obtained. Furthermore, RSDs of migration time and peak height are better than 1% and 1.8%, respectively, again the smallest ever reported in the literature.

4-Chloro-7-nitrobenzofurazan↗
PubMed2000

Recent developments in the separation of inorganic and small organic ions by capillary electrophoresis.

Which method should I use for ion analysis, ion chromatography (IC) or capillary electrophoresis (CE)? In terms of actual theoretical plates CE has a clear-cut advantage. The separation ability of IC is adequate for many sample types, and many separation scientists feel that IC offers greater reliability and confidence than CE. However, IC is a more mature technique and there has been more time to solve problems such as peak tailing and to improve reproducibility. The two techniques should be viewed as complementary. A number of recent developments in ion analysis by CE are discussed. These include some simple ways to control electroosmotic flow and improve reproducibility, separation of isotopes, improved methods of indirect photometric detection, a new contactless conductivity detector, separation of ions at low pH, and in solutions of high salt content. Progress in a new technique called IC-CE will be described in which a soluble ion-exchange polymer is added to the capillary electrolyte to separate anions based on differences in both electrophoretic mobility and ion-exchange interactions.

Electrophoresis, Capillary↗
PubMed2000

Novel way of separating polyfluorocarboxylic acids by ion-exclusion chromatography.

Ion-exclusion chromatography has been successfully applied to the separation of a number of polyfluorocarboxylic acids. The separation of various mono- and dibasic polyfluorocarboxylic acids having a different alkyl group was investigated using a polymethacrylate-based weakly acidic cation-exchange resin (TSK gel OApak-A) in the H -form and conductimetric detection. When water was used as the eluent, polyfluorocarboxylic acids could not be resolved. When an aqueous solution of sulfuric acid, benzoic acid, o-phthalic acid, 1,3,5-benzenetricarboxylic acid, 1,2,4,5-benzenetetracarboxylic acid, and tartaric acid was used, the separation of polyfluorocarboxylic acids occurred for monobasic ones. While, for fluorine-containing dibasic acids, imperfect separation of peaks occurred. In order to improve their separation, the effect of an addition of organic modifiers such as methanol, 2,2,2-trifluoroethanol and 2H-hexafluoro-2-propanol in the eluent was also investigated.

Carboxylic Acids↗
PubMed2000

Conductivity detection of polymerase chain reaction products separated by micro-reversed-phase liquid chromatography.

In this paper, we describe the application of micro-reversed-phase high-performance liquid chromatography (mu-RP-HPLC) for the separation and/or purification of polymerase chain reaction (PCR) products with detection accomplished using a miniaturized conductivity detector. The conductivity detector used two Pt wires and a bipolar waveform applied to the electrode pair from which the conductivity of the bulk solution could be measured. In the mobile phase used for the mu-RP-HPLC separation of the PCR product, the mass detection limit for herring sperm DNA using conductivity was found to be 11 ng. Efficient separation of the PCR amplicon from the other reagents present in the PCR cocktail was achieved in less than 4 min with a capacity factor of 2.5 and separation efficiency of 9.1 x 10(3) plates. The separation was carried out using reversed-phase ion-pair chromatography with a triethylammonium acetate ion-pairing agent.

Calibration↗
PubMed2000

Fast development of separation methods for the chiral analysis of amino acid derivatives using capillary electrophoresis and experimental designs.

The use of experimental design in method development was studied for the chiral separation of several amino acid derivatives with capillary electrophoresis. The aim of this study was to define rapidly experimental conditions under which the enantiomers can be sufficiently separated for quantification and to derive a methodology for the separation of new compounds. Three modified cyclodextrins (CDs) were used as chiral selectors: hydroxypropyl-beta-cyclodextrin, carboxymethyl-beta-CD and sulfobutylether-beta-CD. The following factors were examined: the type of cyclodextrin, the CD concentration, the pH and the % of organic modifier (methanol) of the electrolyte. Two types of fractional factorial design were used depending on the type of analyte and on the number of factors selected: a 3(4-2) fractional factorial design (4 factors studied at 3 different levels) and a 2(3-1) fractional factorial design (3 factors at 2 different levels). From the 14 compounds investigated, 12 could be separated with one or another CD and not more than 9 experiments were required. No generalisation of the best analysis conditions was possible within this family of compounds. Specific analysis conditions must be defined for each analyte. Experimental designs have shown to be very useful to determine rapidly conditions under which each enantiomer can be separated with an acceptable resolution.

Amino Acids↗
PubMed2000

Separation of acidic compounds by strong anion-exchange capillary electrochromatography.

Separation of the acidic compounds in the ion-exchange capillary electrochromatography (IE-CEC) with strong anion-exchange packing as the stationary phase was studied. It was observed that the electroosmotic flow (EOF) in strong anion-exchange CEC moderately changed with increase of the eluent ionic strength and decrease of the eluent pH, but the acetonitrile concentration in the eluent had almost no effect on the EOF. The EOF in strong anion-exchange CEC with eluent of low pH value was much larger than that in RP-CEC with Spherisorb-ODS as the stationary phase. The retention of acidic compounds on the strong anion-exchange packing was relatively weak due to only partial ionization of them, and both chromatographic and electrophoretic processes contributed to separation. It was observed that the retention values of acidic compounds decreased with the increase of phosphate buffer and acetonitrile concentration in the eluent as well as the decrease of the applied voltage, and even the acidic compounds could elute before the void time. These factors also made an important contribution to the separation selectivity for tested acidic compounds, which could be separated rapidly with high column efficiency of more than 220000 plates/m under the optimized separation conditions.

Acetonitriles↗
PubMed2000

Chiral capillary electrophoresis as predictor for separation of drug enantiomers in continuous flow zone electrophoresis.

Separation of the enantiomers of chlorpheniramine and methadone in acidic buffers containing carboxymethyl-betacyclodextrin (CMCD) as chiral selector was investigated by capillary zone electrophoresis. For a range of pH and CMCD concentrations, the mobility difference and resolution of the enantiomers were determined. Then, conditions known to provide well resolved enantiomers and optimized chiral separation were applied to chiral continuous flow electrophoresis. In that approach, a thin film of fluid flowing between two parallel plates is employed as carrier for electrophoresis. The electrolytes and the sample are continuously admitted at one end of the electrophoresis chamber and are fractionated by an array of outlet tubes at the other. The number of pure enantiomeric fractions obtained by chiral continuous flow electrophoresis was found to be directly dependent on the enantiomeric mobility difference. For racemic chlorpheniramine separated in a betaine-acetic acid buffer at a total throughput of 5 mg/h, complete enantiomeric separation is shown to require a mobility difference of about 3 x 10(-9) m2/V s. Furthermore, compared to the previous investigations with hydroxypropyl-beta-cyclodextrin, CMCD was found to permit improved fractionation of methadone enantiomers. With a total racemic drug throughput of about 15 mg/h, continuous flow zone electrophoresis processing with CMCD as chiral selector is shown to have the potential of providing pure enantiomers on a mg/h scale. The results indicate that chiral capillary zone electrophoresis data can be employed as predictor for preparative scale chiral separations based upon continuous flow zone electrophoresis.

Chlorpheniramine↗
PubMed2000

Separation of acidic solutes by nonaqueous capillary electrophoresis in acetonitrile-based media. Combined effects of deprotonation and heteroconjugation.

Nonaqueous capillary electrophoresis (NACE) is a chemical separation technique that has grown in popularity over the past few years. In this report, we focus on the combination of heteroconjugation and deprotonation in the NACE separation of phenols using acetonitrile (ACN) as the buffer solvent. By preparing various dilute buffers consisting of carboxylic acids and tetrabutylammonium hydroxide in ACN, selectivity may be manipulated based on a solute's dissociation constant as well as its ability to form heterogeneous ions with the buffer components. ACN's low viscosity, coupled with its ability to allow for heteroconjugation, often leads to rapid and efficient separations that are not possible in aqueous media. In this report, equations are derived showing the dependence of mobility on various factors, including the pKa of the analyte, the pH and concentration of the buffer, and the analyte-buffer heteroconjugation constant (Kf). The validity of these equations is tested as several nitrophenols are separated at different pH values and concentrations. Using nonlinear regression, the Kf values for the heteroconjugate formation between the nitrophenols and several carboxylate anions are calculated. Also presented in this report are the NACE separations of the 19 chlorophenol congeners and the 11 priority pollutant phenols (used in US Environmental Protection Agency methods 604, 625/1625 and 8270B).

Acetonitriles↗
PubMed2000

Separation of proteins by sodium dodecylsulfate capillary electrophoresis in hydroxypropylcellulose sieving matrix with laser-induced fluorescence detection.

Sodium dodecyl sulfate capillary electrophoresis by using hydroxypropylcellulose as the sieving matrix was developed for separation of proteins. 3-(2-furoyl)quinoline-2-carboxaldehyde, a fluorogenic dye, was used as the pre-column reagent to label proteins, which allows the use of laser-induced fluorescence to improve the detection sensitivity. Five standard proteins within the molecular mass range of 14,000-97,000 were used to test this method and a calibration curve was obtained between the molecular mass of these proteins and their peak migration times. This method was also applied to the separation of proteins from HT29 human colon adenocarcinoma cell extracts, and, typically, nearly 30 protein components could be resolved in a 20-min separation. Similar separation patterns were observed for the cell extract proteins when three running buffer systems were employed, indicating that buffer composition did not have much influence on the separation based on HPC sieving.

Cellulose↗
PubMed2000

Enantiomeric separations of cationic and neutral compounds by capillary electrochromatography with monolithic chiral stationary phases of beta-cyclodextrin-bonded negatively charged polyacrylamide gels.

Enantiomeric separation by capillary electrochromatography with beta-cyclodextrin-bonded negatively charged polyacrylamide gels was examined. The columns used are capillaries filled with a negatively charged polyacrylamide gel, a so-called monolithic stationary phase, to which allyl carbamoylated beta-CD (AC-beta-CD) derivatives covalently bind. The capillary wall is activated first with a bifunctional reagent to make the resulting gel bind covalently to the inner surface of the fused-silica tubing. Enantiomeric separations of 15 cationic compounds were achieved using the above-mentioned columns and mobile phases of 200 mmol l(-1) Tris-300 mmol I(-1) boric acid buffer (pH 7.0 or 9.0) or 200 mmol l(-1) Tris-300 mmol l(-1) boric acid buffer (pH 7.0) containing an achiral crown ether (18-crown-6). Enantiomeric separations of two neutral compounds were also achieved using 200 mmol l(-1) Tris-300 mmol l(-1) boric acid buffer (pH 9.0) as a mobile phase. High efficiencies of up to 150,000 plates m(-1) were obtained. Both the within- and between-run reproducibilities of retention time and separation factor were good. The reproducibilities of retention time and separation factor for three different columns prepared from a different batch of monomers were acceptable. The gel-filled capillaries were stable for at least 3 months with intermittent use, utilizing the mobile phase of 200 mmol I(-1) Tris-300 mmol I(-1) boric acid buffer (pH 9.0).

Acrylic Resins↗
PubMed2000

Separation selectivity of anionic metal complexes of N,N'-bis(hydroxybenzyl)ethylenediamine-N,N'-diacetic acid in ion and ion electrokinetic chromatography.

The complexes of Fe(III), Co(III), Mn(III), Al(III), Cu(II), Ni(II), Cd(II) and Zn(II) with N,N'-bis(hydroxybenzyl)ethylenediamine-N,N'-diacetic acid (HBED) were separated by ion exchange in different modes: ion chromatography (IC) and ion electrokinetic chromatography (IEKC). In column IC these complexes were separated on an IonPac AS4a anion-exchange column (Dionex, USA). Parameters of the background electrolyte that were examined in IEKC mode include polymer, competing ion concentration and pH. The use of poly(diallyldimethylammonium chloride) (PDADMACl) as a modifier in IEKC provides separation selectivity only slightly different from that observed in IC on the IonPac AS4a column. Optimal separation conditions were found to be: 0.1 mM HBED, 50 mM PDADMAOH, 10 mM Na2 B4 O7, pH adjusted to 10 with acetic acid. The use of an aromatic ligand allowed a 10-fold decrease in detection limits of metal ions in comparison with previously studied EDTA. A separation efficiency up to 400,000 theoretical plates was demonstrated for IEKC.

Anions↗
PubMed2000

Pressurized gradient capillary electrochromatographic separation of eighteen amino acid derivatives.

A pressurized gradient capillary electrochromatography (pCEC) instrument was developed to separate 18 amino acid derivatives. A reversed-phase C18 column (3 microm, 130 mm x 75 microm I.D.) and an acetate buffer (50 mmol/l NaAc, pH 6.4) with an ion-pair reagent (1% N,N-dimethylformamide) were used to separate derivatized amino acids from a standard solution (2 microg/ml), and the wavelength of the UV-Vis detector was 360 nm. The pressure on the capillary column was kept at approx. 70 Pa and 3 kV positive voltage was added on the outlet end of column. The effect of voltage on the eluting order of amino acids and the resolution of separation were studied, and it was found that when the voltage was higher than 3 kV, the adsorption of amino acids in the porous C18 column occurred. The effect of salt concentration, injection volume, and column length on the separation of amino acids was determined. The amino acid sample was separated by pCEC, and RSDs of the migration times of each amino acid were all less than 2.5%.

Amino Acids↗
PubMed2000

Separation of two groups of oestrogen mimicking compounds using micellar electrokinetic chromatography.

Two groups of compounds are being investigated due to their reported oestrogen mimicking characteristics in the environment. Separation of phenolic compounds and synthetic oestrogens using micellar electrokinetic chromatography is reported. Photodiode array detection is used for both separations. A standard separation buffer can be used for both groups of compounds including zwitterionic buffer cyclohexylamino-1-propanesulfonic acid, 20 mM at pH 11.5. It was found necessary to include 15% acetonitrile and 25 mM sodium dodecyl sulfate to aid separation and maintain analytes in solution. Optimum separations are achieved using 20 kV with hydrodynamic injection for 5 s. The relative standard deviation (RSD) for reproducibility was investigated for a mixture of phenols and synthetic oestrogens. For these compounds RSD was found to be <0.6% in all cases. Peak efficiencies ranged from 76,000 to 150,000 theoretical plates for different analytes. Application to environmental samples is discussed.

Buffers↗
PubMed2000

Dynamic modification of the capillary wall for electrophoretic separations of small ions.

Separations of small ions were carried out under nonequilibrated conditions using capillaries treated with NaOH, HCl, or tris(hydroxymethyl)aminomethane (Tris) prior to analysis. For separations of benzoic acid isomers or acids and amines under weakly acidic conditions, capillaries flushed with 0.1 M NaOH and subsequently with running buffers prior to analysis were used. Separations of six benzoic acid isomers were accomplished in 4 min in 1 mM phosphate buffers, pH 4.01, containing 2.5 mM hydroxypropyl-beta-cyclodextrin. Without additives, the separation of biological amines and acids were also achieved in 10 min at pH 4.01. Capillaries treated with 0.1 M HCl prior to analysis were tested in separations of six phenols in 5 mM Tris solutions at pH 7.0. As a result of small electrophoretic mobilities of phenols against a small electroosmotic flow, resolution was optimized. We also found that reproducibility was improved using capillaries treated with HCl. The relative standard deviations of migration mobility of phenols were less than 1%, which were smaller than those obtained using capillaries treated with 0.1 M NaOH or Tris.

Electrophoresis, Capillary↗
PubMed2001

Chiral separations using the macrocyclic antibiotics: a review.

The macrocyclic antibiotics have recently gained popularity as chiral selectors in CE, HPLC and TLC. The macrocyclic antibiotics used for chiral separations include the ansamycins, the glycopeptides, and the polypeptide antibiotic thiostrepton. Although not strictly considered macrocyclic antibiotics, the aminoglycosides are antibiotics that have been used for chiral separations in CE. More chiral analytes have been resolved using the glycopeptides than with the other macrocyclic antibiotics combined. The glycopeptides vancomycin, ristocetin A and teicoplanin have been used extensively as chiral selectors in CE, with ristocetin A appearing to be the most useful chiral selector followed by vancomycin and teicoplanin, respectively. The macrocyclic antibiotics have also been used as chiral bonded phases in HPLC, and HPLC stationary phases based on vancomycin, ristocetin A and teicoplanin have been commercialized. Ristocetin A seems to be the most useful glycopeptide HPLC bonded phase, but its greater expense can be a drawback. The macrocyclic antibiotics have been used with micelles to improve efficiency, provide unique selectivity, and extend the range of separations to neutral solutes. Changing the macrocyclic antibiotic used in CE or HPLC can significantly alter the enantioselectivity of the separations. In fact, the glycopeptide antibiotics are complementary to one another, where if a partial enantioresolution is obtained with one glycopeptide, there is a high probability that a baseline or better separation can be obtained with another.

Anti-Bacterial Agents↗
PubMed2001

Conductivity detection and quantitation of isotachophoretic analytes on a planar chip with on-line coupled separation channels.

A poly(methylmethacrylate) chip, provided with two separation channels in the column-coupling (CC) arrangement and on-column conductivity detection sensors and intended, mainly, to isotachophoresis (ITP) and ITP-capillary zone electrophoresis (CZE) separations was developed recently. The present work was aimed at assessing its performance relevant to the detection and quantitation of the ITP analytes. Hydrodynamic (HDF) and electroosmotic (EOF) flows of the solution in the separation compartment of the CC chip were suppressed and electrophoresis was a dominant transport process in the ITP separations with model analytes carried out in this context. When the surfaces of the detection electrodes of the conductivity sensors on the chip were appropriately cleaned qualitative indices of the test analytes [relative step heights (RSHs)], provided by a particular detection sensor, agreed within 1% (expressed via RSDs of the RSH values). Their long-term reproducibilities for one sensor, as estimated from 70 ITP runs repeated in 5 days, were 2% or less. Sensor-to-sensor and chip-to-chip fluctuations of the RSH values for the test analytes were 2.5% or less. In addition, experimentally obtained RSH values agreed well with those predicted by the calculations based on the ITP steady-state model. Reproducibilities of the migration velocities attainable on the CC chips with suppressed EOF and HDF, assessed from the migration time measurements of the ITP boundary between well-defined positions on the separation channels of the chips (140 repeated runs on three chips), ranged from 1.4 to 3.3% for the migration times in the range of 100-200 s. Within-day repeatabilities of the time-based zone lengths for the test analytes characterized 2% RSDs, while their day-to-day repeatabilities were less than 5%. Chip-to-chip reproducibilities of the zone lengths, assessed from the data obtained on three chips for 100 ITP runs, were 5-8%.

Electrochemistry↗