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At least 973 records · Page 54Linked to original sources
PubMed2002

Separation of alkamides from Echinacea purpurea extracts by cyclodextrin-modified micellar electrokinetic chromatography.

Separation of nine important alkyl methylbutyl- and isobutylamides (known as alkamides) obtained from Echinacea purpurea extracts was investigated by using cyclodextrin-modified micellar electrokinetic chromatography (CD-MEKC). Hydrophobic alkamides interact strongly with the micelles from the most common surfactants used in MEKC and this lead to predominant partition of the analytes into the micellar phase, resulting in poor resolution. The addition of neutral CDs to the alkaline (10 mM phosphate buffer pH 8.0) micellar system of sodium dodecyl sulfate (SDS), sodium cholate (SC) and sodium deoxycholate (SDC) was found to improve the separation of the studied alkamides. Among the several combinations surfactant/CD, three different systems showed to be particularly effective: SDS/hydroxypropyl-beta-CD (110 mM/100 mM) and SC/heptakis (2, 3, 6-tri-O-methyl)-beta-CD (200 mM/40 mM) which provided a complete separation of the studied compounds, and SDC/heptakis (2, 6-di-O-methyl)-beta-CD. The importance of appropriate surfactant vs. CD concentration ratio as well as that of total concentration of both surfactant and CD was considered. The optimization of the separation was performed by focussing the need for a rapid separation of nine alkamides diagnostically useful to define the fingerprint of Echinacea species.

Amides↗
PubMed1988

Properties of scrapie prion proteins in liposomes and amyloid rods.

The scrapie prion protein (PrP 27-30) has been demonstrated to be required for infectivity. Aggregates of PrP 27-30 form insoluble amyloid rods which resist dissociation by non-denaturing detergents. Mixtures of the detergent cholate and phospholipids were found to solubilize PrP 27-30 with full retention of scrapie prion infectivity. No evidence for a prion-associated nucleic acid could be found when the phospholipid vesicles with PrP 27-30 were digested with nucleases and Zn2+. Under digestion conditions which allowed hydrolysis of exogenous nucleic acids, no diminution of prion infectivity was observed. Tobacco mosaic virions added to the liposomes at a concentration 100 times lower than the scrapie prion titre could be seen by electron microscopy. These studies indicate that there is no subpopulation of filamentous scrapie viruses hidden amongst the prion rods - indeed, they would have been observed among the liposomes. The partitioning of PrP 27-30 and scrapie infectivity into phospholipid vesicles argues for a central role of PrP 27-30 in scrapie pathogenesis and establishes that the prion amyloid rods are not essential for infectivity.

Amyloid↗
PubMed1993

On the interaction of polypeptides with bile salts or bilirubin-IX alpha.

Aqueous solutions formed by polypeptides, simple models of proteins, and bile salts (sodium cholate and deoxycholate, NaC and NaDC, respectively) or bilirubin-IX alpha (BR) have been studied by CD measurements. They could mimic more complicated biliary systems, thus supplying a possible interpretation of the behavior of some amino acid residues in the biliary proteins. The aggregation of NaDC and NaC in water can be monitored by CD measurements. Bile salts, in submicellar and micellar form, stabilize poly(L-Lys) (PLL) in alpha-helical conformation. The alpha-helix content increases with increasing bile salt concentration and ionic strength. NaDC seems to be a slightly better stabilizing agent of the alpha-helix conformation than NaC. Models characterized by hydrogen bonds between bile salts and PLL are proposed, also resorting to previous data available on the systems formed by NaDC and poly(L-Leu-L-Leu-L-Lys) (PLLL) or poly(L-Leu-L-Leu-L-Asp) (PLLA). Binding of BR to PLL, poly(D-Lys), poly(L-Glu), PLLL, and PLLA in water has been investigated by CD spectra in order to clarify the nature of the association complexes and the mechanism of the BR enantioselective complexation. Potential energy calculations provide binding models capable of explaining the enantioselective ability of the PLL and PLLL alpha-helices toward the left- and right-handed enantiomer of BR, respectively. BR is bound to -NH2 groups of PLL and PLLL lying on a right- and left-handed spiral, respectively. These results, together with those formerly obtained for some bile salts-BR systems, indicate that the selectivity originates from a binding that involves large regions of the BR molecule and gives rise, very probably, to moderate conformational changes from the "ridge tile" structure observed in the crystals. In some cases van der Waals forces can play a crucial role in the chiral recognition of bilirubin. Moreover, possible interaction models of BR with human serum albumin are proposed on the basis of a recent x-ray crystal structure of the protein.

Amino Acid Sequence↗
PubMed1978

Procedure for the simultaneous large-scale isolation of pullulanase and 1,4-alpha-glucan phosphorylase from Klebsiella pneumoniae involving liquid-liquid separations.

A procedure for the simultaneous large-scale isolation of pullulanase and 1,4-alpha-glucan phosphorylase from Klebsiella pneumoniae is described. The pullulanase is solubilized from the cell wall by cholate treatment; cells and cell debris are removed by partition in a poly(ethylene glycol) (PEG)-dextran two-phase system and from the upper (PEG) phase of this system the pullulanase is isolated by ultrafiltration and precipitation with N-cetyl,N-,N-,N-trimethyl ammonium bromide to a purity of about 80% with a yield of 70%. The preparations are free of alpha-amylase activity. The cell containing dextran-rich phase is passed through a Manton-Gaulin homogenizer. Then the phosphorylase is separated from the cell debris by partition in a second PEG-dextran system. From the top phase of this system the phosphorylase is isolated by distribution in a PEG-salt two-phase system followed by batch adsorption on carboxymethyl-Sephadex in a yield of 55%, a purity of around 90%, and nearly free of glycosyltransferase activity. All steps in the isolation of the two enzymes can be performed easily in a large scale.

Cell Fractionation↗
PubMed1978

Non-operative treatment of retained bile duct calculi in patients with an indwelling T tube.

The results of combined instrumental and chemical treatment of retained bile duct calculi in 18 patients with an indwelling T tube are reported. The instrumental extraction of stones was carried out through the T tube channel using a modified Dormia apparatus. The chemical method involved continuous infusion through the T tube of heparin in saline alternating with sodium cholate. The treatment was successful in 16 of 18 patients with from 1 to 14 residual stones. The instrumental extraction of stones is recommended as the treatment of choice 5--6 weeks after choledochotomy in patients with residual stones and an indwelling T tube. Subsequent chemical treatment is recommended if remnants of stones are left in the bile duct after instrumental treatment.

Adult↗
PubMed1979

In vitro dissolution of human gallstones: the efficacy of heparinized solutions.

The use of heparinized solutions to dissolve or fragment stones retained in the biliary tree after surgery is still controversial. In this in vitro study heparin in concentrations of up to 100,000 mu/l did not dissolve or fragment the stones examined, nor did it enhance the dissolution properties of the bile salt, sodium cholate.

Cholelithiasis↗
PubMed1979

The effect of bile acids on colonic myoelectrical activity.

The effect of different concentrations of sodium cholate, sodium chenodeoxycholate and sodium deoxycholate on colonic myoelectrical activity was studied in 4 dogs. There was no statistically significant difference in percentage motility, motility index, basal pressure or mean slow wave frequency with either cholic or chenodeoxycholic acid (5--15 mM). Deoxycholic acid (15 mM), however, caused a marked increase in percentage motility (median control value 4.1, range 0--23; after installation, median value 27--0, range 20.6--45.0, P less than 0.001). This was accompanied by an increase in spike activity, but no alteration in mean slow wave frequency or basal pressure was seen. Cholestyramine inhibited the motor response. It appears that only deoxycholic acid affects both motility and absorption, presumably by different pathways, and may thus assume importance in disorders of colonic motility.

Action Potentials↗
PubMed2005

Separation and determination of active components in Schisandra chinensis Baill. and its medicinal preparations by non-aqueous capillary electrophoresis.

A simple, economical and effective non-aqueous capillary electrophoresis separation and detection method was developed for the quantification of deoxyschizandrin and gamma-schizandrin in Schisandra chinensis Baill. and its medicinal preparations for the first time. After optimization of separation conditions, a buffer of 140 mmol/L sodium cholate in methanol was selected for separating the two analytes, but baseline separation of SA and SB in real samples was not obtained. Therefore second-order derivative electropherograms were applied for resolving overlapping peaks. Regression equations revealed good linear relationships (correlation coefficients 0.9975--0.9988) between peak heights in second-order derivative electropherograms and concentrations of the two analytes. The relative standard deviations (RSD) of the migration times and the peak height of the two constituents were in the ranges 0.62--0.79% and 0.25--2.17% (intra-day) and 1.43--2.06 and 4.08--5.72% (inter-day), respectively. The recoveries of the two constituents ranged from 93.2 to 103.0%. The results indicated that baseline separation of the analytes was sometimes hard to obtain in real samples and second-order derivative electropherograms were applicable for the resolution and analysis of overlapping peaks.

Cyclooctanes↗
PubMed1986

Fast atom bombardment combined with tandem mass spectrometry for determination of bile salts and their conjugates.

Fast atom bombardment desorption of bile salts produces negative ions which show little fragmentation. The lack of fragmentation limits the utility of the method for resolving questions regarding specific structural features. This paper is a report of negative ion fast atom bombardment mass spectra and collision-activated decomposition spectra of cholate, chenodeoxycholate, lithocholate, taurocholate, taurochenodeoxycholate, taurolithocholate, 3 beta-ol-5-cholenate, taurolithocholate-3-sulfate and glycolithocholate-3-sulfate. The collision-activated decomposition spectra are useful for distinguishing bile salt structural features and for quantifying relative amounts of isomeric ions in a mixture. The negative ion mode is well suited for generating anions of bile salts and, when coupled with collisional activation, provides complementary information to the positive ion mode. The collision-activated fragmentation is also unusual as it appears to be an example of reactions occurring remote from the charge site. Furthermore, on the basis of the fragmentations, the charge site can be located in the amphiprotic form of some gas-phase diprotic bile acids such as taurolithocholate-3-sulfate and glycolithocholate-3-sulfate.

Bile Acids and Salts↗
PubMed2006

Synthesis of bridged and metallobridged bis(beta-cyclodextrin)s containing fluorescent oxamidobisbenzoyl linkers and their selective binding towards bile salts.

A series of beta-cyclodextrin (beta-CD) dimers containing fluorescent 2,2'-oxamidobisbenzoyl and 4,4'-oxamidobisbenzoyl linkers--that is, 6,6'-[2,2'-oxamidobis(benzoylamino)]ethyleneamino-6,6'-deoxy-bis(beta-CD) (2), 6,6'-[2,2'-oxamidobis(benzoylamino)]diethylenediamino-6,6'-deoxy-bis(beta-CD) (3), 6,6'-[4,4'-oxamidobis(benzoylamino)]ethyleneamino-6,6'-deoxy-bis(beta-CD) (4), and 6,6'-[4,4'-oxamidobis(benzoylamino)]diethylenediamino-6,6'-deoxy- bis(beta-CD) (5)--were synthesized from the corresponding oxamidobis(benzoic acid)s through treatment with mono[6-aminoethyleneamino-6-deoxy]-beta-CD or mono[6-diethylenetriamino-6-deoxy]-beta-CD. Further treatment of 2-5 with copper perchlorate gave their Cu(II) complexes 6-9 in satisfactory yields. The conformation and binding behavior of 2-9 towards two bile salt guests--sodium cholate (CA) and sodium deoxycholate (DCA)--was comprehensively investigated by circular dichroism, 2D NMR spectroscopy, and fluorescence spectroscopy in Tris-HCl buffer solution (pH 7.2) at 25 degrees C. Thanks to the cooperative host-linker-guest binding mode, the stoichiometric 1:1 complexes formed by bis(beta-CD)s 2-5 with bile salts gave high stability constants (KS values) of up to 10(3)-10(4) M(-1). Significantly, benefiting from the intramolecular 1:2 or 2:4 binding stoichiometry, the resulting complexes of metallobis(beta-CD)s 6-9 with bile salts gave much higher KS values of up to 10(6)-10(7) M(-2). The enhanced binding abilities of bis(beta-CD)s and metallobridged bis(beta-CD)s are discussed from the viewpoints of induced-fit interactions and multiple recognition between host and guest.

Benzoates↗
PubMed1993

Fimbrin localized to an insoluble cytoskeletal fraction is constitutively phosphorylated on its headpiece domain in adherent macrophages.

The actin-bundling protein fimbrin is homologous to 1-plastin, a 65kD phosphoprotein expressed in leukocytes and transformed cells [de Arruda et al., J. Cell Biol. 111, 1069-1080]. Because fimbrin is present in cell adhesion sites, we studied the phosphorylation state of fimbrin and its distribution in macrophages sequentially extracted with Triton-X-100 (soluble fraction), Tween 40-deoxy-cholate (cytoskeletal fraction), and SDS (insoluble cytoskeletal fraction). The approximate distribution of fimbrin and actin among these fractions was found to be: 65% fimbrin/55% actin in the soluble fraction, 30% fimbrin/20% actin in the cytoskeletal fraction, and 5% fimbrin/25% actin in the insoluble cytoskeletal fraction. PMA did not alter this distribution. Fluorescence microscopy of acetone-extracted macrophages showed that actin is concentrated in podosomes at the substratum interface and is diffusely distributed throughout the remainder of the cell. Fimbrin colocalizes with actin in podosomes and also exhibits a punctate distribution in the cytoplasm that overlaps with actin. In Tween 40/DOC-extracted cells, podosomes remain, and fimbrin also exhibits a punctate distribution along actin filaments. Metabolic 32PO4 labeling revealed that fimbrin is constitutively phosphorylated and that phosphorylated fimbrin is concentrated in the insoluble cytoskeletal fraction. PMA increased the relative levels of fimbrin phosphorylation twofold but did not alter the pattern of fimbrin fluorescence or the distribution of phosphorylated fimbrin. Limited trypsin digestion and phosphoamino acid analysis demonstrated that phosphorylation occurs specifically on serine residues within the 10kD headpiece domain of fimbrin. Phosphorylation of the headpiece domain could regulate the actin binding and bundling properties of fimbrin, or it could regulate the interaction of fimbrin with other proteins.

Actins↗
PubMed1996

Micellar electrokinetic capillary chromatography of three natural vitamin A derivatives.

Micellar electrokinetic chromatography (MEKC) using bile salts has been employed to separate retinoids differing in structure and charge; bile salts in MEKC allows the separation of liposoluble molecules but, to the best of our knowledge, there are only few data on the above-mentioned technique for the separation of highly hydrophobic compounds. The three natural vitamin A derivatives, retinal, retinol and retinoic acid, were successfully separated by MEKC using sodium cholate within a relatively short time (ca. 25 min), whereas the separation of these compounds was not successful using sodium dodecyl sulfate or sodium deoxycholate. Several parameters (pH and organic modifiers, in addition to bile salts concentration) have been tested to provide a system that can be extended to synthetic retinoids, which are often used in treating several diseases, including cancer prevention and therapy.

Buffers↗
PubMed1997

Separation of fungicides by micellar electrokinetic capillary chromatography.

Capillary electrophoresis with ultraviolet detection (CE/UV) of selected fungicides (carbendazim, metalaxyl, propiconazole, and vinclozolin) using different buffer compositions was investigated. Capillary zone electrophoresis (CZE) with 10 mM sodium phosphate (pH 7.0) was not useful in separating the four fungicides used in this study. However, the four fungicides were well resolved by employing micellar electrokinetic capillary chromatography (MEKC). Among the two surfactants tested in MEKC, bile salts provided better separation compared to sodium dodecyl sulfate (SDS). A buffer consisting of 10 mM sodium phosphate with 100 mM sodium cholate and 10% methanol (pH 7.0) gave best results; excellent separation of the four compounds was achieved in less than 15 min. The CE/UV method was validated by analyzing deionized and lake-water samples fortified with known concentrations for the four fungicides. Average recoveries of the fungicides in lake water of 4 micrograms/L level ranged from 42 to 87%.

Alanine↗
PubMed1997

Capillary electrophoretic detection of metabolites in the urine of patients receiving hypoglycemic drug therapy.

Micellar electrokinetic chromatography (MEKC) in tandem with diode array detection (DAD) has been exploited as an analytical method for the separation and detection of sulfonylurea drugs. The ultimate goal is the development of an assay to detect these drugs or their metabolites in urine as a means of diagnosing sulfonylurea drug abuse. Using a separation buffer consisting of 5 mM borate/5 mM phosphate/75 mM sodium cholate, separation of both the second and third generation sulfonylurea drugs can be achieved. The characteristic absorbance spectra associated with each of the third generation drugs, glipizide and glyburide, allow for their identification in mixtures. Coinjection of glyburide, its primary metabolite, hydroxy glyburide, and glipizide demonstrated that the metabolite was resolved from the parent drug but shared its absorbance spectral properties. MEKC analysis of a series of solid phase-extracted urine samples from patients prescribed glipizide or glyburide, as well as from control patients not ingesting the drug, showed that the parent compounds were difficult to detect in the urine. However, the use of DAD allowed for detection of metabolites in the urine of these patients. With glyburide patients, only primary metabolites were detected, while urine from patients on glipizide showed a series of peaks whose absorbance spectra was consistent with the presence of both primary and secondary metabolites. In addition, the intensity of the metabolite peaks corresponded reasonably well with the respective dose and in vivo time interval associated with the urine collection. This study shows that MEKC with DAD has potential for further exploration as a clinical assay for detecting surreptitious abuse of sulfonylurea drugs.

Electrophoresis, Capillary↗
PubMed1998

On-line partial filling micellar electrokinetic capillary chromatography-electrospray ionization-mass spectrometry of corticosteroids.

The one-line combination of micellar electrokinetic chromatography (MECC) with electrospray ionization-mass spectrometry (ESI-MS) was investigated using some corticosteroids as model components. The on-line technique is difficult because the micelles in the electrolyte solution tend to soil the mass spectrometer and lower the sensitivity of the spectrometer. To prevent the micelles from reaching the mass spectrometer, several techniques have been developed among which is the partial filling (PF) technique. In this study the PF-MECC technique was investigated in an on-line MECC-ESI-MS study of mixtures of corticosteroids. Because the compounds are uncharged, partitioning or interaction with micelles is required to achieve separation. Surfactant solutions of sodium dodecyl sulfate (SDS), sodium cholate (SC), and SDS/SC mixtures were used as micellar phase. Good MECC separation was achieved after optimization of the surfactant concentrations and the length of the injected micellar plug. Both hydrodynamic and electrokinetic injections of the micellar solutions were tested. A basic ammonium acetate solution was used as the CE electrolyte solution. The ESI-MS analysis of the compounds was performed in the positive ionization mode, using an acidic sheath liquid. Because of the low MS intensities of the corticosteroids, the peaks were isolated during the MS runs. MS-MS and MS-MS-MS data on the corticosteroids were obtained by off-line injection of the compounds.

Adrenal Cortex Hormones↗
PubMed1998

Rapid estimation of octanol-water partition coefficients of pesticides by micellar electrokinetic chromatography.

Micellar electrokinetic chromatography (MEKC) was evaluated as a new technique for the rapid estimation of octanol-water partition coefficient (logKow). Retention measurements for more than 40 reference pesticides with varied structural characteristics and hydrophobicity were carried out in two MEKC systems, based on sodium dodecyl sulfate (SDS) and sodium cholate (SC), respectively. To enable an accurate determination of capacity factors in the SC-MEKC system, cypermethrin (a synthetic pyrethroid insecticide) was utilized instead of Sudan III as the SC micelle tracer, since a few highly hydrophobic pesticides were found to elute after Sudan III. The linear correlation between logarithmic capacity factor (logk') and logKow in the two systems was examined. It was found that, under the typical buffer condition (10 mM sodium phosphate with 60 mM surfactant, pH 7.0), the SDS-MEKC system provided a somewhat wider dynamic range for hydrophobicity (logKow from -1.0 to 4.5). However, the correlation of logk' with logKow was not very high when all the reference pesticides were included in one single calibration set. For the SC-MEKC system, the dynamic range for logKow was in the range of 1.0-5.5, and a good linear correlation existed between logk' and logKow, even when all reference pesticides were incorporated into a single calibration group. By comparing the regression line of the reference pesticides with that of a group of simple aromatic derivatives, it was discovered that molecular size and functionality posed a less significant effect on the measurement of logKow in the SC-MEKC system than in the SDS-MEKC system. Thus, SC-MEKC shall be the system of choice for the estimation of logKow. The typical error on logKow determination using the current MEKC technique was within 0.5 units, suggesting that MEKC can be a valuable complement to reversed phase high performance liquid chromatography (RP-HPLC) for the indirect determination of logKow. Besides maintaining all the advantages of the HPLC approach, the MEKC technique showed some unique benefits, such as better inter-column reproducibility, higher throughput, and less handling of toxic pesticides and solvents.

Chromatography↗
PubMed2004

Separation and determination of biphenyl nitrile compounds by microemulsion electrokinetic chromatography with mixed surfactants.

A mixture of six biphenyl nitrile compounds and three related substances with high hydrophobicity and similar structures was successfully separated by microemulsion electrokinetic chromatography (MEEKC) within 30 min. The microemulsion system contained 100 mM sodium dodecyl sulfate (SDS), 80 mM sodium cholate (SC), 0.81% v/v heptane, 7.5% v/v n-butanol, 10% v/v acetonitrile, and 10 mM borate. The addition of SC, organic modifiers, sample preparation, and temperature all showed remarkable effects on the separation. The capacity factor (k) was calculated by using dodecyl benzene as the marker for microemulsion, and the calculated partition coefficient log P(o/w) of the solutes was in the range of 3.35-7.38. The log k values matched well with the log P(o/w) with a correlation coefficient of 0.96. In addition, the linear correlation coefficients of each compound between peak area and concentration were from 0.996 to 0.998 with the repeatability RSD value < 1.2% for migration time and < 4.8% for peak area, and the highest theoretic plate number was > 586000. MEEKC was compared with micellar electrokinetic chromatography (MEKC) indicating that the former method is more suitable for this separation and can be used for the quality control of biphenyl nitrile compounds in the synthesis of liquid crystals.

Biphenyl Compounds↗
PubMed2003

Mixed micellar electrokinetic capillary chromatography separation of depolymerized grape procyanidins.

Oligomeric procyanidins are potent antioxidant polyphenols of potential interest as disease-preventing agents. Their efficiency depends on the size and composition of their oligomeric structures. The mean degree of polymerization of these compounds is usually estimated by thiolysis with thiol-alpha-toluene followed by analysis using high-performance liquid chromatography (HPLC). We show the development of a mixed micellar electrokinetic chromatography (MEKC) method for the separation of the major components obtained after thiolysis with cysteamine (catechins and their cysteamine conjugates). MEKC studies using sodium dodecyl sulfate (SDS as pseudostationary phase led to long migration times, e.g., with 100 mM SDS, at pH 7, the solutes were separated in about 40 min), while the use of sodium cholate (SC) produced an elution window relatively short. Using a mixed micellar SC-SDS system (50 mM phosphate at pH 7 containing 40 mM SC and 10 mM SDS), it is possible to separate these compounds in less than 15 min. The proposed method is useful to separate the major components of the thiolysate in effluents from food processing (e.g., skins and seeds from grape and apple) considered as potential procyanidin sources.

Biflavonoids↗