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PubMed2002

Use of vancomycin silica stationary phase in packed capillary electrochromatography: III. enantiomeric separation of basic compounds with the polar organic mobile phase.

The separation of basic compounds into their enantiomers was achieved using capillary electrochromatography in 50 or 75 microm inner diameter (ID) fused-silica capillaries packed with silica a stationary phase derivatized with vancomycin and mobile phases composed of mixtures of polar organic solvents containing 13 mM ammonium acetate. Enantiomer resolution, electroosmotic flow, and the number of theoretical plates were strongly influenced by the type and concentration of the organic solvent. Mobile phases composed of 13 mM ammonium acetate dissolved in mixtures of acetonitrile/methanol, ethanol, n-propanol, or isopropanol were tested and the highest enantioresolutions were achieved using the first mobile phase, allowing the separation of almost all investigated enantiomers (9 from 11 basic compounds). The use of capillaries with different ID (50 and 75 microm ID) packed with the same chiral stationary phase revealed that a higher number of theoretical plates and higher enantioresolution was achieved with the tube with lowest ID.

Acetonitriles↗
PubMed2005

From solution-phase to solid-phase enyne metathesis: crossover in the relative performance of two commonly used ruthenium pre-catalysts.

A crossover in the ability of two distinct ruthenium-based metathesis pre-catalysts to effect the synthesis of dialkenylboronic esters in solution and on the solid-phase was observed. Specifically, while the Grubbs 2nd generation pre-catalyst 3 affords a greater degree of conversion to product than the Hoveyda-Grubbs pre-catalyst 2 in a solution-phase enyne-metathesis reaction, this trend is reversed in the solid-phase variant. Systematic investigation showed this trend to be general, regardless of variations in the homoallylic alcohol and alkynylboronic ester components of the reaction, as well as in the type of solid support employed. Experiments to determine a mechanistic hypothesis for this trend highlighted the significance of the ruthenium remaining bound to the substrate after metathetic rearrangement and found the presence of phosphine ligand to be detrimental to the success of the solid-phase reaction. Therefore, these results suggest an expanded role for phosphine-free pre-catalysts, such as 2, in challenging solid-phase metathesis reactions.

Catalysis↗
PubMed2006

Chiral separations on polysaccharide stationary phases using polar organic mobile phases.

About 30% of a chemically diverse set of compounds were found to separate on four polysaccharide chiral stationary phases using polar organic mobile phases. No structural features appeared to correlate to successful separations. Titrations between normal and polar organic mobile phases suggested that separation mechanisms do not differ between these mobile phases. Attempts made to control retention met with varying degrees of success. Addition of hexane to alcohols had minor effects on retention although this was occasionally beneficial. Addition of water to alcohols increased retention. Addition of water to acetonitrile decreased retention. Addition of alcohol to acetonitrile also proved beneficial to the separation of some compounds. Loading studies performed to mimic preparative separations indicated that the benefits of polar organic mobile phases are largely due to increased solubility.

Acetonitriles↗
PubMed1992

Operational aspects of antibody affinity constants measured by liquid-phase and solid-phase assays.

The association constant of monoclonal antibodies (Mabs) to tobacco mosaic virus has been determined in solution and solid-phase binding assays. The ELISA equilibrium titration method developed by Friguet et al. (1985) was found to be suitable for large antigens such as viruses. In the case of intact IgG antibody, it gave equilibrium constant (K) values ca 30% lower than those obtained by classical solution-phase assay while in the case of Fab', the same values were obtained in both assays. Solid-phase binding assays gave higher K values than solution-phase assays by a factor which varied with the Mab tested (1.5- to 5.4-fold higher). Furthermore, in solution-phase assay, K values were found to depend on the antibody concentration used in the assay. These results confirm the operational nature of antibody affinity constants and indicate that in order to compare the affinity of different Mabs in a meaningful way, it is necessary to use a single technique under standardized conditions.

Antibodies, Monoclonal↗
PubMedDate not supplied

Simultaneous acquisition of phase-contrast angiograms and stationary-tissue images with Hadamard encoding of flow-induced phase shifts.

A technique for the simultaneous acquisition of three-dimensional phase-contrast angiograms and stationary-tissue images is described. Hadamard multiplexed encoding of flow information permits image acquisition times that are a third shorter than those of previous phase-contrast methods. The encoding scheme described also enables differentiation of flow-induced phase shifts from phase shifts due to resonance offset conditions such as field inhomogeneities and chemical shift. Display strategies that combine this phase information with the flow image are described.

Blood Vessels↗
PubMedDate not supplied

Ghost phase cancellation with phase-encoding gradient modulation.

Motion artifacts are a dominant cause of magnetic resonance image quality degradation. Periodic or nearly periodic motion results in image replicates of the moving structures in spin-warp Fourier imaging. The replicates, or ghosts, propagate in the image in the phase-encoding, or y, direction. These ghosted images can be considered to consist of the time-averaged spin density I0 and a ghost mask g. A set of j ghosted images Ij may be acquired in which the ghost mask is intentionally phase shifted by varying amounts relative to I0 with interleaved acquisitions that have shifted phase-encoding orders or by acquiring multiple images during a single readout period in the presence of an oscillating phase-encoding gradient. The resulting complex images Ij have the same time-averaged spin density I0 but have ghost contributions gj that, on a pixel-by-pixel basis, trace part of a circle around I0. The source images Ij can then be used to estimate I0. Simulations and experiments with the phase-encoding gradient modulation method show good general ghost suppression for a variety of quasi-periodic motion sources including both respiratory-type artifacts and flow artifacts. The primary limitation of the method is the need for rapid gradient switching.

Artifacts↗
PubMed2002

Cryogenic grinding of indomethacin polymorphs and solvates: assessment of amorphous phase formation and amorphous phase physical stability.

The effect of cryogenic grinding on five crystal forms of indomethacin (IMC) was investigated with particular interest in the formation of amorphous phase. Powder X-ray diffraction (PXRD) and differential scanning calorimetry (DSC) demonstrated that amorphous phase formation took place for all three polymorphs (gamma, alpha, and delta) and one solvate (IMC methanolate). In the latter case, a postgrinding drying stage was needed to remove desolvated methanol from the ground amorphous product because methanol destabilized amorphous IMC presumably via a plasticizing effect. The crystal structure of another solvate, IMC t-butanolate, was unaffected by grinding, indicating that amorphous phase formation on grinding does not occur in all cases. Ground amorphous materials possessed similar glass transition temperatures but significant differences in physical stability as assessed by both isothermal and nonisothermal crystallization. It is argued that physical factors, namely residual crystal phase and specific surface area, determine the isothermal and nonisothermal crystallization behavior of ground amorphous samples as opposed to intrinsic differences in the structure of the amorphous phase.

Anti-Inflammatory Agents, Non-Steroidal↗
PubMed2006

Linear free energy relationship as a tool for characterization of three teicoplanin-based chiral stationary phases under various mobile phase compositions.

Teicoplanin, teicoplanin aglycon, and methylated teicoplanin aglycon chiral stationary phases (CSPs) have been compared on the basis of the regression coefficients calculated from the linear free energy relationship (LFER) equation. The parameters have been obtained from the measurements of a set of 34 structurally diverse solutes. Influence of mobile phase composition - variation of methanol (MeOH) content - on the participation of different interactions types in the retention mechanism has been evaluated. Retention of the various interaction forces in analytes differs with both the CSP and the mobile phase composition. Hydrophobic interactions play a major role in mobile phases for high buffer contents. The more hydrophobic the CSP, the more important are they in the retention mechanism. With increase of MeOH contents in the mobile phase the major role in the interaction mechanism is shifted to more polar forces in which basicity and dipolarity/polarizability dominate. Although the LFER model does not address chiral aspects, we have attempted to explore the importance of the individual interactions in chiral discrimination of amino acids and their N-tert-butyloxycarbonyl derivatives.

Amino Acids↗
PubMed1999

Phase Behavior and Phase Structure of Protein-Surfactant-Water Systems.

Phase behavior of oppositely charged ovalbumin-DOTAC and BSA-DOTAC, and similarly charged ovalbumin-SDS, BSA-SDS, lysozyme-DOTAC, and BLG-SDS systems within the concentration range of 20 wt% of both protein and surfactant are examined in water. Aqueous solutions of ovalbumin yield, in succession, precipitation, gel, and solution with increased addition of the surfactant dodecyltrimethylammonium chloride (DOTAC). The stability range of each region is determined. Both isotropic and anisotropic gels are detected. Solutions of bovine serum albumin (BSA) form only a solution phase with oppositely charged DOTAC. One solution phase is also obtained with all similarly charged protein-surfactant systems except the BLG-SDS-water system, which produces a gel phase in addition to a large solution phase. (2)H NMR longitudinal (R(1)) and transverse (R(2)) relaxation rates are determined in solution and gel by following the behavior of selectively deuterated surfactant at the alpha-methylene group next to the surfactant head group for the oppositely charged systems ovalbumin-DOTAC and BSA-DOTAC. Large R(2)-values proved the existence of large protein-surfactant aggregates in both systems. Copyright 1999 Academic Press.

Journal Article↗
PubMed1995

Induction of phase I and phase II drug-metabolizing enzyme mRNA, protein, and activity by BHA, ethoxyquin, and oltipraz.

Various natural and synthetic compounds are known to protect against cancer by elevating phase II detoxification enzymes. Generally classified as monofunctional, these inducers are believed to trigger cellular signal(s) that activate gene transcription through an antioxidant or electrophile response element (ARE/EpRE) in responsive genes. In contrast, the phase I enzymes of drug metabolism (cytochrome P450s) are not believed to be induced by monofunctional inducers and P450 genes have not been found to contain functional ARE/EpREs. In this study, rats were treated with the monofunctional inducers tert-butylated hydroxyanisole, ethoxyquin, and oltipraz to study the inducibility of individual glutathione S-transferase isozymes, NADP(H):quinone oxidoreductase, gamma-glutamylcysteine synthetase, UDP-glucuronosyl transferase, and cytochrome P450 enzymes. Hepatic mRNAs were analyzed on Northern blots using gene-specific oligonucleotide probes for GST Ya1, Ya2, Yc1, Yc2, Yb1, Yb2, and Yf, for UGT 1*06, and for P450 1A1, 1A2, 2B1, 2C11, 3A2, and 4A1. NADP(H):quinone oxidoreductase and gamma-glutamylcysteine synthetase mRNAs were detected using cDNA probes. All the phase II detoxification enzymes analyzed, except GST Yf, were induced by the three monofunctional inducers, suggesting that these genes may be regulated by a mechanism involving an ARE/EpRE element in their promoter region. Interestingly, it was found that ethoxyquin was a particularly good inducer for both members of the P450 2B family, 2B1 and 2B2, and both ethoxyquin and oltipraz were also capable of modestly inducing P450 1A2 and 3A2. Oltipraz was found to slightly induce P450 2B2, but not 2B1, at the dose and time analyzed. Induction of mRNA generally correlated well with induction of protein levels determined by Western blot and/or enzyme activity measurements for selected enzymes. The results of this study suggest that many phase II enzymes may contain ARE/EpRE elements in addition to those confirmed to be regulated by a mechanism involving ARE/EpRE elements. In addition, it was found that several P450 enzymes were induced by monofunctional inducers, suggesting a possibility that some phase I enzymes may also be regulated by a mechanism involving ARE/EpRE elements.

Animals↗
PubMed1988

Chemical and immunochemical studies on lipopolysaccharides of Coxiella burnetii phase I and phase II.

Lipopolysaccharides of Coxiella burnetii phase I and II were comparatively investigated by chemical and immunochemical methods. LPS of phase I (LPS I) and phase II cells (LPS II) show no serological cross reaction, indicating that the serological determinants of LPS II are masked in LPS I. Chemical analysis of LPS I and II show that phase I and II cells can be considered as S and R forms of Coxiella burnetii. The structure of LPS II has recently been elucidated and shows a dimannosylated core of an alpha(1,3)-linked heptose-disaccharide which is attached to a "KDO-like" substance. In enterobacterial core-types, alpha(1,3)-linked heptose-disaccharide is also part of the inner core structure, although the heptose occurring in enterobacterial R cores is the L-glycero-D-manno-heptose. In Coxiella burnetii we have only the rare D-glycero-D-manno-heptose which is the biosynthetic precursor of the former and is in many enteric LPS, present only in addition to L-glycero-D-mannoheptose. In these R-cores, it is occupying mostly terminal positions (Radziejewska-Lebrecht et al., 1981) and is absent from the main chain. The complete structure of LPS I is not yet available, but some important points could recently be clarified. The immunodominant sugars in LPS I are C-3-branched sugars, 6-deoxy-3-C-methyl-L-gulose (L-virenose) and 3-C-(hydroxymethyl)-L-lyxose (dihydro-hydroxy-L-streptose). These two sugars have not been found so far in other lipopolysaccharides and the latter one not previously in any other natural product. Their identification is based on GLC-MS comparison with authentic and synthetic compounds. Both branched sugars (and in addition part of the mannose) are the terminal sugars in LPS I. Sites of attachment of phase I-specific sugars to the LPS II-core are: the 3-position of a branched heptose and, presumably, the 4-position of a terminal D-mannose. The extreme acid-lability of the linkages of both branched sugars was investigated in detail and is caused by the nature of the branched sugars (deoxyhexose with bulky axial substituents; pentofuranose with axial OH-groups). No information is so far available on the (penultimate) sugars to which the branched sugars are linked, but methylation analyses with LPS I, and with the recently described I/CR mutant, which is selectively lacking the virenopyranose, are presently performed.

Carbohydrate Conformation↗
PubMed1992

Average phase difference theory and 1:1 phase entrainment in interlimb coordination.

The dynamics of coupled biological oscillators can be modeled by averaging the effects of coupling over each oscillatory cycle so that the coupling depends on the phase difference phi between the two oscillators and not on their specific states. Average phase difference theory claims that mode locking phenomena can be predicted by the average effects of the coupling influences. As a starting point for both empirical and theoretical investigations, Rand et al. (1988) have proposed d phi/dt = delta omega--K sin phi, with phase-locked solutions phi = arcsin(delta omega/K), where delta omega is the difference between the uncoupled frequencies and K is the coupling strength. Phase-locking was evaluated in three experiments using an interlimb coordination paradigm in which a person oscillates hand-held pendulums. Delta omega was controlled through length differences in the left and right pendulums. The coupled frequency omega c was varied by a metronome, and scaled to the eigenfrequency omega v of the coupled system; K was assumed to vary inversely with omega c. The results indicate that: (1) delta omega and K contribute multiplicatively to phi; (2) phi = 0 or phi = pi regardless of K when delta omega = 0; (3) phi approximately 0 or phi approximately pi regardless of delta omega when K is large (relative to delta omega); (4) results (1) to (3) hold identically for both in phase and antiphase coordination. The results also indicate that the relevant frequency is omega c/omega v rather than omega c.(ABSTRACT TRUNCATED AT 250 WORDS)

Adult↗
PubMed1991

Detection of barbiturate-induced surface changes in cerebrocortical synaptosomes by phase partitioning in an aqueous two-phase system.

The barbiturates tested in this work (barbital, phenobarbital, thiopental and pentobarbital) modify the partition of synaptosomes in a Dextran T500-poly(ethylene glycol) 4000 two-phase system. Under adequate experimental conditions, the drugs increase the partition into the upper phase and this effect appears to be due to an action on the biological material and not on the interface potential of the system. This conclusion can be drawn from the fact that synaptosomes preincubated with low concentrations (0.1 mM) of barbital and pentobarbital maintained an increased partition into the upper phase. The extent of the effect observed appeared to be inversely proportional to the hydrophobicity of the drugs since phenobarbital and barbital showed a higher effect than thiopental and pentobarbital. Dithionite-induced anoxia, rotenone and ouabain also induced a similar increase of partition of synaptosomes into the upper phase, suggesting that the surface changes detected by phase partitioning modification of synaptosomes could be somehow related to the bioenergetic maintenance of the membrane ATPase.

Animals↗
PubMed1984

Utility of the gas-phase sequencer for both liquid- and solid-phase degradation of proteins and peptides at low picomole levels.

The utility of the commercially available gas-phase sequencer for complete analysis of peptide samples was investigated. Using the program supplied with the instrument, significant extractive loss of samples in Polybrene was observed, even at input levels up to 500 pmol. In order to reduce this loss, the sequencer program was modified by increasing the phenylisothiocyanate (PITC)-coupling steps from two to three and lengthening the duration of ethyl acetate (S2) delivery while reducing the delivery rate. These changes gave improved results with peptides, e.g., all eight residues of angiotensin II were identified at the 25-pmol level. In addition, background contamination was decreased and repetitive yields were increased. The instrument was also found to function well with samples coupled to solid supports; however, some of the methodologies that work adequately for covalent attachment of peptides to solid supports at the level 1-10 nmol were found to give unacceptable coupling/sequenceable yields at or below the 100-pmol level. The coupling methods tried were (1) reaction of homoserine lactone with aminopropyl (AP)-glass, (2) reaction of alpha- and epsilon-NH2 groups with p-phenylenediisothiocyanate (DITC)-glass, and (3) reaction of alpha-COOH groups with aminoaryl (AA)-glass via EDAC (1-ethyl-3,3'-dimethylaminopropyl-carbodiimide). Of these, the first method gave combined yields of 42-94% while the latter two were only 9-35% efficient. The covalently bound samples provided sequence information even at the resulting low levels, e.g., 9/13 residues of dynorphin including Lys-13 at 11 pmol. In general, sequencer runs on solid-phase samples gave "cleaner" analyses and slightly higher repetitive yields (1-2%). Sequence information has also been obtained on peptides made by solid-phase synthesis prior to cleavage from the polystyrene support. With improved coupling efficiencies, solid-phase techniques would provide an alternative to immobilization of peptides in Polybrene films for low picomole level gas-phase sequencing.

Amino Acid Sequence↗
PubMed1979

Properties of bilayer membranes in the phase transition or phase separation region.

The increase in passive permeability of bilayer membranes near the phase transition temperature is usually explained as caused by either the increase in the amount of 'boundary lipid' present in the membrane, or by the increase in lateral compressibility of the membrane. Since both the amount of 'boundary lipid' and the lateral compressibility show a similar anomaly near the transition temperature, it is difficult to distinguish experimentally between the two proposed mechanisms. We have examined some details of both of the proposed pictures. The fluid-solid boundary energy, neglected in previous work, has been computed as a function of the domain size. For a single component uncharged lipid bilayer, the results rule out the existence of even loosely defined solid domains in a fluid phase, or vice versa. Thermodynamic fluctuations, which are responsible for anomalous behaviour near the phase transition temperature, are not intense enough to approximate the formation of a domain of the opposite phase. Turning next to lateral compressibility of bilayer membranes we have considered two-component mixtures in the phase separation region. We present the first calculation of lateral compressibility for such systems. The behaviour shows interesting anomalies, which should correlate with existing and future data on transport across membranes.

Lipid Bilayers↗
PubMed1981

Studies on ovarian and adrenal studies at different phases of the menstrual cycle. IV. The effect of dexamethasone suppression and subsequent ACTH stimulation at different phases of the menstrual cycle and following the administration of 150 mg of depot-medroxy-progesterone acetate (DMPA).

In an attempt to assess the effect of depot-medroxyprogesterone acetate (DMPA) on adrenal function, to peripheral levels of a variety of steroids were estimated after dexamethasone suppression and subsequent ACTH stimulation in 5 subjects. The steroid responses observed 16 and 54 days after a single injection of 150 mg of DMPA were compared with those obtained in the same women before DMPA treatment or with those found at different phases of the cycle in another group of 6 normally menstruating women. The levels of cortisol, pregnenolone, 17-hydroxypregnenolone, dehydroepiandrosterone, androstenedione and dihydrotestosterone were significantly suppressed by dexamethasone and stimulated by ACTH in all phases of the cycle, and before and after DMPA administration. The extent of suppression or stimulation (expressed as a percentage) was different in case of different steroids, but was rather constant with regard to the same steroid. Hence, the functional capacity of the adrenal as reflected by the levels of these steroids. Dexamethasone administration did not exert any influence on the levels of progesterone and 17-hydroxyprogesterone during the different phases of the cycle; however, ACTH administration increased the levels of these two steroids in the follicular phase and also after DMPA treatment. The levels of estradiol and lutropin were not influenced by dexamethasone or ACTH at any of the occasions studied. It is concluded that the functional capacity of the adrenal cortex is constant during the various cycle phases and is not affected by the administration of a single dose of 150 mg of DMPA.

17-alpha-Hydroxypregnenolone↗
PubMed1990

Polyalkylenes used as stationary phases for preparative reversed-phase liquid chromatography.

Polyethylene and polypropylene were employed as stationary phases for preparative liquid chromatography and compared with LiChroprep RP-18. Polyalkylene phases are chemically stable and have homogeneous hydrophobic surfaces, but they are physically less resistant than silica-based phases. The influence of organic modifiers and salt ions on the capacity factors of aromatic hydrocarbons and peptides was determined. Peptides prepared by solid-phase peptide synthesis were purified on polypropylene. The results demonstrate the usefulness of polyalkylenes in preparative reversed-phase liquid chromatography, particularly for basic peptides.

Chromatography, Liquid↗
PubMed1992

Cation-exchange liquid chromatography of choline and acetylcholine on free shielded silanols of silica-based reversed-phase stationary phases.

Free anionic functions present on the surface of reversed-phase packing materials were used for the selective cation-exchange preconcentration and separation of the neurotransmitters choline and acetylcholine from a biological matrix. The cation-exchange behaviour of different reversed-phase packing materials in the neat aqueous mobile phase, the properties of an end-capped column, the dependence of capacity factors and peak shape on the concentration of counter ions, ionic strength, pH and the addition of acetonitrile and optimum conditions for enzymatic conversion of solutes to hydrogen peroxide were studied. The studied reversed-phase columns exhibit better pH stability and longer lifetimes than normal silica-based cation exchangers. Acetylcholine is an effective and sensitive test sample for the measurement of adsorption on silica support. A large sample volume was injected onto a precolumn inserted instead of an injection valve and after injection the solutes were focused and separated on an analytical column with a mobile phase containing tetramethylammonium perchlorate as the counter ion.

Acetonitriles↗