SEARCH · PubMed Health

Results for “phasing”

Explore indexed PubMed citations for clinical trials, systematic reviews and public health research. Read source abstracts and follow each citation to its original PubMed record.

Quote a phrase for an exact phrase match. Source license links do not imply unrestricted reuse.

At least 145 records · Page 8Linked to original sources

PubMed1999

Effects of electrostatic interaction on the phase stability and structures of cubic phases of monoolein/oleic acid mixture membranes.

To elucidate effects of electrostatic interactions due to the surface charges on structures and phase stability of cubic phases of lipids, the mixture membranes of monoolein (MO) and oleic acid (OA) (OA/MO membrane) have been investigated by small-angle X-ray scattering method. As increasing OA concentration in the OA/MO membrane, a phase transition from Q(224) to Q(229) phase occurred, and above 1.0 mol% OA, OA/MO membranes were in the Q(229) phase. However, when NaCl concentration in the bulk phase is large, the Q(224) phase is more stable than the Q(229) phase in the OA/MO membranes containing high concentrations of OA. These results indicate that the electrostatic repulsion between the headgroups of these membranes makes the Q(229) phase more stable than the Q(224) phase. We have also found that lowering pH induces a phase transition from Q(229) to Q(224), and at lower pH a phase transition from Q(224) to H(II). These results are discussed in terms of the spontaneous curvature of the monolayer membrane and a lipid packing parameter of the membrane.

Glycerides↗

PubMed1994

Studies of the thermotropic phase behavior of phosphatidylcholines containing 2-alkyl substituted fatty acyl chains: a new class of phosphatidylcholines forming inverted nonlamellar phases.

We have synthesized a number of 1,2-diacyl phosphatidylcholines with hydrophobic substituents adjacent to the carbonyl group of the fatty acyl chain and studied their thermotropic phase behavior by differential scanning calorimetry, 31P-nuclear magnetic resonance spectroscopy, and x-ray diffraction. Our results indicate that the hydrocarbon chain-melting phase transition temperatures of these lipids are lower than those of the n-saturated diacylphosphatidylcholines of similar chain length. In the gel phase, the 2-alkyl substituents on the fatty acyl chains seem to inhibit the formation of tightly packed, partially dehydrated, quasi-crystalline bilayers (Lc phases), although possibly promoting the formation of chain-interdigitated bilayers. In the liquid-crystalline state, however, these 2-alkyl substituents destabilize the lamellar phase with respect to one or more inverted nonlamellar structures. In general, increases in the length, bulk, or rigidity of the alkyl substituent result in an increased destabilization of the lamellar gel and liquid-crystalline phases and a greater tendency to form inverted nonlamellar phases, the nature of which depends upon the size of the 2-alkyl substituent. Unlike normal non-lamella-forming lipids such as the phosphatidylethanolamines, increases in the length of the main acyl chain stabilize the lamellar phases and reduce the tendency to form nonlamellar structures. Our results establish that with a judicious choice of a 2-alkyl substituent and hydrocarbon chain length, phosphatidylcholines (and probably most other so-called "bilayer-preferring" lipids) can be induced to form a range of inverted nonlamellar structures at relatively low temperatures. The ability to vary the lamellar/nonlamellar phase preference of such lipids should be useful in studies of bilayer/nonbilayer phase transitions and of the molecular organization of various nonlamellar phases. Moreover, because the nonlamellar phases can easily be induced at physiologically relevant temperatures and hydration levels while avoiding changes in polar headgroup composition, this new class of 2-alkyl-substituted phosphatidylcholines should prove valuable in studies of the physiological role of non-lamella-forming lipids in reconstituted lipid-protein model membranes.

Biophysical Phenomena↗

PubMed2000

Mechanisms of phase behaviour and protein partitioning in detergent/polymer aqueous two-phase systems for purification of integral membrane proteins.

Detergent/polymer aqueous two-phase systems are studied as a fast, mild and efficient general separation method for isolation of labile integral membrane proteins. Mechanisms for phase behaviour and protein partitioning of both membrane-bound and hydrophilic proteins have been examined in a large number of detergent/polymer aqueous two-phase systems. Non-ionic detergents such as the Triton series (polyoxyethylene alkyl phenols), alkyl polyoxyethylene ethers (C(m)EO(n)), Tween series (polyoxyethylene sorbitol esters) and alkylglucosides form aqueous two-phase systems in mixtures with hydrophilic polymers, such as PEG or dextran, at low and moderate temperatures. Phase diagrams for these mixtures are shown and phase behaviour is discussed from a thermodynamic model. Membrane proteins, such as bacteriorhodopsin and cholesterol oxidase, were partitioned strongly to the micelle phase, while hydrophilic proteins, BSA and lysozyme, were partitioned to the polymer phase. The partitioning of membrane protein is mainly determined by non-specific hydrophobic interactions between detergent and membrane protein. An increased partitioning of membrane proteins to the micelle phase was found with an increased detergent concentration difference between the phases, lower polymer molecular weight and increased micelle size. Partitioning of hydrophilic proteins is mainly related to excluded volume effects, i.e. increased phase component size made the hydrophilic proteins partition more to the opposite phase. Addition of ionic detergent to the system changed the partitioning of membrane proteins slightly, but had a strong effect on hydrophilic proteins, and can be used for enhanced separation between hydrophilic proteins and membrane protein.

Detergents↗

PubMed1986

Phase equilibria of membrane lipids from Acholeplasma laidlawii: importance of a single lipid forming nonlamellar phases.

A basis for the reorganization of the bilayer structure in biological membranes is the different aggregate structures formed by lipids in water. The phase equilibria of all individual lipids and several in vivo polar lipid mixtures from acyl chain modified membranes of Acholeplasma laidlawii were investigated with different NMR techniques. All dioleoyl (DO) polar lipids, except monoglucosyldiglyceride (MGDG), form lamellar liquid crystalline (L alpha) phases only. The phase diagram of DOMGDG reveals reversed cubic (III), reversed hexagonal (HII), and L alpha phases. In mixtures of DOMGDG and dioleoyldiglycosyldiglyceride (DODGDG), the formation of an III (or HII) phase is enhanced by DOMGDG and low hydration or high temperatures. For in vivo mixtures of all polar DO lipids, a transition from an L alpha to an III phase is promoted by low hydration or high temperatures (50 degrees C). The phospholipids are incorporated in this III phase. Likewise, III and HII phases are formed at similar temperatures in a series of in vivo mixtures with different extents of acyl chain unsaturation. However, their melting temperatures (Tm) vary in an expected manner. All cubic and hexagonal phases, except the III phase with DOMGDG, exist in equilibrium with excess water. The maximum hydration of MGDG and DGDG is similar and increases with acyl chain unsaturation but is substantially lower than that for, e.g., phosphatidylcholine. The translational diffusion of the lipids in the cubic phases is rapid, implying bicontinuous structures. However, their appearances in freeze-fracture electron microscope pictures are different. The III phase of DOMGDG belongs to the Ia3d space group.(ABSTRACT TRUNCATED AT 250 WORDS)

Acholeplasma laidlawii↗

PubMed1987

Evidence for the existence of three or more slow phases in the refolding of ribonuclease A and some characteristics of the phases.

The slow refolding kinetics of RNase A have been analyzed, by using a nonlinear least-squares program for deconvoluting the kinetic phases and applying statistical tests for quality of fit. It is found that a minimum of three slow phases are required to fit the kinetic data properly, and this is true whether the method of detection is absorbance of fluorescence. Since the number of phases and the relaxation times for each phase are independent of the method of detection, it is concluded that the same three rate-limiting processes are seen by absorbance and fluorescence. These phases correspond to the XY, CT, and ct phases described in our earlier studies. The fact that fluorescence-detected kinetics are somewhat slower than absorbance-detected kinetics is a trivial effect due not to differences in relaxation times but to the fact that the amplitude of the CT phase is enhanced in fluorescence measurements, at the expense of the faster XY phase, because of intrinsic fluorescence changes associated with the isomerization of proline-93. By use of a new double-jump technique [Schmid, F.X., Grafl, R., Wrba, A., & Beintema, J.J. (1986) Proc. Natl. Acad. Sci. U.S.A. 83, 872], it is shown that proline-93 isomerizes as the rate-limiting step in only one of the three phases, the CT phase, and that this phase involves only 25-30% of the RNase molecules. There is still no indication as to the molecular events that occur in the large, ammonium sulfate dependent XY phase, which is the pathway for formation of the nativelike intermediate.

Amino Acid Isomerases↗

PubMed2001

Intracellular Ca2+ signaling pathway is involved in light-induced phase advance, but may not be in phase delay, of the circadian melatonin rhythm in chick pineal cell.

Chick pineal cells have photoreceptive, circadian clock and melatonin synthetic capacities, and express circadian oscillation of melatonin release in vitro. Light pulses cause phase-dependent phase shift of the melatonin rhythm. The purpose of this study was to address the questions whether intracellular calcium is involved in both light-induced phase advance and delay. Thapsigargin and cyclopiazonic acid, which deplete the intracellular calcium stores, blocked the light-induced phase advance in a dose-dependent manner. The pulses of ryanodine receptor antagonist (dantrolene sodium or ruthenium red) also blocked the light-induced phase advance. Most agents did not cause a significant phase shift by themselves. On the other hand, all the agents used, failed to block the light-induced phase delay, even if the magnitude of phase delay was decreased using low intensity light. An antagonist of nitric oxide synthase blocked neither light-induced phase advance nor phase delay. These results indicate the following possibilities: (1) the mechanism of light-induced phase advance and delay may be different in chick pineal cells, or (2) if intracellular calcium is involved in both light-induced phase advance and delay, the sensitivity to light and/or agents used in this study may differ according to Zeitgeber time.

Animals↗

PubMed1986

The dynamics of phase partition. A study of parameters affecting rat liver organelle partitioning in aqueous two-polymer phase systems.

Separation of subcellular organelles by two-phase partition is thought to reflect differential partition of the organelles between the two phases or between one of the phases and the interface. Studies by Fisher and colleagues [Fisher & Walter (1984) Biochim. Biophys. Acta 801, 106-110] suggest that cell separation by phase partition is a dynamic process in which the partition changes with time. This is mainly due to association of the cells with sedimenting droplets of one phase in the bulk of the other. Rat liver organelle partition was studied to determine whether the same dynamic behaviour is observed. Partition was clearly time-dependent during 24 h at unit gravity, and was also affected by altering the volume ratio of the two phases and the duration of phase mixing. These results indicate that, as with cells, the partition of organelles between phases is a dynamic process, and is consistent with the demonstration that organelles adhere to the phase droplet surfaces. Optimization of the volume ratio between phases may lead to significant processing economies. Organelle sedimentation in the upper phase was significantly faster than in the isoosmotic sucrose. Theoretical modelling of apparent organelle sizes indicates that aggregation occurs in the poly(ethylene glycol)-rich upper phase. This phenomenon is likely to limit the use of this technique in organelle separations unless means can be found to decrease aggregation.

Acetylglucosaminidase↗

PubMed1990

Phorbol-ester-induced down-regulation of protein kinase C in mouse pancreatic islets. Potentiation of phase 1 and inhibition of phase 2 of glucose-induced insulin secretion.

The influence of down-regulation of protein kinase C on glucose-induced insulin secretion was studied. A 22-24 h exposure of mouse pancreatic islets to the phorbol ester 12-O-tetradecanoylphorbol 13-acetate (TPA; 0.16 microM) in RPMI 1640 culture medium (8.3 mM-glucose, 0.43 mM-Ca2+) abolished TPA (0.16 microM)-induced insulin secretion and led to a potentiation of phase 1 and a decrease in phase 2 of glucose-induced insulin secretion. Thus, although the total insulin release during 40 min of perfusion with glucose (16.7 mM) (45-85 min) was unaffected, the percentage released during phase 1 (45-55 min) was increased from 12.9 +/- 1.5 (4)% in controls to 35.8 +/- 3.9 (4)% in TPA-treated islets (P less than 0.01), and the percentage released during phase 2 (65-85 min) was decreased from 63.2 +/- 3.9 (4)% to 35.3 +/- 1.4 (4)% (P less than 0.005). In contrast, TPA exposure in TCM 199 medium (5.5 mM-glucose, 1.26 mM-Ca2+) caused a total abolition of both phases 1 and 2 of glucose-induced secretion. However, inclusion of the alpha 2-adrenergic agonists adrenaline (10 microM) or clonidine (10 microM), or lowering of the Ca2+ concentration in TCM 199 during down-regulation, preserved and potentiated phase 1 of glucose-induced secretion. Furthermore, perifusion of islets in the presence of staurosporine (1 microM), an inhibitor of protein kinase C, potentiated phase 1 and inhibited phase 2 of glucose-induced secretion. In addition, down-regulation of protein kinase C potentiated phase 1 and inhibited phase 2 of carbamoylcholine (100 microM)-induced insulin secretion at 3.3 mM-glucose, and abolished the potentiating effect of carbamoylcholine (100 microM) at 16.7 mM-glucose. These results substantiate a role for protein kinase C in insulin secretion, and suggest that protein kinase C inhibits phase 1 and stimulates phase 2 of both glucose-induced and carbamoylcholine-induced insulin secretion.

Alkaloids↗

PubMed2002

First phase viral kinetic parameters as predictors of treatment response and their influence on the second phase viral decline.

It has recently been shown that upon initiation of interferon (IFN) treatment there is a biphasic decline in hepatitis C virus (HCV) RNA levels. In preliminary results, the rate of second phase viral decline has been shown to be an excellent predictor of treatment response. In this analysis, we determined whether the first phase viral kinetic parameters affected the rate of second phase viral decline. We also assessed whether first phase viral kinetic parameters could be used to predict treatment response within 24 h of initiating treatment. This study is a retrospective analysis of two completed studies from which detailed kinetic data were obtained in patients infected with genotype 1 HCV. In both studies, viral levels were measured frequently over the first 24 h, allowing the determination of IFNs effectiveness in blocking viral production and the viral load at the end of the first phase (v1). The second phase decline slope was calculated by log-linear regression on measurements of serum HCV RNA during days 2, 7 and 14. In study one, sustained viral response (SVR) rates were obtained, allowing the determination of the first phase's predictive power for SVR. Logistic regression and fisher exact tests were used to analyse data. In study one, no patient achieved SVR without an IFN effectiveness greater than 98% and a V1 less than 250 000 copies/mL. When V1 and IFN effectiveness were combined to predict SVR, a negative predictive value= 100%, positive predictive value=71% and accuracy of 95% was obtained after only 24 h of IFN treatment. Both studies illustrated strong correlations for both IFN effectiveness and V1 with the rate of 2nd phase slope (P < 0.001). V1 also correlated significantly with a calculation of infected cell loss (delta), which is a major determinant of the second phase viral decline. These results suggest that early viral kinetics may predict lack of response after only 24 h of treatment initiation and indicate a strong link between the degree of viral load reduction during the first phase, and the subsequent 2nd phase decline slope. This might be explained by a viral dynamics model assuming a jump-start of the immune response when viral loads are reduced below a threshold, subsequently giving rise to a faster 2nd phase decline slope.

Antiviral Agents↗

PubMedDate not supplied

Two-phase helical CT for detection of early gastric carcinoma: importance of the mucosal phase for analysis of the abnormal mucosal layer.

PURPOSE: To evaluate the efficacy of two-phase dynamic helical computed tomography (CT), including the gastric mucosal phase, for detection of early gastric carcinoma with typical hyperattenuating and atypical nonhyperattenuating enhancement patterns. METHOD: Two-phase helical CT scanning was performed using the water-filling method as negative oral contrast material for 212 patients with proven adenocarcinoma on endoscopic biopsy. Two gastrointestinal radiologists prospectively analyzed the focal alterations of the inner hyperattenuating mucosal layer and the outer hypoattenuating layer before the information obtained at barium study and pathologic examination was available. The first, so-called mucosal phase was obtained at 38-45 seconds after the start of intravenous injection of contrast material for a total of 150 ml/sec at a rate of 4 ml/sec to obtain maximum enhancement of the inner mucosal layer. The second delayed phase was obtained at 3 minutes. RESULTS: Fifty-four cases of early gastric cancer were suspected on two-phase helical CT preoperatively. Postoperatively, 49 cases of early gastric cancer were pathologically confirmed. The detection rate for the typical hyperattenuating early gastric cancer, that is the type I enhancement pattern defined as the localized thickening of the inner hyperattenuating layer, using two-phase helical CT was 18% (9/49 patients). The type 2 enhancement pattern, defined as the focal interruption of the inner hyperattenuating mucosal layer without abnormal enhancement of the outer hypoattenuating layer on the mucosal phase, was seen in 15 cases. These were pathologically confirmed as early gastric cancer IIb + IIc (three patients), IIc (four patients), IIc + IIa (one patient), IIc + III (three patients), IIb + IIc (one patient), and advanced cancer (T2) lesions (three patients). The type 3 enhancement pattern was defined as the focal polypoid protrusion of the inner hyperattenuating layer without abnormal enhancement of the outer thickened hypoattenuating layer on the mucosal phase, and was seen in seven patients who were pathologically confirmed with early gastric cancer IIb + IIc (three patients), IIc + IIa (one patient), and IIc + lIb (three patients). The lesions became less distinct on the delayed phase. Five T2 advanced gastric cancers were falsely interpreted as early gastric cancer. The detection rate for early gastric cancer after considering type 2 and 3 atypical enhancement patterns was increased to 57% (28/49 patients). CONCLUSION: Helical CT with two-phase scan including the mucosal phase was efficient for identifying the enhancement patterns of early gastric cancer.

Adenocarcinoma↗

PubMed2002

Theory of bent-core liquid-crystal phases and phase transitions.

We study phases and phase transitions that can take place in the recently discovered bow-shaped or bent-core liquid-crystal molecules. We show that to completely characterize phases exhibited by such bent-core molecules a third-rank tensor T(ijk) order parameter is necessary in addition to the vector and the nematic (second-rank) tensor order parameters. We present an exhaustive list of possible liquid phases, characterizing them by their space-symmetry group and order parameters, and catalog the universality classes of the corresponding phase transitions that we expect to take place in such bent-core molecular liquid crystals. In addition to the conventional liquid-crystal phases such as the nematic phase, we predict the existence of other liquid phases, including the spontaneously chiral nematic (N(T)+2)(*) and chiral polar (V(T)+2)(*) phases, the orientationally ordered but optically isotropic tetrahedratic T phase, and a nematic N(T) phase with D(2d) symmetry that is neither uniaxial nor biaxial. Interestingly, the isotropic-tetrahedratic transition is continuous in mean-field theory, but is likely driven first order by thermal fluctuations. We conclude with a discussion of smectic analogs of these phases and their experimental signatures.

Journal Article↗

PubMed2005

Structure solution in binary systems under high pressure: phase decomposition and phase synthesis.

There are binary systems (compounds) for which no structural solution can be found for a new high-pressure state by assuming a single phase. In accordance with Gibb's phase rule, an additional variable--composition--leads to an additional degree of freedom for a binary system (one more than in a one-component system). Although the bulk composition of a system may remain fixed, compositional variation between phases should be taken into account when considering phase transitions under pressure in binary compounds. This approach allows for a binary system the following kinds of phase transitions that are not possible in a one-component system: (i) phase (compound) decomposition into two phases with different compositions; (ii) phase synthesis from two initial phases; and (iii) phase separation from an initial phase into phases of different compositions. Examples of these kinds of high-pressure transformations and structure solution are given for the following binary systems: In-Bi, In-Sn, Hg-Sn, Cd-Sb and Sn-Bi.

Journal Article↗

PubMed2006

FljA-mediated posttranscriptional control of phase 1 flagellin expression in flagellar phase variation of Salmonella enterica serovar Typhimurium.

Flagellar phase variation of Salmonella is a phenomenon where two flagellin genes, fliC (phase 1) and fljB (phase 2), are expressed alternately. This is controlled by the inversion of a DNA segment containing the promoter for the fljB gene. The fljB gene constitutes an operon with the fljA gene, which encodes a negative regulator for fliC expression. Previous biochemical analysis suggested that phase variation might depend on alternative synthesis of phase-specific flagellin mRNA (H. Suzuki and T. Iino, J. Mol. Biol. 81:57-70, 1973). However, recently reported results suggested that FljA-dependent inhibition might be mediated by a posttranscriptional control mechanism (H. R. Bonifield and K. T. Hughes, J. Bacteriol. 185:3567-3574, 2003). In this study, we reexamined the mechanism of FljA-mediated inhibition of fliC expression more carefully. Northern blotting analysis revealed that no fliC mRNA was detected in phase 2 cells. However, only a moderate decrease in beta-galactosidase activity was observed from the fliC-lacZ transcriptional fusion gene in phase 2 cells compared with that in phase 1 cells. In contrast, the expression of the fliC-lacZ translational fusion gene was severely impaired in phase 2 cells. The half-life of fliC mRNA was shown to be much shorter in phase 2 cells than in phase 1 cells. Purified His-tagged FljA protein was shown to bind specifically to fliC mRNA and inhibit the translation from fliC mRNA in vitro. On the basis of these results, we propose that in phase 2 cells, FljA binds to fliC mRNA and inhibits its translation, which in turn facilitates its degradation.

Bacterial Proteins↗

PubMed2003

Exercise elicits phase shifts and acute alterations of melatonin that vary with circadian phase.

To examine the immediate phase-shifting effects of high-intensity exercise of a practical duration (1 h) on human circadian phase, five groups of healthy men 20-30 yr of age participated in studies involving no exercise or exposure to morning, afternoon, evening, or nocturnal exercise. Except during scheduled sleep/dark and exercise periods, subjects remained under modified constant routine conditions allowing a sleep period and including constant posture, knowledge of clock time, and exposure to dim light intensities averaging (+/-SD) 42 +/- 19 lx. The nocturnal onset of plasma melatonin secretion was used as a marker of circadian phase. A phase response curve was used to summarize the phase-shifting effects of exercise as a function of the timing of exercise. A significant effect of time of day on circadian phase shifts was observed (P < 0.004). Over the interval from the melatonin onset before exercise to the first onset after exercise, circadian phase was significantly advanced in the evening exercise group by 30 +/- 15 min (SE) compared with the phase delays observed in the no-exercise group (-25 +/- 14 min, P < 0.05). Phase shifts in response to evening exercise exposure were attenuated on the second day after exercise exposure and no longer significantly different from phase shifts observed in the absence of exercise. Unanticipated transient elevations of melatonin levels were observed in response to nocturnal exercise and in some evening exercise subjects. Taken together with the results from previous studies in humans and diurnal rodents, the current results suggest that 1) a longer duration of exercise exposure and/or repeated daily exposure to exercise may be necessary for reliable phase-shifting of the human circadian system and that 2) early evening exercise of high intensity may induce phase advances relevant for nonphotic entrainment of the human circadian system.

Adult↗

PubMed1989

Phase determination of the circadian rhythm of conidiation in heterocaryons between two out-of-phase mycelia in Neurospora crassa.

Neurospora grows vegetatively as a syncytium in which multiple nuclei exist within a connected cytoplasm. Because of the ability of separate and distinct mycelia to fuse, the possibility exists of generating heterocaryotic cultures in which the nuclei and cytoplasms of two different strains are comingled into the same syncytium. We have used such heterocaryons, in which the component parts differed with respect to their circadian clock phase, to examine whether or not clock-dominant phases exist in the circadian cycle. To this end, the phase subsequent to the formation of heterocaryons by pairs of mycelial discs that are initially at different circadian phases was examined in Neurospora crassa. The resulting phase was an average of the parent phases in many cases, but was sometimes observed to correspond more closely to just one of the original parental phases. In these cases, we did not observe any dominant phases in the circadian cycle; the phase of a particular parent disc was more dominant in the heterocaryon when the proportion of the nuclei from that parent was greater in the heterocaryon. In some instances, which occurred mostly when the difference in phase of the parental discs was large, the resultant phase could not be related in a simple way to the parental phases. An interpretation based on a limit cycle model of the circadian oscillation is possible.

Cell Cycle↗

PubMed2000

[Retention behavior of some polycyclic aromatic hydrocarbons on alkylphosphonate-modified magnesia-zirconia composite stationary phase for reversed-phase liquid chromatography].

An alkylphosphonate-modified magnesia-zirconia composite stationary phase (PZMS) for reversed-phase liquid chromatography was prepared. The reversed-phase chromatographic performance of the new packing material was investigated with some polycyclic aromatic hydrocarbons (PAHs) as solutes. The effect of the methanol content in the mobile phase on the retention of PAHs was examined. The logarithmic capacity factor of PAHs was decreased linearly with increasing volume percent of the methanol in the mobile phase, which is similar to that observed on Zorbax ODS. The capacity factor of PAHs on the new stationary phase was also correlated to their partition coefficient between n-octanol and water (log P). A good linear relationship between them was obtained. These results show that the new material can behave as a reversed-phase packing. The separations of phenanthrene and anthracene, and terphenyl isomers were investigated on the new stationary phase and the Zorbax ODS, respectively. The retention of the solutes on the Zorbax ODS is greater than that on the new stationary phase, but the separation selectivity of the solutes on the new stationary phase is better than that on the Zorbax ODS. The better separation selectivity on the new stationary phase may be contributed from the Lewis acid-base interaction between the solutes and the residual Lewis acid sites on the stationary phase.

Alkylation↗

PubMed2005

Transfer doublet and an elaborated phase plate holder for 120 kV electron-phase microscope.

A Zernike-type phase plate, which consisted of an amorphous carbon film, was developed for a 120 kV transmission electron microscope (TEM). The thickness of the film causes the scattered electrons to experience a pi/2 phase shift. The axial electrons pass through the central hole of the phase plate. The TEM was modified with an additional lens doublet, which allowed more flexibility in applying the phase plates. The doublet transfers the image from the back focal plane to a plane below the objective lens where a special phase plate holder, anticontaminator, and other necessary devices could be employed. The diameter of the central hole in the phase plate was 1 microm. The same mechanical system as in the specimen stage is used to align the axial beam into the hole. The use of a heating holder to protect the phase plate from contamination and consequential charging was investigated. Comparative diffractograms of amorphous carbon are shown with and without using a phase plate, demonstrating the change in phase contrast modulation from a sine to a cosine function when a phase plate is used. Images of biological specimens acquired using a phase plate are presented and the contrast enhancement due to the cosine transfer function is clearly demonstrated.

Animals↗

PubMed2000

Polar organic phase liquid chromatography with packed capillary columns using a vancomycin chiral stationary phase

Vancomycin immobilized on silica served as the chiral stationary phase (CSP) in this investigation with polar organic solvents as the mobile phase in liquid chromatography (LC). It was shown that trace amounts of water were beneficial for improving peak shape and efficiency. To regulate the retention and selectivity an acid and/or base were added to the mobile phase where an excess of acid was shown to be preferential for enantioseparation. An unusual increase in selectivity with increasing temperature was shown for the acidic drug, thalidomide. Additionally, nonlinear van't Hoff plots were obtained for metoprolol enantiomers that showed increased retention with increasing temperature. Metoprolol also showed unusual behavior in the polar organic phase when water was added to resemble reversed-phase chromatography, with minimum retention observed at high water or high methanol concentrations. In both instances a high degree of electrostatic interaction between metoprolol and vancomycin was concluded. Metoprolol and ten of its analogs were examined on this CSP to evaluate the enantiorecognition process. A comparison in enantioselectivity for a number of acidic and basic drugs using this CSP was also carried out using the polar organic phase, reversed phase, and normal phase LC which were all compared to the results obtained in supercritical fluid chromatography (SFC). Polar organic phase LC offered a better separation of basic molecules while reversed phase LC was preferred for the resolution of acids. SFC showed the broadest enantioselectivity overall and normal phase LC indicated similar properties, as expected, to SFC but with lower column efficiency. Copyright 2000 Wiley-Liss, Inc.

Journal Article↗