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PubMed2003

A polycatenar mesogen with a perfluorinated moiety showing continuous phase transformation between a smectic A phase and a structured, fluid, optically isotropic phase.

A polycatenar mesogen consisting of a four aromatic ring system with three long alkoxy chains and a bulky perfluorinated substituent has been synthesized and found to show the polymorphism of a cubic phase, a columnar phase and a smectic A phase, including a structured, fluid, optically isotropic phase with the phase transformation between the smectic A phase and the isotropic phase occurring continuously.

Journal Article↗

PubMedDate not supplied

Helical CT for detecting focal liver lesions in patients with breast carcinoma: comparison of noncontrast phase, hepatic arterial phase, and portal venous phase.

PURPOSE: Our goal was to compare noncontrast phase (NCP), hepatic arterial phase (HAP), and portal venous phase (PVP) helical CT for the detection of focal liver lesions in patients at risk for having metastases from breast carcinoma. METHOD: Eighty-four consecutive CT scans in 80 women with known or suspected liver metastases from breast carcinoma were prospectively evaluated with triple phase helical CT. After NCP, Isovue 300 was administered at 3 ml/s for 40 s, then 2 ml/s for 30 s, with scan delays of 25 s (HAP) and 76 s (PVP), slice thickness of 7 mm, and pitch of 1:1. Two reviewers evaluated each phase for focal liver lesions in a blinded and random fashion followed by side-by-side review for consensus. RESULTS: By consensus, 40 CT scans were normal and 44 CT scans had a total of 105 lesions (46 lesions were graded malignant). PVP detected 39 (85%), HAP 27 (59%), and NCP 28 (61%) malignant lesions. Two malignant lesions were seen only on HAP, 3 only on NCP, and 10 only on PVP. The remainder of lesions were seen on more than one phase. PVP was graded best for detecting lesions in 27 (61%), HAP best in 7 (16%), NCP best in 4 (9%), and PVP equivalent to HAP in 6 (14%) of the 44 cases with lesions. CONCLUSION: In our breast cancer patient population, PVP was superior to NCP and HAP for liver lesion detection. Because no CT scan was converted from negative to positive due to the addition of NCP or HAP, the routine use of these two phases cannot be justified when the clinical concern is the presence or absence of metastases.

Adult↗

PubMedDate not supplied

Detection of hypervascular hepatocellular carcinoma by dynamic magnetic resonance imaging with double-echo chemical shift in-phase and opposed-phase gradient echo technique: comparison with dynamic helical computed tomography imaging with double arterial phase.

PURPOSE: The technique of double-echo chemical shift gradient echo magnetic resonance imaging (MRI) with the fast low-angle shot (double-echo FLASH) sequence provides in-phase and opposed-phase images in a single breath hold. The purpose of this study was to evaluate the efficacy of dynamic MRI with double-echo FLASH imaging for the detection of hypervascular hepatocellular carcinoma by comparing it with dynamic helical computed tomography (CT) imaging with double arterial phase. MATERIALS AND METHODS: Twenty-nine patients with 67 hypervascular hepatocellular carcinoma nodules who underwent both dynamic MRI with double-echo FLASH imaging (repetition time/echo time/flip angle: 160/3.6, 7.0/80 degrees ) and dynamic helical CT imaging with double arterial phase were enrolled in the study. For dynamic MRI, precontrast, arterial, portal venous, and equilibrium phase images were obtained before and approximately 19, 60, and 120 seconds, respectively, after intravenous injection of 0.1 mmol/kg of gadopentetate dimeglumine at a rate of 2 ml/s. For dynamic CT imaging, quadraphase images, including early arterial, late arterial, portal venous, and equilibrium phases, were obtained serially approximately 20, 30, 70, and 180 seconds, respectively, after intravenous administration of 2 ml/kg of 300 mgI/ml of nonionic contrast medium at a rate of 5 ml/s. Three masked observers independently interpreted images obtained with each technique in random order, separately and without patient identifiers. Sensitivity and positive predictive values as well as the area below the alternative-free response receiver operating characteristic curve (Az) for each imaging technique were calculated and compared statistically. RESULTS: Mean sensitivity and positive predictive values of MRI for hypervascular hepatocellular carcinoma were 48% and 94%, respectively, and those of CT imaging were 47% and 91%, respectively. In 11 (38%) of the 29 patients, at least one observer judged dynamic MRI to be superior, whereas in 5 patients (17%), dynamic CT was judged to be superior. There was no significant difference in the sensitivity and positive predictive values between these techniques (p > 0.05). There was no significant difference either in mean Az values between CT (0.55) and MRI (0.57) (p = 0.61). CONCLUSION: Dynamic MRI with double-echo FLASH imaging can detect hypervascular hepatocellular carcinoma as well as dynamic helical CT imaging with double arterial phase.

Adult↗

PubMed2006

Barotropic phase transition between the lamellar liquid crystal phase and the inverted hexagonal phase of dioleoylphosphatidylethanolamine.

The phase transition between the lamellar liquid crystal (Lalpha) phase and the inverted hexagonal (H(II)) phase of dioleoylphosphatidylethanolamine (DOPE) in aqueous NaCl solutions was observed by means of differential scanning calorimetry (DSC) under ambient pressure and light-transmittance technique under high pressure. The pressure dependence of the transition temperature (dT/dp) and the thermodynamic quantities for the Lalpha/H(II) transition were compared with those of another phase transition found in the DOPE bilayer membrane, which is the transition from the lamellar crystal (Lc) phase to the Lalpha phase. The dT/dp value of the Lalpha/H(II) transition was about 3.5 times as large as that of the Lc/Lalpha transition while the thermodynamic quantities were significantly smaller than those of the latter to the contrary. Comparing the enthalpy and volume behavior of the Lalpha/H(II) transition with that of the Lc/Lalpha transition, we concluded that the Lalpha/H(II) transition can be regarded as the volume-controlled transition for the reconstruction of molecular packing.

Calorimetry, Differential Scanning↗

PubMed1990

Ethanol induces interdigitated gel phase (L beta I) between lamellar gel phase (L beta') and ripple phase (P beta') in phosphatidylcholine membranes: a scanning density meter study.

Effects of ethanol on dipalmitoylphosphatidylcholine (DPPC) and distearoylphosphatidylcholine (DSPC) dispersions were investigated with an automated scanning density meter and a differential scanning calorimeter (DSC). The temperature-dependent profile of specific volume measured by the density meter clearly exhibited phase transitions of the DPPC and the DSPC dispersions as drastic changes in the thermal expansion coefficients. On increasing the ethanol concentration in the DPPC dispersions, the pretransition temperature was reduced faster than the main transition temperature was. An interdigitated gel phase (L beta I) appeared as a region of lower specific volume at the pretransition temperature when the ethanol concentration reached 40 mg/ml. The L beta I phase spread both its ends in an ethanol-dependent fashion, and the high-temperature end merged to the main transition at 50 mg/ml of ethanol. The temperature-ethanol phase diagram has been determined for DPPC. The transitions L beta' to L beta I and from L beta I to P beta' were also observed on the thermograms of DSC measurements. In the DSPC dispersions, the L beta I phase was induced between the L beta' and the P beta' phases by a lower ethanol concentration (about 20 mg/ml).

1,2-Dipalmitoylphosphatidylcholine↗

PubMed1993

Phase transitions of reversed-phase stationary phases. Cause and effects in the mechanism of retention.

We provide a somewhat historical perspective on the work that has been accomplished that supports the suggestion of phase transitions in reversed-phase liquid chromatographic bonded phases. In addition to this general review, we consider from both a practical and theoretical viewpoint the implications of such transitions in the rational design of improved reversed-phase separations. Analytical theory and molecular simulation approaches to chromatographic stationary phases and related systems are reviewed. Initial results are presented on the temperature, density and chain length dependences of stationary phase properties. The role of computer simulation in analyzing transition behavior and retention processes is discussed.

Chemical Phenomena↗

PubMedDate not supplied

Aqueous two-phase systems containing urea: influence on phase separation and stabilization of protein conformation by phase components.

During recombinant Escherichia coli fermentation with high expression levels, inclusion bodies are often formed. Aqueous two-phase systems have been used in the presence of urea for the initial recovery steps. To investigate phase behavior of such systems we determined phase diagrams of poly(ethylene glycol) (PEG)/sodium sulfate/urea/water and PEG/dextran T-500 (DEX)/urea/phosphate buffer/water at different concentrations of urea and different molecular weight of PEG. PEG/Na2SO4 aqueous two-phase systems could be obtained including up to 30% w/w urea at 25 degrees C and PEG/dextran T-500 up to 35% w/w urea. The binodial was displaced toward higher concentrations with increasing urea concentrations. The partition coefficient of urea was near unity. An unstable mutant of T4-lysozyme with an amino acid replacement in the core (V149T) was used to analyze the effect of phase components on the conformation of the enzyme. We showed that partitioning of tryptophan was not dependent on the concentration of urea in the phase system.

Amino Acid Substitution↗

PubMed2007

Lateral phase separation gives multiple lamellar phases in a "binary" surfactant/water system: the phase behavior of sodium alkyl benzene sulfonate/water mixtures.

We have examined the structure of the lamellar phase (Lalpha) that coexists with a micellar solution (L1) for a commercial sodium alkyl benzene sulfonate (LAS) mixed with water. The surfactant is a mixture containing C10-C13 alkyl chains, having all positional isomers of the benzene sulfonate group present except the 1-isomer. Unusually for ionic surfactants, the difference in compositions between the coexisting L1 and Lalpha phases is large (L1 = approximately 20 wt % LAS; Lalpha = approximately 65 wt %). The main technique employed was X-ray diffraction, supplemented by optical microscopy and differential scanning calorimetry (DSC). At ambient temperatures, the lamellar phase gives a single diffraction pattern with the main reflection (d) at approximately 32.5 A, whatever the composition. However, above 40 degrees C, the diffraction peak becomes broader and moves to higher d values. At higher temperatures still, several distinct and different diffraction peaks are observed, differing in detail according to composition. The largest d values (approximately 42-4 A) are observed for the lowest LAS concentrations, while the largest number of separate reflections (five) occurs for samples with approximately 44-50% LAS, both at the highest temperatures. Although there are some differences in the data between heating and cooling cycles, the d values return to the original value at low temperature. There are no observable transitions in DSC, nor is there any heterogeneity in the lamellar phase observable by microscopy. The data clearly indicate that there is some lateral separation of the different LAS isomers within the bilayers, which results in the formation of local lamellar regions having different surfactant compositions. This lateral phase separation may arise from the presence of an (electrostatic) attractive interaction, which gives rise to an upper consolute loop within the lamellar phase region of a pure LAS isomer. Similar mechanisms may occur in biological membranes and could be responsible for the occurrence of membrane lipid patches.

Journal Article↗

PubMed1978

Late S phase cells (Chinese hamster ovary) induce early S phase DNA labeling patterns in G1 phase nuclei.

Cells (Chinese hamster ovary) in G1 phase were fused with cells in late S phase to determine if a cell in late S phase can induce DNA synthesis in the nucleus of a G1 cell and, if so, to determine if the DNA synthesis so induced in a G1 phase nucleus has an autoradiographic pattern characteristic of early or of late S phase synthesis. The results indicate (i) that 89% of the G1 nuclei in late-S/G1 binucleates synthesized DNA, while only 2% of the control unfused G1 cells synthesized DNA, and (ii) that in all late-S/G1 binucleates the G1 nucleus was induced to synthesize early S phase DNA. These results are compatible with the idea that a cytoplasmically transmissible factor initiates DNA synthesis but that an intranuclear mechanism defines the temporal order of replication.

Cell Cycle↗

PubMed1995

Direct-space methods in phase extension and phase determination. III. Phase refinement using Sayre's equation.

An algorithm is described for refining a set of phases to agree with the Sayre equation. All operations are carried out using Fourier transforms with modest computer-store requirements even for very large systems. The procedure is tested with two moderate-sized proteins, one containing heavy atoms, and is found to give good refinement with data at more than atomic resolution (1.17 A) and useful, if less good, refinement when the data resolution is lower (1.5 A). It is concluded that at atomic resolution, or slightly below, the Sayre equation still has something to offer both for phase refinement and phase extension, especially if used cautiously with weighted multiple isomorphous replacement phases acting as a constraint on the phase changes. Even when the Sayre equation on its own refines phases badly, or not at all, it may still make an important contribution in conjunction with other real-space refinement procedures.

Journal Article↗

PubMed1997

Two distinct epithelial responses may compensate for the ureteral obstruction in early and late phase of unilateral ureteral obstruction-treated rat: cellular proliferation in acute phase and osteopontin expression in chronic phase.

In order to clarify cellular responses in dilated renal tubules in the acute and chronic phase of ureteral obstruction, we investigated the expression of proliferating cell nuclear antigen and osteopontin (OPN) in unilateral ureteral obstruction (UUO)-treated rat kidneys. The results showed that renal epithelial cells proliferate in association with tubular dilatation to compensate for the ureteral obstruction in the acute phase of UUO while the proliferative activity decreases in the chronic phase. In the chronic phase, however, the expression of OPN was up-regulated in various tubules but not associated with the tubular dilatation. Taken together with its chemoattractant activity for macrophage, OPN may be involved in the interstitial fibrosis as another compensatory mechanism in the chronic phase of ureteral obstruction. Therefore, these results suggest that two distinct epithelial responses may compensate for the ureteral obstruction in the acute and chronic phase of UUO-treated rat, respectively.

Acute Disease↗

PubMed2003

Phase-shift extraction and wave-front reconstruction in phase-shifting interferometry with arbitrary phase steps.

A new approach to reconstructing the object wave front in phase-shifting interferometry with arbitrary unknown phase steps is proposed. With this method the actual phase steps are first determined from measured intensities with an algorithm based on the statistic property of the object phase distribution in the recording plane. Then the original object field is calculated digitally with a derived formula. This method is simple, accurate, and capable of retrieving the original object field, including its amplitude and phase distributions simultaneously, with arbitrary and unequal phase steps in a three- or four-frame method. The effectiveness and correctness of this approach are verified by a series of computer simulations for both smooth and diffusing surfaces.

Journal Article↗

PubMed2003

Defective S phase chromatin assembly causes DNA damage, activation of the S phase checkpoint, and S phase arrest.

The S phase checkpoint protects the genome from spontaneous damage during DNA replication, although the cause of damage has been unknown. We used a dominant-negative mutant of a subunit of CAF-I, a complex that assembles newly synthesized DNA into nucleosomes, to inhibit S phase chromatin assembly and found that this induced S phase arrest. Arrest was accompanied by DNA damage and S phase checkpoint activation and required ATR or ATM kinase activity. These results show that in human cells CAF-I activity is required for completion of S phase and that a defect in chromatin assembly can itself induce DNA damage. We propose that errors in chromatin assembly, occurring spontaneously or caused by genetic mutations or environmental agents, contribute to genome instability.

Ataxia Telangiectasia Mutated Proteins↗

PubMed2000

Adsorption/partition model of liquid chromatography for chemically bonded stationary phases of the aliphatic cyano, reversed-phase C8 and reversed-phase C18 types.

A novel approach was introduced to modeling solute retention in the liquid chromatography systems, employing silica-based aliphatic chemically bonded stationary phases of the cyano, reversed-phase C8 and reversed-phase C18 types, and the mixed binary eluents most frequently used in the reversed-phase and normal-phase chromatography modes (i.e. using the methanol-water and the 2-propanol-n-hexane liquid mixtures, respectively). This approach takes notice of the mixed (adsorption/partition) mechanism of solute retention, in which both, the adsorptive and the dispersive forces contribute to the overall energetics of this process. Performance of our new model was compared with that of the widely recognized and on a routine basis applied Schoenmakers approach, and it was found out that both models perform with a practically equal and outstanding accuracy.

Chromatography, Liquid↗

PubMed1991

LC-MS compatible HPLC separation for xenobiotics and their phase I and phase II metabolites: simultaneous anion exchange and reversed-phase chromatography.

Benzene and five of its mammalian metabolites, phenol, phenyl-beta-D-glucuronide, phenylsulfate, phenylmercapturate, and t,t-muconic acid, are separated on a methylstyrene-divinylbenzene-based anion exchange--reversed-phase column. The retention of the model compounds is manipulated by modifying the type, ionic strength, and pH of the mobile phase buffer, and the type and percent of organic mobile phase modifier. The separations developed are compatible with both particle beam (PB) and thermospray (TSP) interfaces used in liquid chromatography-mass spectrometry (LC-MS). These separations should be adaptable to the study of a wide range of xenobiotics and their phase I and phase II metabolites, and provide an LC-MS compatible alternative to the use of iron pairing reagents.

Benzene↗

PubMed2004

Comment on "Phase-shift extraction and wave-front reconstruction in phase-shifting interferometry with arbitrary phase steps".

We comment on the recent Letter by Cai et al. [Opt. Lett. 28, 1808 (2003)] in which an approach to phase-shifting interferometry with arbitrary phase steps was proposed. Cai et al. based their method of phase shifting on the idea that the intensities of the reference and object beams can be measured previously, which actually makes the whole posterior phase-shifting procedure absolutely unnecessary. Their method is also based on the statement that the phase of the Fresnel diffraction pattern of a test object if generally a spatially random distribution, which in most situations is wrong.

Comment↗

PubMed2006

The enantioseparation of amino acids on a teicoplanin chiral stationary phase using non-aqueous mobile phases after pre-column derivatization with sulfur-containing reagents: the considerations of mobile phase composition and analyte structure variation on resolution enhancement.

Amino acids were derivatized with sulfur-containing reagents in alkaline medium and enantioresolved by HPLC on a teicoplanin chiral stationary phase. Much better resolution was achieved using methanol-based mobile phase compared with elution with acetonitrile-based solvent mixture. The value of selectivity factor for many derivatives examined in the study can be easily several tenths of 100 or even exceed 100 in some cases. This magnitude of resolution is suitable for the preparative-scale application of isolating alpha-amino acid enantiomers in the derivatized form using a short column. The resolution is believed to be a result of the hydrogen bonding and steric hindrance by the nitrogen and sulfur atoms from the isothiocyanatyl fragment of the reagent, respectively, and is enhanced as the fragment is structurally phenylated (e.g. 2,4-difluorophenyl isothiocyanate and others examined in this study). The enhancement is even more significant if the aromatic moiety of the reagent becomes more acidic through halogenation with chlorine or fluorine for the stronger pi-pi interaction. However, this type of enhancement is offset to some extent and sometimes obscured by a chlorinated reagent that is relatively large in size as compared with the fluorinated one. Judging from the chromatographic data and the elution profile, the mechanisms leading to the resolutions are believed to be different under the elution of polar-organic mobile phases (i.e. methanol- and acetonitrile-based mobile phases).

Amino Acids↗

PubMed1984

Bare silica as a reverse-phase stationary phase: liquid chromatographic separation of antihistamines with buffered aqueous organic mobile phases.

Unbonded silica gel is an effective support for reverse-phase liquid chromatographic separations of lipophilic amines. Simple buffered aqueous-organic mobile phases provide rapid isocratic separations of antihistamines. Phenylpropanolamine hydrochloride, chlorpheniramine maleate, and dextromethorphan hydrobromide are separated in 8 min on bare silica with a mobile phase of 75% methanol and 25% water which is 0.01 M in (NH4)2HPO4. Quantitation is reproducible. A wide variety of additional compounds may be separated using the same mobile phase.

Chromatography, Liquid↗