Search results for "liquid [scintillation counter]"
showing 10 items of 1764 documents
Isobaric vapor-liquid equilibria and densities for the system methyl 1,1-dimethylethyl ether+2-propanol
2002
Vapor-liquid equilibrium data at 50, 75 and 94 kPa have been determined for the binary system methyl 1,1-dimethylethyl ether + 2-propanol, in the temperature range 308-344 K. The measurements were made in an equilibrium still with circulation of both the vapor and liquid phases. Excess volumes have been also determined from density measurements using a vibrating tube densimeter at 298.15 K. The system exhibits positive deviation from ideal behavior and does not present azeotropy within the range of pressures studied. The excess volume of the system is negative over the whole mole fraction range. The activity coefficients and boiling points of the solutions were well correlated with the mole…
Hexagonal-columnar mesophases of acylated azacrowns with enhanced stabilities
1992
A series of discotic liquid crystals based on completely acylated macrocyclic oligoamines (azacrowns) has been synthesized. Discotic mesophases could be very highly stabilized by making use of an increased steric hindrance, caused by supplemental lateral meta-substituents which were introduced into the cinnamic acids used as the acylation agents. Employing this method yields compounds exhibiting hexagonal mesophases over a very broad range of more than 300°. Even if very large macrocycles are used as the core of such disc-shaped compounds, enantiotropic mesophases are achieved. Themeta-substituents as well as the size of the azacrowns were varied and their influence on the mesomorphic behav…
Interpretive search of optimal isocratic and gradient separations in micellar liquid chromatography in extended organic solvent domains
2020
Abstract Micellar liquid chromatography (MLC) is a reversed-phase mode with mobile phases containing an organic solvent and a micellised surfactant. Most procedures developed in MLC are implemented in the isocratic mode, since the general elution problem in chromatography is less troublesome. However, gradient elution may be still useful in MLC to analyse mixtures of compounds within a wide range of polarities, in shorter times. MLC using gradients is attractive to determine by direct injection moderate to low polar compounds in physiological samples. In these analyses, the use of initial micellar conditions (isocratic or gradient) with a fixed amount of surfactant above the critical micell…
Micellar Liquid Chromatography: A Worthy Technique for the Determination of β-Antagonists in Urine Samples
1998
Several beta-antagonists (acebutolol, atenolol, celiprolol, labetalol, metoprolol, nadolol, propranolol) were determined in urine samples with fluorometric detection after direct injection, in less than 15 min, with a micellar mobile phase of 0.1 M sodium dodecyl sulfate (SDS), 15% propanol, and 1% triethylamine at pH 3. The limits of detection (38 criterion) were usually between 3 and 30 ng/mL. The addition of propanol and triethylamine and the reduction of the pH of the mobile phase improved the efficiency of the chromatographic peaks that was rather low in pure micellar eluents. The selection of the composition of the mobile phase was easily performed through the use of an interpretive p…
The Use of 15N NMR for the Understanding of Nitrogen Physisorption.
1994
Abstract Nitrogen adsorption at liquid nitrogen temperature, 77K, is universally employed to determine pore dimensions. The nature of nitrogen physisorbed within the micropores of ZSM-5 zeolite was studied by in situ15N NMR as it depends on the partial pressure of the nitrogen and the temperature above and below 77K. An increase in the volume of adsorption of nitrogen at 77K occurs at a relative pressure of ~0.18 for this zeolite. The nature of the nitrogen was studied below and above this increase in nitrogen adsorption. We find that two states (phases) of nitrogen are evident. We conclude that two phases can be present but that a solid phase of nitrogen is not evident even as the temperat…
Determination of four parabens and bisphenols A, F and S in human breast milk using QuEChERS and liquid chromatography coupled to mass spectrometry
2018
Abstract For the first time, a multiresidue, sensitive and high throughput method for determination of bisphenol A, F and S and 4 parabens (methyl paraben, ethyl paraben, propyl paraben and butyl paraben) in human breast milk was developed. The proposed method includes an extraction and clean-up procedure based on QuEChERS methodology followed by liquid chromatography coupled to triple quadrupole mass spectrometry determination. Negative atmospheric pressure chemical ionization in the selected reaction monitoring mode was used for mass detection. During the method validation the recoveries varied between 83 and 115% with a precision lower than 20% for all analytes using spiked levels from 0…
New spectrophotometric procedure for determining cefotaxime based on derivatization with 1,2-naphthoquinone-4-sulphonate into solid-phase extraction …
1998
Cefotaxime was derivatised with 1,2-naphthoquinone-4-sulphonate (NQS), extracted into solid-phase cartridges (C18) and detected using a UV-visible detection system. Optimum conditions for this new procedure were: hydrogencarbonate-carbonate buffer, pH 10.5, 5-min reaction time at 25 degrees C and an NQS concentration of 7.1x10(-3) mol l(-1). The accuracy and the precision of the liquid-solid procedure were tested. The procedure was used to measure cefotaxime in pharmaceutical and urine samples. The results obtained were contrasted with those reported for a HPLC method for urine samples. The generalized H-point standard additions method was used to measure cefotaxime in urine samples.
Effect of vitrification on human oocytes: a metabolic profiling study.
2013
Objective To evaluate the effect of oocyte vitrification in the metabolomic profile of embryos developed from vitrified and fresh oocytes in our ovum donation program. Design Analysis of the metabolic profiles of spent culture medium samples corresponding to embryos developed from vitrified and fresh oocytes. Setting In vitro fertilization (IVF) unit/metabolomic facility. Patient(s) Oocyte donors between the ages of 18 and 35 years. Intervention(s) Metabolomic profile liquid chromatography coupled with mass spectrometry (LC-MS) of spent media samples. Main Outcome Measure(s) Identification of spent media components and metabolites present and absent in vitrified and fresh day-3 embryos. Res…
Development of a novel methodology for determination of dialkyl phosphates in human urine using liquid chromatography-tandem mass spectrometry
2019
Abstract In this study a fast and sensitive method was developed for the quantitative determination of six dialkyl phosphates (DAPs) in human urine using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The proposed methodology was based on liquid-liquid extraction (LLE) with diethyl ether and ethyl acetate using MgSO4 and NaCl, followed by liquid chromatography and mass spectrometry detection in the selected reaction mode (SRM) with negative electrospray ionization (ESI-). Detection settings were optimized by design of experiments (DoE). Dibutyl phosphate (DBP) was used as internal standard. Several criteria established in the SANTE/11813/2017 guidance document for pesticide resi…
Mycotoxin Analysis of Human Urine by LC-MS/MS: A Comparative Extraction Study
2017
The lower mycotoxin levels detected in urine make the development of sensitive and accurate analytical methods essential. Three extraction methods, namely salting-out liquid–liquid extraction (SALLE), miniQuEChERS (quick, easy, cheap, effective, rugged, and safe), and dispersive liquid–liquid microextraction (DLLME), were evaluated and compared based on analytical parameters for the quantitative LC-MS/MS measurement of 11 mycotoxins (AFB1, AFB2, AFG1, AFG2, OTA, ZEA, BEA, EN A, EN B, EN A1 and EN B1) in human urine. DLLME was selected as the most appropriate methodology, as it produced better validation results for recovery (79–113%), reproducibility (RSDs < 12%), and repeatability (RSDs…