Search results for "liquid"
showing 10 items of 4351 documents
Comparison of spectrophotometric and HPLC methods for determining sialic acid in infant formulas
2011
Abstract Two methods for determining sialic acid in infant formulas – spectrophotometry and HPLC with fluorescence detection – have been optimised and validated, the first one allows to determine total sialic acid while the second allows to differentiate the two main forms of sialic acid (N-acetylneuraminic acid (Neu5Ac) and N-glycolylneuraminic acid (Neu5Gc)). A common sample preparation procedure (hydrolysis and purification) for both methods has been proposed. The linearity (from 6 to 150 μg of total sialic acid in the assay for spectrophotometry, and from 12.5 to 250 ng and 1 to 5 ng of Neu5Ac and Neu5Gc, respectively, for HPLC) is adequate. The detection and quantification limits (0.29…
Rapid and simultaneous high-performance liquid chromatography assay of polyamines and monoacetylpolyamines in biological specimens
2000
A rapid, resolutive and reproducible reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed for polyamines and acetylpolyamines by adopting pre-column derivatization with benzoyl chloride. In a single run lasting less than 15 min ten polyamines were separated as well as traces of benzoic acid, methylbenzoate and benzoic anhydride. These contaminants, produced during the derivatization reaction, were almost all eliminated by washing steps envisaged in the same procedure. This simple and sensitive method can be applied to routine determination of polyamines in biological samples. A fine application of this procedure to the determination of endogenous content of p…
Separation of the enantiomers of primary and secondary amphetamines by liquid chromatography after derivatization with (−)-1-(9-fluorenyl)ethyl chlor…
2003
The chiral reagent (−)-1-(9-fluorenyl)ethyl chloroformate (FLEC) has been evaluated for the enantioselective analysis of amphetamines by liquid chromatography. For separation of the FLEC diastereomers conventional reversed-phase conditions were used. The conditions affording the best enantiomeric resolution and sensitivity were determined for amphetamine, methamphetamine, ephedrine, pseudoephedrine, 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDE). All the amphetamines assayed could be separated with resolution factors ranging from 0.91 to 1.92. Although FLEC is typically used as a fluorogenic reagent, it was shown t…
Chromium liquid waste inertization in an inorganic alkali activated matrix: Leaching and NMR multinuclear approach
2015
A class of inorganic binders, also known as geopolymers, can be obtained by alkali activation of aluminosilicate powders at room temperature. The process is affected by many parameters (curing time, curing temperature, relative humidity etc.) and leads to a resistant matrix usable for inertization of hazardous waste. In this study an industrial liquid waste containing a high amount of chromium (≈ 2.3 wt%) in the form of metalorganic salts is inertized into a metakaolin based geopolymer matrix. One of the innovative aspects is the exploitation of the water contained in the waste for the geopolymerization process. This avoided any drying treatment, a common step in the management of liquid ha…
Biopartitioning micellar chromatography to pedict mutagenicity of aromatic amines
2007
[EN] Mutagenicity is a toxicity endpoint associated with the chronic exposure to chemicals. Aromatic amines have considerable industrial and environmental importance due to their widespread use in industry and their mutagenic capacity. Biopartitioning micellar chromatography (BMC), a mode of micellar liquid chromatography that uses micellar mobile phases of Brij35 in adequate experimental conditions, has demonstrated to be useful in mimicking the drug partitioning process into biological systems. In this paper, the usefulness of BMC for predicting mutagenicity of aromatic amines is demonstrated. A multiple linear regression (MLR) model based on BMC retention data is proposed and compared wi…
Gas—liquid chromatographic analyses
1985
Abstract The gas chromatographic retention behaviour of methylethyl, 1-methylpropyl, 2-methylpropyl, 1,2-dimethylpropyl, 1-methylbutyl and 3-methylbutyl esters of benzoic and o-, m- and p-chlorobenzoic acids on low-polarity (SE-30) and polar (OV-351) capillary columns under several temperature-programmed and isothermal conditions is reported. The retention data and the Kovats retention indices for all 24 components are given and the separation of a complex mixture is discussed. The retention index increments have been used to examine the effects of chain branching and chlorine substitution. The results are compared with those for n-alkyl benzoates and monochlorobenzoates.
Application of Dopant-Assisted Atmospheric Pressure Photoionisation HPLC–MS Method for the Sensitive Determination of Polycyclic Aromatic Hydrocarbon…
2017
Multiple food research studies have shown that the polycyclic aromatic hydrocarbon (PAHs) are frequently found in processed cocoa products and chocolate. In a present study a method based on dopant-assisted atmospheric pressure photoionisation (DA-APPI) combined with a liquid chromatography/high-resolution mass spectrometer (HPLC-HRMS) for high-sensitivity analysis of four EU marker PAHs in dark chocolate samples was developed and fully validated according to the performance criteria set in EU guidelines. PAHs detection was achieved by HRMS in positive electrospray ionization mode with toluene used as a dopant to enhance the ionization efficiency of non-polar PAHs. The on-column instrument …
Extraction of polycyclic aromatic hydrocarbons from cookies: a comparative study of ultrasound and microwave-assisted procedures.
2008
The chromatographic determination of 15 polycyclic aromatic hydrocarbons (PAHs) in cookies has been improved in order to obtain a fast method with a low limit of detection through the combination of microwave-assisted extraction (MAE), oil saponification and solid-phase extraction clean-up before the injection of purified extracts in a C18 201TP52 (5 microm, 250 x 2.1 mm) column. Using acetonitrile-water as mobile phase, with a 50% to 95% w/w acetonitrile gradient for a fixed flow of 0.250 ml min(-1), 15 PAHs were separated in 45 min. The column temperature was maintained at 15 degrees C; and fluorimetric detection was made at a fixed excitation wavelength of 264 nm and emission measurement…
Covalent DNA adducts formed by benzo[c]chrysene in mouse epidermis and by benzo[c]chrysene fjord-region diol epoxides reacted with DNA and polynucleo…
1997
The metabolic activation in mouse skin of benzo[c]chrysene (B[c]C), a weakly carcinogenic polycyclic aromatic hydrocarbon (PAH) present in coal tar and crude oil, was investigated. Male Parkes mice were treated topically with 0.5 mumol of B[c]C, and DNA was isolated from the treated areas of skin at various times after treatment and analyzed by 32P-postlabeling. Seven adduct spots were detected, at a maximum level of 0.89 fmol of adducts/microgram of DNA. Four B[c]C-DNA adducts persisted in skin for at least 3 weeks. Treatment of mice with 0.5 mumol of the optically pure putative proximate carcinogens (+)- and (-)-trans-benzo[c]chrysene-9,10-dihydrodiols [(+)- and (-)-B[c]C-diols] led to th…
Characterization of gramicidin A in an inverted micellar environment. A combined high-performance liquid chromatographic and spectroscopic study
1992
We have investigated the conformational adaptability of gramicidin A incorporated into reverse micelles of sodium bis(2-ethylhexyl)sulfosuccinate (AOT)/isooctane/water, a so far unexplored "host" membrane-mimetic model system for this peptide. A high-performance liquid chromatographic strategy previously developed for the study of gramicidin in phospholipid vesicles and normal micelles [Bañó et al. (1989) FEBS Lett. 250, 67; Bañó et al. (1991) Biochemistry 30, 886] has been successfully extended to this system. The method has permitted the separation of peptide conformational species, namely, double-stranded dimers and monomers, and an accurate quantitation of their proportion in the invert…