Biomedical subjects

J J Jiménez

Publications and source records attributed to J J Jiménez.

At least 19 recordsLinked to original sources

PubMed2006

Sample preparation methods for beeswax characterization by gas chromatography with flame ionization detection.

New and simpler methods of sample preparation to determine several families of compounds in beeswax by conventional and high temperature gas chromatography are proposed. To analyze hydrocarbons and palmitates, a dilution of sample is enough whereas for the total acid content, a hydrolysis and simultaneous methylation with BF3-methanol results more effective than the usual methods; for the total content of alcohols, a further acetylation with acetic anhydride is necessary. Free alcohols are directly acetylated in a sample dissolution but for free acids and monoesterified 1,2,3-propanetriols analysis, a previous extraction with acetonitrile is required. The concentrations of all the compounds studied are expressed in weight percentage referred only to one standard: octadecyl octadecanoate. The precision of the analytical methods has been evaluated showing its importance in the analysis of beeswaxes used in apiculture.

Alcohols↗

PubMed2006

Trace analysis of tiamulin in honey by liquid chromatography-diode array-electrospray ionization mass spectrometry detection.

A liquid chromatography with diode array or electrospray ionisation mass spectrometry detection (LC-DAD-ESI-MS) method for the determination of tiamulin residues in honey is presented. The procedure employs a solid-phase extraction (SPE) on polymeric cartridges for the isolation of tiamulin from honey samples diluted in aqueous solution of tartaric acid. Chromatographic separation of the tiamulin is performed, in isocratic mode, on a C18 column using methanol and ammonium carbonate 0.1% in water, in proportion (30:70, v/v). Average analyte recoveries were from 88 to 106% in replica sets of fortified honey samples. The LC-ESI-MS method detection limits differ from 0.5 microg kg(-1) for clear honeys to 1.2 microg kg(-1) for dark honeys. The developed method has been applied to the analysis of tiamulin residues in multifloral honey samples collected from veterinary treated beehives.

Chromatography, Liquid↗

PubMed2005

Comparative study of the enantioselective separation of several antiulcer drugs by high-performance liquid chromatography and supercritical fluid chromatography.

A comparative study of the enantiomeric separation of several antiulcer drugs such as omeprazole, lansoprazole, rabeprazole and pantoprazole using HPLC and supercritical fluid chromatography (SFC) on the Chrialpak AD column is presented in this work. The results show that employing the above mentioned column only two compounds (omeprazole and pantoprazole) could be enantiomerically resolved using HPLC, on the contrary SFC allowed the enantiomeric separation of all the compounds studied with higher resolutions and lower analysis times.

2-Propanol↗

PubMed2005

Determination of azolic fungicides in wine by solid-phase extraction and high-performance liquid chromatography-atmospheric pressure chemical ionization-mass spectrometry.

A method for simultaneous analysis of eight azolic fungicides: cyproconazole, diniconazole, tetraconazole, thiabendazole, flusilazole, triadimenol, triadimefon, carbendazim and the degradation product 2-aminobenzimidazole in wine samples is described. The compounds are isolated from the samples and concentrated by solid-phase extraction on polymeric cartridges. The determination is carried out by liquid chromatography with mass spectrometric detection in positive ionization and selected ion monitoring modes. The influence of parameters such as the mobile phase composition, column temperature, corona current and fragmentor voltage is studied and the proposed method is validated. Recoveries of the nine compounds added to wine samples range from 83 to 109%, with relative standard deviations below 10%. The quantitation limits are between 9 and 31 microg/L. Real wine samples are analyzed by the proposed method, also.

Atmospheric Pressure↗

PubMed2004

Liquid-liquid extraction followed by solid-phase extraction for the determination of lipophilic pesticides in beeswax by gas chromatography-electron-capture detection and matrix-matched calibration.

Analytical methods for the simultaneous analysis of lindane, chlorpyriphos, z-chlorfenvinphos, endosulfan A and B, 4,4'-DDE, 4,4'-TDE, acrinathrine, bromopropylate, tetradifon, coumaphos and fluvalinate in pure beeswax samples are studied. For the analysis of bleached beeswaxes, a liquid-liquid extraction with acetonitrile followed by a clean-up on polymeric cartridges is the best option in terms of recovery and precision. However, some interferences that hinder the identification and quantification of important varroacides are found when non-bleached beeswaxes are analyzed. The analysis of all compounds in the latter samples require a clean-up by coupling an ODS cartridge before the polymeric cartridge. Considerations about the influence of the matrix in the quantitative analysis by a classical external standard calibration are also made and the use of a matrix-matched calibration is advised. Recoveries resulted to be about 100% with coefficients of variation between 10% and 20% (n = 5) for concentrations of 0.5 and 5 mg/kg.

Calibration↗

PubMed2004

Chiral separation of some triazole pesticides by supercritical fluid chromatography.

The enantiomeric separation of six triazole pesticides: cyproconazole, propiconazole, diniconazole, hexaconazole, tebuconazole and tetraconazole, using supercritical fluid chromatography and the Chiralpak AD column, is presented in this work. The effect of different organic modifiers such as methanol, ethanol and 2-propanol on the retention and resolution was studied as well as the presence of additives in the mobile phase. The results obtained were highly successful, all the compounds were enantiomerically separated and in most of the cases the analysis time was close to 10 min. The type of organic modifier that provided the best results depended on the compound.

Chromatography, Supercritical Fluid↗

PubMed2004

Quality assurance of commercial beeswax. Part I. Gas chromatography-electron impact ionization mass spectrometry of hydrocarbons and monoesters.

The use of low-temperature capillary gas chromatography coupled to electron impact mass spectrometry for the characterization of crude beeswaxes yielded by Apis mellifera is described. The system allows the identification of a great number of compounds, some of them not reported till now in beeswax, such as a family of ethyl esters, tetracosyl oleate, and several saturated and unsaturated hydrocarbons. The information acquired makes possible the differentiation between pure beeswax and some foundation beeswax samples where mixture of pure beeswax with another substances is suspected.

Gas Chromatography-Mass Spectrometry↗

PubMed2004

Evaluation of new surfactant expanded zirconium and titanium phosphates for polycyclic aromatic hydrocarbons extraction from waters.

A newly synthesized family of materials prepared with surfactant as organic template were tested for the extraction of polycyclic aromatic hydrocarbons (PAHs) from water, using pyrene (Pyr) and benzo[a]pyrene (B[a]P) as PAHs representatives. Particular attention was paid to the evaluation of the recovery factors with dichloromethane as eluent in order to estimate their potential as adsorbing solid phases for PAH remediation or analysis. Eleven lamellar MCM-50 type materials incorporating n-alkyl- (n = 12, 16, 18) trimethylammonium bromide molecules with different concentrations and chain lengths and two hexagonal MCM-41 type materials incorporating octadecyl-trimethyl ammonium bromide were tested. Best results were obtained by preparing lamellar MCM-50 zirconium and titanium phosphates in the presence of n-dodecyl-trimethylammonium at a relative molar concentration (surfactant/phosphate) of 1.

Absorption↗

PubMed2003

Quality assurance of commercial beeswax II. Gas chromatography-electron impact ionization mass spectrometry of alcohols and acids.

Gas chromatography with mass spectrometric detection was used to find the fraction of alcohols and acids present in pure beeswax from Apis mellifera. Some new compounds not described till now were found, such as a family of unsaturated linear fatty acids, several hydroxyacids and 1,2,3-propanetriol monoesters. The chromatographic profiles obtained from pure beeswax and bee-rejected foundation beeswax can be used to discriminate them; they mainly differ in the amount of some acids and alcohols.

Acids↗

PubMed2002

Separation of albendazole sulfoxide enantiomers by chiral supercritical-fluid chromatography.

The enantioseparation of albendazole sulfoxide (ABZSO) by chiral supercritical-fluid chromatography (SFC) on two columns, based on the polysaccharide derivatives Chiralpak AD and Chiralcel OD, was studied. The effect of different modifiers, methanol, ethanol, 2-propanol, and acetonitrile, was examined. The results showed that ABZSO can be separated on both columns, using an alcohol-type modifier. Using the Chiralpak AD column, the best results were obtained with 2-propanol and, in the case of the Chiralcel OD, with methanol.

Acetonitriles↗

PubMed2002

Factors affecting the extraction, hydrolysis and derivatization steps for the quantitation of total residues of amitraz in honey by gas chromatography with electron capture detection.

A study about the most adequate conditions for the determination of the amitraz total residues in honey by gas chromatography is presented. Solvent and solid phase extraction procedures as well as the influence of several parameters on the extraction, hydrolysis and derivatization steps are considered. Solid phase extraction on ODS cartridges was found to be not reliable for the determination of total residues, because recovery for 2,4-dimethylaniline (DMA) was poor. Liquid-liquid extraction with hexane was accomplished in a single step and was more reproducible. The pH of the aqueous solution had to be set at pH 11 to achieve extraction of DMA. The derivatization of DMA with heptafluorobutyric anhydride (HFBA) was practically instantaneous at room temperature.

Chromatography, Gas↗

PubMed2002

Extraction of thymol, eucalyptol, menthol, and camphor residues from honey and beeswax. Determination by gas chromatography with flame ionization detection.

A gas chromatographic method to determine thymol, eucalyptol (cineole), menthol and camphor residues in honey and beeswax is proposed. To isolate the compounds, three methods involving liquid-liquid extraction with methylene chloride, distillation, or solid-phase extraction on octadecylsilica cartridges can be used. The GC separation is carried out on a 60 m x 0.53 mm Stabilwax DA capillary column, using a flame ionization detector. The method is applied to the analysis of natural honey and also honey and beeswax samples from beehives treated with the above compounds.

Camphor↗

PubMed2002

Capillary gas chromatography with mass spectrometric and atomic emission detection for characterization and monitoring chlordimeform degradation in honey.

Capillary gas chromatography-mass spectrometry and capillary gas chromatography-atomic emission detection have been successfully used to identify and monitor the main degradation products of chlordimeform when this compound is initially present in honey. The analysis of laboratory-spiked honey samples over 28 weeks revealed the occurrence of two degradation products: 4-chloro-o-toluidine (I) and N-formyl-4-chloro-o-toluidine (III). During this period the concentration of chlordimeform decreased to 7.5% of its initial value; the concentration of compound I increased gradually whereas compound III was present in a larger proportion and reached a maximum around the 14th week.

Chlorphenamidine↗

PubMed2001

Applications of the Chiralpak AD and Chiralcel OD chiral columns in the enantiomeric separation of several dioxolane compounds by supercritical fluid chromatography.

Two chiral columns based on polysaccharide derivatives (Chiralpak AD and Chiralcel OD) have been tested for the chiral separation of several dioxolane compounds, using supercritical fluid chromatography. The compounds studied included ketoconazole and some of its precursors. The effect of the different modifiers and the pressure, on the chromatographic parameters was also evaluated. In general, the alcohol modifiers provided better results than acetonitrile, and all the compounds could be separated with these two columns, but the selection of the column depends on the kind of compound.

Chromatography, Supercritical Fluid↗

PubMed2001

Use of deactivated fused-silica capillary precolumns in pesticide analysis by gas chromatography with electron-capture detection.

The advantages and disadvantages of coupling a retention gap of fused-silica between the injection port and the chromatographic column are discussed. The influence on the peak width and height of several factors such as the solvent (n-hexane, acetone, ethyl acetate and methanol), the gap (length, inner diameter, deactivation mode), the injection volume and the pesticide concentration has been examined. Those factors have very different incidences so, it is not possible to extract a general recommendation about the use of gaps. For this reason, checking its viability in each particular case is more advisable.

Chromatography, Gas↗

PubMed2001

Analysis of pesticide residues in wine by solid-phase extraction and gas chromatography with electron capture and nitrogen-phosphorus detection.

A feasible and reproducible method for multiresidue analysis of several common pesticides, of different polarities, in wine samples is proposed. The method combines a solid-phase extraction on polymeric cartridges eluted with ethyl acetate and a gas chromatographic determination using electron capture and nitrogen-phosphorus detection. To avoid the matrix effect, previous washing of the cartridges with a mixture of water-2-propanol (90:10) and further clean-up of the extract on Florisil cartridges, together with a calibration using spiked extracts, are recommended.

Chromatography, Gas↗

PubMed2001

High-performance liquid chromatographic determination of methyl anthranilate, hydroxymethylfurfural and related compounds in honey.

A high-performance liquid chromatographic method for determining 5-hydroxymethyl-2-furaldehyde (hydroxymethylfurfural), 2-furaldehyde (furfural), furan-2-carboxylic acid (2-furoic acid), furan-3-carboxylic acid (3-furoic acid), furan-3-carboxaldehyde (3-furaldehyde) and 2-aminobenzoic acid methyl ester (methyl anthranilate) in honey and honeydew samples is described. To prevent matrix interference and to isolate the compounds, a clean-up step which implies a solid-phase extraction on polymeric cartridges and an elution with 0.5 ml methanol is recommended. The compounds are separated on a reversed-phase column with a gradient of (A) 1% aqueous acetic acid-acetonitrile (97:3, v/v) and (B) acetonitrile-water (50:50, v/v), with UV detection at 250 nm. The method is applied to the analysis of samples from different botanical origin.

Calibration↗

PubMed2001

[Diet of an anecic earthworm from the Colombian savannas: questioning ecological groups].

An ecological classification based on a set of morphological characters may be used to describe earthworm functions in soil. However these relationships have been seldom verified. Gizzards of the earthworm Martiodrilus carimaguensis (Glossoscolecidae) were studied to find out if its anecic morphology was in agreement with its diet (shallow litter remains and deep organo-mineral material). By direct observation of 13 adults' gizzard contents with a dissecting and a phase contrast microscope, the volumetric percentage of plant fragments, roots, amorphous organic matter and mineral particles reached respectively 63, 5, 6.5 and 30% v/v. Eighty percent of plant fragments were microscopic, and mostly incorporated into the organo-mineral earthworm casts well preserved in the gizzard. Coprophagy and rhizophagy were the dominant feature of M. carimaguensis diet. Yet, the casts produced revealed a high variability in its diet, what could be related to transitional adoption of a typical anecic diet during some periods.

Animals↗