0000000000082621
AUTHOR
S. Torres-cartas
SENSITIZED LANTHANIDE FLUORESCENCE DETECTION OF STEROIDAL HORMONES
Several steroidal hormones with an α,β-unsaturated carbonyl group sensitized the fluorescence of terbium(III) ions: medroxyprogesterone, medroxyprogesterone acetate, methyltestosterone, nandrolone, nandrolone decanoate, progesterone, testosterone, testosterone enanthate, and testosterone propionate, but other steroids which have this chromophore did not give any signal: clostebol acetate, dehydrotestosterone, dydrogesterone, methandienone, and methenolone enanthate. Sensitized fluorescence was used to detect the steroids when eluted with micellar mobile phases of sodium dodecyl sulphate (SDS)-acetonitrile and SDS-pentanol containing 0.01 M Tb(III), with 245 nm and 545 nm as excitation and e…
Retention-structure relationship studies for some steroidal hormones in micellar liquid chromatography
The retention behavior in a C18 column of fourteen steroidal hormones (clostebol acetate, dehydrotestosterone, dydrogesterone, medroxyprogesterone, medroxyprogesterone acetate, methandienone, methyltestosterone, nandrolone, nandrolone decanoate, progesterone, testosterone, testosterone enanthate, testosterone propionate and, stanozolol) with pure micellar mobile phases prepared from sodium dodecyl sulfate (SDS), and hybrid mobile phases comprising SDS-acetonitrile and SDS-pentanol, was correlated with their octanol-water partition coefficients. Similar correlations were found with retention data obtained by other authors in gas chromatography, conventional reversed-phase liquid chromatograp…
Biopartitioning micellar chromatoraphy to predict blood to lung, blood to liver, blood to fat and blood to skin partition coefficients of drugs
[EN] 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 the partition coefficients from blood to lung, blood to liver. blood to fat and blood to skin is demonstrated. PLS2 and multiple linear regression (MLR) models based on BMC retention data are proposed and compared with other ones reported in bibliography. The proposed models present better or similar descriptive and predictive capability. (C) 2008 Elsevier B.V. All rights r…
Influence of photo-initiators in the preparation of methacrylate monoliths into poly(ethylene-co-tetrafluoroethylene) tubing for microbore HPLC.
[EN] In this study, poly(butyl methacrylate-co-ethyleneglycol dimethacrylate) polymeric monoliths were in situ developed within 0.75 mm i.d. poly(ethylene-co-tetrafluoroethylene) (ETFE) tubing by UV polymerization via three different free-radical initiators fscce-azobisisobutyronitrile (AIBN), 2,2-dimethoxy-2-phenylacetophenone (DMPA) and 2-methyl-4'-(methylthio)-2-morpholinopropiophenone (MTMPP). The influence of the nature of each photo-initiator and irradiation time on the morphological features of the polymer was investigated by scanning electron microscopy, and the chromatographic properties of the resulting microbore columns were evaluated using alkyl benzenes as test substances. The …
Magnetic molecularly imprinted polymer for the simultaneous selective extraction of phenoxy acid herbicides from environmental water samples
[EN] A selective magnetic molecularly imprinted polymer (MMIP) was synthetized with 4-chloro-2-methylphenoxyacetic acid as template and 4-vinylpiridine as monomer in presence of vinylized magnetite nanoparticles. Scanning electron microscopy, nitrogen adsorption-desorption isotherms, Fourier transform infrared spectrometry and vibrating sample magnetometry were applied to characterize the resulting material. The synthesized MMIP was applied as sorbent in magnetic molecularly imprinted solid-phase extraction (MMISPE) for selective extraction of a mixture of the five herbicides 4-chloro-2-methylphenoxyacetic acid (MCPA), 4-(4-chloro-2-methylphenoxy)butyric acid (MCPB), mecoprop (MCPP), fenoxa…
Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography
[EN] In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch®), or mixtures of H2O2 and H2SO4, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification…
Preparation of monolithic polymer-magnetite nanoparticle composites into poly(ethylene-co-tetrafluoroethylene) tubes for uses in micro-bore HPLC separation and extraction of phosphorylated compounds
[EN] This paper describes the fabrication of a novel microbore monolithic column modified with magnetite nanoparticles (MNPs) prepared in a poly(ethylene-co-tetrafluoroethylene) (EFTE) tubing, and its application as stationary phase for the chromatographic separation of phosphorylated compounds. In order to obtain the composite column, a two-step procedure was performed. The formation of a glycidyl methacrylate-based monolith inside the activated ETFE tube was firstly carried out. Then, two incorporation approaches of MNPs in monoliths were investigated. The generic polymer was modified with 3-aminopropyltrimethoxysilane (APTMS) to be subsequently attached to MNP surfaces. Alternatively, AP…
Resolution of mixtures of steroidal hormones with micellar eluents of sodium dodecyl sulphate and acetonitrile or pentanol
An optimization strategy was applied to explore the capability of hybrid micellar eluents of sodium dodecyl sulphate (SDS), using acetonitrile or pentanol as modifiers, to resolve mixtures of eleven steroids showing a wide range of hydrophobicity (clostebol acetate, dehydrotestosterone, dydrogesterone, medroxyprogesterone, medroxyprogesterone acetate, methandienone, methyltestosterone, progesterone, testosterone, testosterone enanthate and testosterone propionate). The accurate prediction of the retention behaviour of the steroids, with relative errors in the 0.8–1.7% and 0.4–2.9% ranges for SDS-acetonitrile and SDS-pentanol eluents, respectively, demonstrated the reliability of the methodo…
Polymer-based materials modified with magnetite nanoparticles for enrichment of phospholipids
[EN] A polymeric material modified with magnetic nanoparticles (MNPs) has been synthesized and evaluated as sorbent both for solid-phase extraction (SPE) and dispersive magnetic solid-phase extraction (MSPE) of phospholipids (PLs) in human milk samples. The synthesized sorbent was characterized by scanning electron microscopy and its iron content was also determined. Several experimental variables that affect the extraction performance (e.g. loading solvent, breakthrough volume and loading capacity) were investigated and a comparison between conventional SPE and MSPE modalities was done. The proposed method was satisfactorily applied to the analysis of PLs in human milk fat extracts in diff…
Biopartitioning micellar chromatography to pedict mutagenicity of aromatic amines
[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…
Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases
[EN] In this study, porous polymer monoliths were in situ synthesized in fluoropolymers tubing to prepare microbore HPLC columns. To ensure the formation of robust homogeneous polymer monoliths in these housing supports, the inner surface of fluoropolymer tubing was modified in a two-step photografting process. Raman spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the inner poly(ethylene-co-tetrafluoroethylene) (ETFE) wall and the subsequent attachment of a monolith onto the wall. Poly(glycidyl methacrylate-co-divinylbenzene), poly(butyl methacrylate-co-ethyleneglycol dimethacrylate) and poly(styrene-co-divinylbenzene) monoliths were in situ synt…
Comparison between micellar liquid chromatography and capillary zone electrophoresis for the determination of hydrophobic basic drugs in pharmaceutical preparations
[EN] The determination of highly hydrophobic basic compounds by means of conventional reversed-phase liquid chromatographic methods has several drawbacks. Owing to the characteristics of micellar liquid chromatography (MLC) and capillary electrophoresis (CE), these techniques could be advantageous alternatives to reversed-phase chromatographic methods for the determination of these kinds of compounds. The objective of this study was to develop and compare MLC and CE methods for the determination of antipsychotic basic drugs (amitryptiline, haloperidol, perphenazine and thioridazine) in pharmaceutical preparations. The chromatographic determination of the analytes was performed on a Kromasil…
DETERMINATION OF STEROIDAL HORMONES IN URINE SAMPLES BY MICELLAR LIQUID CHROMATOGRAPHY FOLLOWING SOLID-PHASE EXTRACTION
Steroidal hormones were determined in spiked urine samples using micellar mobile phases of sodium dodecyl sulphate (SDS)-pentanol, solid-phase extraction (SPE), and detection in the UV region. In the optimized procedure, a 10 mL aliquot of urine sample is loaded into a C18 cartridge and washed with 2 mL of 50:50 (v/v) methanol-water, followed by 200 μL of 70:30 (v/v) methanol-water. The retained steroids are eluted with 2 mL of methanol and the eluate evaporated to dryness under nitrogen at 50°C. The residue is redissolved with 200 μL of the micellar mobile phase used in the chromatographic separation and injected into the chromatograph. The performance of the procedure was checked for 13 s…