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Biomedical subjects

David C Sherrington

Publications and source records attributed to David C Sherrington.

16 recordsLinked to original sources

Direct determination of ciprofloxacin by mass spectrometry after a two-step solid-phase extraction using a molecularly imprinted polymer.

A molecularly imprinted polymer (MIP) has been prepared for the first time with ciprofloxacin (CIPRO) as the template molecule, via a noncovalent synthetic procedure. Prior to its use as a sorbent in SPE, the MIP was evaluated chromatographically to confirm that it was indeed molecularly imprinted. The MIP was then used to extract CIPRO selectively from urine samples by means of a two-step SPE procedure in which a commercial Oasis cartridge and a molecularly imprinted SPE cartridge were combined in series. This approach allowed the matrix compounds present in the samples to be removed effectively. The urine extracts obtained after this two-step SPE procedure was applied were relatively clean compared to the original samples, and this made it possible to inject directly the extracts into a mass spectrometer and thus quantify CIPRO in urine samples at low levels and reduce the time of analysis.

Evaluation Study↗

Evaluation of a new hypercrosslinked polymer as a sorbent for solid-phase extraction of polar compounds.

A new hypercrosslinked polymer (HXLGp) with hydrophilic character due to the presence of hydroxyl moieties has been tested as a sorbent for the solid-phase extraction (SPE) of several polar compounds from water samples. This new sorbent enables the on-line extraction of 300 ml of sample with recoveries higher than 80% for polar compounds such as oxamyl, methomyl or desisopropylatrazine (DIA). The HXLGp has also been compared to other commercially available sorbents such as Oasis HLB (hydrophilic macroporous), to hydrophobic hypercrosslinked resins and to a previously synthesized sorbent based on N-vinylimidazole-divinylbenzene. The results are consistently better with the new synthesized sorbent. The method was successfully applied to the on-line SPE-HPLC of tap and river water samples. The validation with river water samples provided good linearity range and detection limits between 0.03 for methomyl and 4-nitrophenol (4NP) to 0.2 microg l(-1) for phenol (Ph).

Chromatography↗

Selective enrichment of anti-inflammatory drugs from river water samples by solid-phase extraction with a molecularly imprinted polymer.

A molecularly imprinted polymer (MIP) is synthesised by a noncovalent protocol in which ibuprofen was used as a template molecule. The polymer was evaluated chromatographically and it was seen that the MIP showed cross-reactivity. Subsequently, when this polymer was used as sorbent in SPE it was possible to selectively extract a mixture of nonsteroidal anti-inflammatory drugs from aqueous samples when a cleanup step with dichloromethane was performed. The performance of the MIP was evaluated with river water and water from a wastewater treatment plant, and compared with the performance of a commercial Isolute ENV+ sorbent.

Anti-Inflammatory Agents↗

A new molecularly imprinted polymer for the selective extraction of naproxen from urine samples by solid-phase extraction.

A non-covalent molecularly imprinted polymer (MIP) was synthesised using naproxen (a non-steroidal, anti-inflammatory drug (NSAID)) as a template molecule. The MIP was chromatographically evaluated to confirm the imprinting effect, and was then applied as a selective sorbent in solid-phase extraction (SPE) to selectively extract naproxen. After this study, the MIP was used to extract naproxen from urine samples; it was demonstrated that by applying a selective washing step with acetonitrile (ACN) the compounds in the sample that were structurally related to naproxen could be eliminated.

Anti-Inflammatory Agents, Non-Steroidal↗

Molecularly imprinted solid-phase extraction of naphthalene sulfonates from water.

A new polymeric sorbent synthesised by exploiting molecular imprinting technology has been used to selectively extract naphthalene sulfonates (NSs) directly from aqueous samples. In the non-covalent molecular imprinting approach used to prepare this polymer, 1-naphthalene sulfonic acid (1-NS) and 4-vinylpyridine (4-VP) were used as a template molecule and functional monomer, respectively, and both dissolved in a mixture of methanol/water (4:1) as porogen together with the cross-linker ethylene glycol dimethacrylate. The new non-covalent molecularly imprinted polymer (MIP) prepared in aqueous environment was used as a sorbent in solid-phase extraction (SPE) to selectively extract a group of naphthalene mono- and disulfonates. When one litre of a standard aqueous solution, which contained a mixture of eight NSs, was percolated through the SPE cartridge, all the NSs were retained on the MIP because of the cross-reactivity of the polymer. Recoveries were higher than 80% for all the compounds even after a clean-up step with methanol (MeOH). The MIP was also used to analyse water from the Ebro river.

Naphthalenesulfonates↗

Bifurcated, modular syntheses of chiral annulet triazacyclononanes.

Three chiral 2,6-disubstituted tri-N-methyl azamacrocycles have been prepared by modular methods. These macrocycles were accessed from three chiral 1,4,7-triazaheptanes intermediates that were prepared by two independent routes. The first of these routes involved the benzylamine opening of chiral tosyl aziridines followed by debenzylation but was problematic on solubility grounds. A second, more effective, route was developed which avoided debenzylation by using ammonia in the nucleophilic opening of chiral tosyl aziridines.

Aza Compounds↗

The synthesis of an isopropyl substituted 1,4,7-triazacyclononane via an in situ sequential macrocyclisation method.

Using L-valine methyl ester hydrochloride as starting material, the synthesis of (2S)-2-isopropyl-1,4,7-trimethyl-1,4,7-triazacyclononane is described. Various standard Richman-Atkins cyclisation methods gave only poor yields in the key macrocyclisation step. Efficient macrocyclisation yields were, however, realised when an in situ sequential cyclisation method was developed.

Chemistry, Organic↗

On-line solid-phase extraction with molecularly imprinted polymers to selectively extract substituted 4-chlorophenols and 4-nitrophenol from water.

Three polymers have been synthesised using 4-chlorophenol (4-CP) as the template, following different protocols (non-covalent and semi-covalent) and using different functional co-monomers, 4-vinylpyridine (4-VP) and methacrylic acid (MAA). The polymers were evaluated to check their selectivity as molecularly imprinted polymers (MIPs) in solid-phase extraction (SPE) coupled on-line to liquid chromatography. The solid-phase extraction procedure using MIPs (MISPE), including the clean-up step to remove any interferences, was optimised. The 4-VP non-covalent polymer was the only one which showed a clear imprint effect. This MIP also showed cross-reactivity for the 4-chloro-substituted phenols and for 4-nitrophenol (4-NP) from a mixture containing the 11 priority EPA (Environmental Protection Agency) phenolic compounds and 4-chlorophenol. The MIP was applied to selectively extract the 4-chloro-substituted compounds and 4-NP from river water samples.

Chlorophenols↗

Non-covalent and semi-covalent molecularly imprinted polymers for selective on-line solid-phase extraction of 4-nitrophenol from water samples.

Two molecularly imprinted polymers (MIPs) have been synthesised for the selective extraction of 4-nitrophenol (4-NP) from water samples. One polymer was synthesised via a non-covalent approach and the other via a semi-covalent approach. The selectivity of the polymers for 4-NP was evaluated when these polymers were applied in on-line solid-phase extraction (MISPE) coupled to reversed-phase HPLC. The MISPE conditions for both MIPs were optimised and a clean-up step was included to eliminate non-specific interactions. Differences between the two MIPs were observed with the non-covalent MIP being the more selective of the two, whereas the recoveries were slightly higher for the semi-covalent MIP. The performance of the imprinted polymers in the MISPE of real water samples was also evaluated.

Chromatography, Liquid↗

Spherical molecularly imprinted polymer particles: a promising tool for molecular recognition in capillary electrokinetic separations.

Spherical molecularly imprinted polymer particles obtained via precipitation polymerization, were introduced as a pseudostationary phase in capillary electrophoresis (CE) to study molecular recognition. Analyses were performed via a partial filling technique using (+)-ephedrine-imprinted microspheres (100-200 nm) which were polymerized from methacrylic acid and 1,1,1-Tris(hydroxymethyl)propanetrimethacrylate using acetonitrile as the solvent. The influence of pH and the modifier content on the separation was investigated. A 0.1% w/v suspension in an aqueous 10 mM phosphate buffer (pH 2.5 with 40% acetonitrile) was hydrodynamically injected into the CE system (80% of the effective capillary length) and led to full baseline separation of racemic ephedrine within 10 min.

Adrenergic Agents↗