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Biomedical subjects

J R Dean

Publications and source records attributed to J R Dean.

17 recordsLinked to original sources
PubMed2005

An assessment of the bioavailability of persistent organic pollutants from contaminated soil.

A procedure to assess the bioavailability of persistent organic pollutants (POPs) from soil samples has been developed. The procedure is based on the use of simulated in vitro gastrointestinal extraction to remove POPs from soil matrices. The level of recovery, using this approach, is assessed following liquid-liquid extraction (LLE) and analysis by gas chromatography-mass selective detection (GC-MSD). The remaining soil residue is then extracted using pressurised fluid extraction (PFE) followed by GC-MSD analysis to assess the residual fraction. The residual fraction is monitored to determine the unavailable fraction i.e. not available for absorption in the gastrointestinal tract of humans. The procedure was applied to four soil samples i.e. an aged, spiked soil and three certified reference materials (CRMs) contaminated with POPs. Recoveries of pesticides (lindane, endosulfan I, endrin, DDE, DDD and endosulfan II), phenols (cresol, TCP and PCP), and base neutral compounds (hexachloroethane, acenaphthene, dibenzofuran, fluorene and hexachlorobenzene) from aged, spiked soil following extraction with gastric fluid ranged from 0.8 to 8.3% while following intestinal extraction ranged from 5.5 to 13.5%, irrespective of POP. Recoveries of pesticides (lindane, endosulfan I, endrin, DDE, DDD and endosulfan II) from CRM 805-050 following extraction with gastric fluid were below the limit of detection while following intestinal extraction ranged from 5.3 to 12.8%. Recoveries of phenols (cresol, TCP and PCP) from CRM 401-225 following extraction with gastric fluid ranged from 1.6 to 2.0% while following intestinal extraction ranged from 4.1 to 5.4%. Recoveries of base neutral acid analytes (hexachloroethane, acenaphthene, dibenzofuran, fluorene and hexachlorobenzene) from CRM 107-100 following extraction with gastric fluid ranged from 1.4 to 4.0% while following intestinal extraction ranged from 6.6 to 12.7%. It has been found that the majority of POPs present i.e. >75%, would be excreted if consumed and not be absorbed in the gastrointestinal tract of humans.

Amylases↗
PubMed2005

SPE/LC/ESI/MS with phthalic anhydride derivatisation for the determination of alcohol ethoxylate surfactants in sewage influent and effluent samples.

A new method for the analysis of alcohol ethoxylates (AEs) using electrospray ionisation liquid chromatography/mass spectrometry (ESI LC/MS) is described. The procedure incorporates a novel derivatisation step with phthalic anhydride for the analysis of EO0-20 ethoxylates in a single analysis. The derivatives obtained have proved to be very stable and the negative ion spectra show reduced background ions and competing adduct formation as compared to positive ion spectra. An automated solid phase extraction (SPE) step is used to allow both pre-concentration and clean-up of the environmental samples. The method provides more efficient recovery of AEs across the C12-C18 range than previously reported in the literature. Recoveries from final effluent spiked at 100 microg/L total AE, for the 126 species analysed, were found to be in the range 55-117%, with approximately 100 of the individual analytes having recoveries of 90-105%. An LOD of 0.02 microg/L for individual ethoxylate components is reported with the instrument operated in scan mode over the range m/z 300-1300. The method was applied to sewage effluent and influent samples, with AEs determined at approximately 7 and 5000 microg/L, respectively.

Alcohols↗
PubMed2004

Characterisation and analysis of persistent organic pollutants and major, minor and trace elements in Calabash chalk.

Analysis of Calabash chalk has been done using energy dispersive X-ray fluorescence spectroscopy (EDXRF), X-ray diffraction (XRD) and pressurised fluid extraction (PFE) followed by gas chromatography (GC) with mass selective detection (MSD). It was found by XRD that the composition of Calabash chalk was an aluminium silicate hydroxide from the kaolin clay group with the possible formula Al(2)Si(2)O(5)(OH)(4). Multi-elemental analysis by EDXRF was able to quantify 22 elements in Calabash chalk including lead at a mean concentration of approximately 40 mg/kg. A range of persistent organic pollutants were identified and quantified in Calabash chalk including alpha lindane, endrin, endosulphan II and p,p'-DDD using PFE-GC-MSD.

Aluminum Silicates↗
PubMed2001

Pressurised fluid extraction of bupirimate and ethirimol from aged soils.

This paper assesses the effect of pressurised fluid extraction (PFE) on the recovery of bupirimate and its degradation product, ethirimol from a range of soil types. The analytes were extracted under standard conditions (pressure, 2000 p.s.i.; temperature, 100 degrees C; and, three static flush cycles of 5 min static extraction time each) using a variety of individual and combined solvents. It was found that the recovery of bupirimate was dependent upon the organic matter content of soil.

Gas Chromatography-Mass Spectrometry↗
PubMed2000

Extraction of DDT [1,1,1,-trichloro-2,2-bis(p-chlorophenyl)ethane] and its metabolites DDE [1,1-dichloro-2,2-bis(p-chlorophenyl)-ethylene] and DDD [1,1-dichloro-2,2-bis(p-chlorophenyl)-ethane]) from aged contaminated soil.

Pressurised liquid extraction (PLE) was used to extract DDT [1,1,1,-trichloro-2,2-bis(p-chlorophenyl)ethane] and its metabolites, DDD [1,1-dichloro-2,2-bis(p-chlorophenyl)ethane] and DDE [1,1-dichloro-2,2-bis(p-chlorophenyl)ethylene] from an aged, contaminated soil. Using three sequential static phases, PLE removed an equivalent quantity of DDT and its metabolites as Soxhlet extraction, in less time and with less solvent. Recovery was almost quantitative, implying appropriate sample work-up and manipulation.

DDT↗
PubMed2000

Pressurised liquid extraction of pentachlorophenol from dyestuffs and cotton.

Pressurised liquid extraction (PLE) was used to extract pentachlorophenol from cotton and dyestuffs. Five dyes and one dyed cotton were investigated for pentachlorophenol. The dyed cotton was found to have between 5.3 and 5.9 microg g(-1) pentachlorophenol, while the dyes were found to have between 42 and 2569 microg g(-1) pentachlorophenol present. The latter were found to be dye and manufacturing site dependant. Recovery experiments, in all cases, were found to be quantitative indicating appropriate sample work-up and manipulations.

Coloring Agents↗
PubMed2000

Influence of solvent and soil type on the pressurised fluid extraction of PAHs.

Pressurised fluid extraction (PFE) of polycyclic aromatic hydrocarbons (PAHs) from a certified reference material (CRM) 524 has been firstly optimised following a central composite design. The instrumental parameters of the PFE (pressure, temperature, extraction time and number of solvent cycles) were studied in order to obtain maximum extraction yields. Neither pressure nor extraction time or temperature seemed to have any significant effect on the extraction yield, therefore one extraction cycle was enough to exhaustively extract all the PAHs from CRM 524. Once the instrumental conditions were established, the extraction yields obtained with eight different solvents or solvent mixtures [acetone, dichloromethane, acetonitrile, acetone-dichloromethane (1 + 1 v/v), acetone-isohexane (1 + 1 v/v), isohexane, methanol and toluene] from the CRM 524 were compared and showed that the best recoveries were obtained with acetone-isohexane (1 + 1 v/v). Finally, the effect of sand, silt, clay and the organic matter content of soil was investigated with respect to recovery of PAHs by PFE with different solvents or solvent mixtures for aged soil samples. In this case, eight soils with different sand, silt, clay and organic matter contents were slurry spiked with PAHs and aged for 19 days. Three aliquots of each slurry spiked soil were extracted with the previously mentioned solvents and the results were studied by means of principal component analysis (PCA) of the whole data set (soil composition, solubility parameter of the solvent and recoveries of all PAHs) and partial least squares (PLS). Clay and organic matter content and the squared solubility parameter have the highest correlation with the recovery of PAHs from soil samples.

Environmental Monitoring↗
PubMed2000

The strengthening effect of percutaneous vertebroplasty.

AIM: To examine whether single-needle vertebroplasty is effective in strengthening vertebrae. MATERIALS AND METHODS: Four adjacent intact lumbar vertebrae were removed from each of nine adult post-mortem subjects. One or two vertebra of each set was injected with low viscosity acrylic bone cement using a single-track posterolateral approach. Vertebral strength was measured during constant rate axial compression. RESULTS: Single-needle injection delivered different quantities of cement (1-8 ml) in an asymmetric distribution. Injected vertebrae were stronger than controls in 10 out of 12 cases (P < 0.01), suggesting that cement injection increases the load needed to cause initial vertebral fracture. Compression was continued past the point of initial failure, to simulate progressive vertebral collapse. Injected specimens were more resistant to deformation than control specimens (P < 0.05), most of which initially deformed with little increase in load. CONCLUSION: Single-track injection of bone cement appeared to strengthen vertebrae against both initial failure and subsequent collapse. The magnitude of strength increase from vertebroplasty was variable, and did not correlate with the volume of cement injected. Further investigation is needed to optimize the technique.Gishen, P. (2000). Clinical Radiology55, 471-476.

Aged↗
PubMed1999

Intrapituitary fluid levels following haemorrhage: MRI appearances in 13 cases.

Demonstration of fluid levels on MRI is well recognised in cerebral haematomas, tumours and cysts. The occurrence of fluid levels within haemorrhagic pituitary tumours has not previously been described in detail. Evidence of haemorrhage was identified in 27 of 125 pituitary tumours. Fluid levels occurred in 13 of these haemorrhagic tumours. No association with histological type was identified. Recognised risk factors for haemorrhage were identified in half of the cases.

Adenoma↗
PubMed1997

Extraction of pharmaceuticals using pressurised carbon dioxide.

This paper reviews the applications of super- and sub-critical carbon dioxide for the extraction of pharmaceuticals from various matrices. The matrices covered are divided into the following types: animal feed, formulations, biological and miscellaneous, with various sub-divisions as appropriate. The polar nature of most pharmaceuticals often precludes the use of carbon dioxide only, so it is common to find the addition of a more polar solvent, as modifier. As the majority of sample types covered are solid, little if any pre-treatment is required, with the exception of grinding, prior to insertion in the sample extraction cell. For liquid-type matrices, sample pre-treatment is the normal. Often this may involve adsorption on an inert support e.g. Celite or diatomaceous earth, or immobilisation on a functionalised silica surface, e.g. C18. The later may take the form of a solid phase extraction cartridge or disk. An attempt has also been made to sample from liquid matrices directly using a modified extraction cell. The variety of sample types, matrices and analyte polarity places stringent requirements on the use of pressurised carbon dioxide. Its potential for effective recovery is examined in this review.

Animal Feed↗
PubMed1995

A comparison between solid phase extraction and supercritical fluid extraction for the determination of fluconazole from animal feed.

The application of supercritical fluid extraction with carbon dioxide and modified carbon dioxide for the determination of fluconazole from an animal feed was studied. A fractional factorial design approach was used to examine the significant experimental variables for quantitative extraction of fluconazole. Gas chromatography with either flame ionisation or mass selective detection was used for quantitation of the extracts. The results indicated that modifier (methanol) had the greatest effect on the recovery of fluconazole from the animal feed.

Animal Feed↗
PubMed1989

Application of high-performance liquid chromatography--inductively coupled plasma mass spectrometry to the investigation of cadmium speciation in pig kidney following cooking and in vitro gastro-intestinal digestion.

The speciation of cadmium in retail pig kidney has been examined by size-exclusion chromatography (SEC) coupled directly to inductively coupled plasma mass spectrometry (ICP-MS). Approximately 35% of the cadmium from uncooked kidney was soluble after aqueous extraction at pH 8 and SEC - ICP-MS revealed three discrete peaks whose retention times corresponded to estimated relative molecular masses of 1.2 x 10(6), 7.0 x 10(4) and 6 x 10(3)-9 x 10(3). In the cooked kidney, 35% of the Cd was soluble and was all associated with a peak of a relative molecular mass (Mr) of 6 x 10(3)-9 x 10(3). After simulated gastric digestion of cooked pig kidney at pH 2.5, 60% of the cadmium was solubilised and associated with a species of Mr less than 1 x 10(3). When the digest was also subjected to simulated intestinal digestion at pH 6.8, a single peak, which corresponded to 20% of the original cadmium, was eluted. This peak co-eluted with the single peak extracted at pH 8.0 from the cooked kidney. It was also of similar estimated Mr to the single broad peak observed after simulated gastro-intestinal digestion of equine renal metallothionein (Mr = 1.1 x 10(4]. The results suggest that the majority of soluble cadmium in retail pig kidney is associated with a metallothionein-like protein that survives both cooking and simulated in vitro gastro-intestinal digestion.

Animals↗
PubMed1978

Long-term study of smoking by secondary schoolchildren.

We report the methodology and some first year results of a 5-year longitudinal study of smoking. In 6330 Derbyshire secondary schoolchildren aged 11-16 years, 6% of boys and 2.5% of girls were smoking one or more cigarettes per week. Higher rates of regular smoking and of children who had tried smoking were found in secondary modern schools, followed by middle, comprehensive and grammar schools. The results clarify the relationship between children's smoking habits and those of the parents and siblings. Boys were more likely to smoke if their fathers smoked and girls were more likely to smoke if their mothers smoked. Irrespective of parental smoking, whether or not siblings smoked had a great influence on whether the child would smoke. Having more money to spend, working at a part-time job, spending more evenings out with a mixed-sex peer group, at a youth club, or out dancing, and playing truant from school were all associated with an increased risk of smoking.

Adolescent↗
PubMed1974

The role of ribonuclease II in the maturation of precursor 16S ribosomal ribonucleic acid in Escherichia coli.

The suggested involvement of ribonuclease II in the maturation of rRNA has been examined directly by determining the activity of the enzyme and the amount of p16S rRNA in cell-free extracts from Escherichia coli A19 and its temperature-sensitive derivative N464 grown under experimental conditions designed to vary the amounts of enzyme and precursor independently. In strain A19 the enzyme showed maximum activity in circumstances where the amount of p16S rRNA was normal (e.g. exponential-phase cells) or raised eight times (e.g. during inhibition of growth by methionine starvation of the relaxed auxotroph or by chloramphenicol or puromycin treatment). In strain N464 at the non-permissive temperature the ribonuclease II activity may be decreased by 50% without effect upon the amount of p16S rRNA, whereas in methionine starvation of this strain the enzyme activity is at a maximum and the p16S rRNA is eight times that in exponential-phase cells. These observations are discussed in relation to the previously implied role of ribonuclease II in the maturation of rRNA within ribosome precursors.

Centrifugation↗
PubMedDate not supplied

Isotope ratio and isotope dilution analysis of lead in wine by inductively coupled plasma-mass spectrometry.

The lead content of 12 wine samples was measured by inductively coupled plasma-mass spectrometry using the methods of standard addition and isotopic dilution analysis. An additional wine sample was analysed by external calibration, standard addition and isotopic dilution analysis. The lead content of the wine samples was in the range 30-150 ng ml-1 and good agreement between the different techniques was observed. Analysis of lead isotope ratios revealed significant differences between Australian and European wines, reflecting the different isotopic composition of Australian lead.

Australia↗
PubMedDate not supplied

Determination of antifungals in rodent diet by supercritical fluid extraction followed by packed column supercritical fluid chromatography with ultraviolet detection.

Supercritical fluid extraction (SFE) followed by packed column supercritical fluid chromatography with ultraviolet detection was evaluated as a quantitative method for determining 4 antifungals (fluconazole, tioconazole, hexaconazole, and UK-47,265) in rodent diet. Chromatography was achieved with a cyano-bonded silica column, UV detection at 210 nm, and methanol-modified supercritical carbon dioxide as mobile phase. The effects of modifier concentration, temperature, and column pressure on antifungal retention time was studied. Off-line SFE was optimized at 2 spike levels, ranging from 0.5 to 10 g/kg, for each of the 4 antifungals. Average recoveries ranged from 79.0% for UK-47,265 to 96.5% for hexaconazole. Overall, the procedure provides a suitable method for analyzing antifungals in spiked rodent diet.

Animals↗