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At least 289 records · Page 16Linked to original sources
PubMed2005

Low part per trillion determination of reactive alkanethiols in wastewater by in situ derivatization-solid-phase microextraction followed by GC/MS.

A solid-phase microextraction (SPME) procedure for the simultaneous determination of volatile alkanethiols (i.e., methane-, ethane-, propanethiol) and dihydrogen sulfide in aqueous samples as stable thioethers followed by GC/MS determination was developed. Accordingly, N-ethylmaleimide as derivatization reagent in the aqueous phase was used for the first time, improving the analyte stability and method sensitivity in comparison to the determination of free forms. Thus, pH of the aqueous medium, reaction time, and derivatization reagent concentration have been evaluated, and the main parameters affecting the SPME process (i.e., coating selection, extraction mode and time profile, extraction and desorption temperatures) optimized. At the selected derivatization and extraction conditions, the proposed method provided no matrix effect either in the derivatization reaction or in the microextraction steps. RSD values were lower than 11% and LODs from 0.74 to 5.2 ng L(-1). The developed procedure was successfully applied to different water and wastewater samples, where dihydrogen sulfide and some of the target alkanethiols were identified at low-microgram per liter concentrations.

Journal Article↗
PubMed2002

Recovery, enrichment and selectivity in liquid-phase microextraction comparison with conventional liquid-liquid extraction.

Mathematical descriptions for extraction recovery and enrichment were applied for liquid-phase microextraction (LPME) and comparison with conventional two- and three-phase liquid-liquid extraction techniques (LLE) was made. The LPME theoretical calculations were verified by experimental determination of actual partition coefficients and by data obtained with LPME in a robust hollow fibre formate. With hollow fibre LPME operated in the two-phase mode, analytes were extracted from 1 to 4 ml aqueous samples into 25-50 microl of an organic solvent present in the pores and in the lumen of the porous hollow fibres. Compared with conventional two-phase LLE, two-phase LPME provided substantially higher enrichments for compounds with relatively large partition coefficients (K(org)/d>500). In contrast, because of the large volume of organic solvent relative to the sample volume, LLE provided high recovery and moderate enrichment even for compounds with relatively low partition coefficients (K(org)/d>5). Thus, two-phase LPME may be used for substantially enhanced extraction selectivity and enrichment of relatively hydrophobic analytes as compared with LLE whereas conventional two-phase LLE is superior for more hydrophilic analytes. Similar results were found for three-phase LPME where analytes where extracted from 1 to 4 ml aqueous samples through approximately 20 microl organic solvent immobilized within the pores of the hollow fibre and into 25 microl of an aqueous acceptor solution inside the lumen of the hollow fibre. The fundamental differences of LPME and LLE were further demonstrated with practical experiments on extraction of the basic drugs promethazine, methadone, and haloperidol from human plasma and urine.

Chromatography, Gas↗
PubMed1987

Extraction of human organ-specific cancer neoantigens from cancer cells and plasma membranes with 1-butanol.

Immunoprotective tumor antigens of experimental tumors are selectively extracted by 1-butanol. Human organ-specific cancer neoantigens (OSNs) are tumor substances in cancer extracts to which patients with cancer of the same organ respond in the in vitro assay of leukocyte adherence inhibition. Here we determined whether OSNs as measured by leukocyte adherence inhibition assay are also selectively solubilized by 2.5% (v/v) 1-butanol. Butanol extracts of live tissue-cultured human cancer cells as well as extracts of primary breast cancer contained OSNs as determined by leukocyte reactivity in leukocyte adherence inhibition. With two-phase butanol, OSN activity was recovered in the aqueous and not in the organic phase, indicating that OSN is not a lipoprotein. The butanol-soluble OSN, whether allogeneic or autologous, was recognized by the T4 subset of T-cells in association with Class II major histocompatibility complex antigens of monocytes. Autologous OSN was extracted from membrane preparations of autologous primary cancer. Butanol extracts contained the previously identified Mr 40,000 protein OSN. Butanol removed about 50% of the Mr 40,000 protein OSN from live cancer cell membranes. Probably because of residual OSN in the membrane fragments and the ability of OSN to reassociate with the membrane, the T8 subset of pure T-cells responded positively to autologous cancer extracts. Passage of the autologous extract through an anti-Class I major histocompatibility complex antigen affinity column but not through a control affinity column negated the activity of the extract with pure autologous T-cells. The results indicate that human OSNs share with immunoprotective tumor antigens of experimental tumors the unique physicochemical property of being selectively extracted by 2.5% butanol.

1-Butanol↗
PubMed2003

Determination of 39 polybrominated diphenyl ether congeners in sediment samples using fast selective pressurized liquid extraction and purification.

In order to reduce time of analysis, a new pressurized liquid extraction (PLE) method that automatically and rapidly achieves quantitative and selective extraction of 39 polybrominated diphenyl ether (PBDE) congeners in sediment samples was optimized. It consists of on-line cleanup by inclusion of sorbents in the extraction cell. The new method was compared with a conventional method based on the use of Soxhlet extraction followed by solid-phase extraction (SPE) with cartridges. The instrumental determination was performed by GC-MS, using negative chemical ionization in the selected-ion monitoring mode. Recoveries from 47 to 82% were obtained for spiked tri- to hepta-PBDE congeners in sediment sample. The repeatability of replicate extractions was better than 15% relative standard deviation. The detection limits obtained with the new developed method were between 1 and 46 pg/g dry weight. The reduction in the sample preparation (extraction + cleanup) time (from days to 30 min) with a similar efficiency than that afforded by the conventional Soxhlet extraction-SPE cleanup technique indicates the suitability of this method. The method was applied to sediment samples where the analytes were detected in the range of 0.86-2.49 ng/g dry mass.

Ethers↗
PubMed1996

Analysis of cocaine, benzoylecgonine, and cocaethylene in urine by HPLC with diode array detection.

A solid phase extraction method was developed for the isolation of cocaine, benzoylecgonine, and cocaethylene from urine followed by high-performance liquid chromatography/diode array detection. The application of a new solid hybrid phase extraction technology produced much cleaner extracts than conventional extraction procedures and made the selective extraction of substances with different polarities possible. Two internal standards with great structural resemblance to benzoylecgonine (a carboxylic acid) and to the two esters, cocaine and cocaethylene, respectively, were synthesized. A linear response over a broad concentration range was obtained. The sensitivity, specificity, and accuracy were satisfactory for each analyte. Hydrolysis of cocaine and cocaethylene to benzoylecgonine during extraction and analysis was less than 0.5%. The method described can be used to corroborate cocaine use, to establish cocaine overdoses, and to study pharmacological effects of cocaine and its metabolites.

Chromatography, High Pressure Liquid↗
PubMed2004

Is smokeless tobacco a risk factor for coronary heart disease? A systematic review of epidemiological studies.

BACKGROUND: There is on-going debate about the wisdom of substituting smokeless tobacco products for cigarette smoking as a 'harm reduction' strategy. It is generally believed that health risks associated with smokeless tobacco use (ST) are lower than those with cigarette smoking. However, the population attributable risk of smoking is higher for cardiovascular diseases than for any cancers, and few studies or reviews have considered the cardiovascular outcomes of ST use. A systematic review was therefore carried out to highlight the gaps in the evidence base. METHODS: Electronic databases were searched, supplemented by screening reference lists, smoking-related websites, and contacting experts. Analytical observational studies of ST use (cohorts, case-control, cross-sectional studies) were included if they reported on cardiovascular disease (CVD) outcomes, or risk factors. Data extraction covered control of confounding, selection of cases and controls, sample size, clear definitions and measurements of the health outcome and ST use. One or two independent reviewers carried out selection, extraction and quality assessments. RESULTS: A narrative review was carried out. Very few studies were identified; only three from Sweden consider CVD outcomes and these are discrepant. There may be a modest association between use of Swedish snuff (snus) and cardiovascular disease (e.g., relative risk=1.4, 95% confidence interval 1.2-1.6) in one prospective cohort study. Several other studies have considered associations between ST use and intermediate outcomes (CVD risk factors). CONCLUSIONS: There may be an association between ST use and cardiovascular disease. However, further rigorous studies with adequate sample sizes are required.

Cardiovascular Diseases↗
PubMed2003

Health effects associated with smokeless tobacco: a systematic review.

BACKGROUND: It is believed that health risks associated with smokeless tobacco (ST) use are lower than those with cigarette smoking. A systematic review was therefore carried out to summarise these risks. METHODS: Several electronic databases were searched, supplemented by screening reference lists, smoking related websites, and contacting experts. Analytical observational studies of ST use (cohorts, case-control, cross sectional studies) with a sample size of >/=500 were included if they reported on one or more of the following outcomes (all cause mortality, oral and pharyngeal cancers, other cancers, cardiovascular diseases, dental diseases, pregnancy outcomes, surgical outcomes). Data extraction covered control of confounding, selection of cases and controls, sample size, clear definitions and measurements of the health outcome, and ST use. Selection, extraction and quality assessments were carried out by one or two independent reviewers. RESULTS: A narrative review was carried out. Many of the studies lacked sufficient power to estimate precise risks, mainly due to the small number of ST users. Studies were often not designed to investigate ST use, and many also had major methodological limitations including poor control for cigarette smoking and imprecise measurements of exposure. Studies in India showed a substantial risk of oral or oropharyngeal cancers associated with chewing betel quid and tobacco. Studies from other regions and of other cancer types were not consistent. Few studies have adequately considered the non-cancer health effects of ST use. CONCLUSIONS: Chewing betel quid and tobacco is associated with a substantial risk of oral cancers in India. Most recent studies from the US and Scandinavia are not statistically significant, but moderate positive associations cannot be ruled out due to lack of power. Further rigorous studies with adequate sample sizes are required, especially for cardiovascular disease.

Areca↗
PubMed1978

Disposition of clonidine in rats as determined by radioimmunoassay.

The disposition of the potent antihypertensive drug clonidine has been poorly understood through the lack of a convenient and sensitive assay. A radioimmunoassay for clonidine has been developed and is capable of detecting as little as 10 pg of clonidine. 2,6-Dichlorophenyl-guanidine, a known metabolite of clonidine, did not cross-react with the antiserum whereas another metabolite, 4-hydroxyclonidine, was as potent as clonidine in displacing labeled clonidine from the antibody. However, a simple solvent extraction step before the radioimmunoassay selectively extracted clonidine from a mixture of clonidine and 4-hydroxyclonidine in alkaline plasma and this procedure permitted a specific assay for clonidine. The plasma levels of clonidine in rats after the administration of a hypotensive dose (100 microgram/kg i.v.) were determined by radioimmunoassay and these data indicated that the disposition of clonidine conforms to an open two-compartment, pharmacokinetic model. Clonidine rapidly accumulated in the brain as shown by the attainment of peak concentrations within 2 min of i.v. injection.

Animals↗
PubMed1992

Solid-phase extraction of urinary 11-dehydrothromboxane B2 for reliable determination with radioimmunoassay.

In this paper we elaborate a one-step procedure for the selective extraction of urinary 11-dehydrothromboxane B2 on octylsilyl silica cartridges for reliable determination with radioimmunoassay. The immunoreactivity profile of nonselectively extracted urine after HPLC separation showed that as much as 70% of the total 11-dehydrothromboxane B2 immunoreactivity comigrates with polar interfering material. Its amount could be considerably decreased using acetonitrile:water (18:82, v/v) as wash solvent before elution of 11-dehydrothromboxane B2 from the cartridge. Alternatively, very high immunoreactive purity was achieved without the preceding wash step by selective elution of the analyte with dichloromethane:hexane (70:30). After both optimized steps in the extraction procedure were combined, immunoreactivity was found only in HPLC fractions corresponding to the retention volume of authentic 11-dehydrothromboxane B2. The homogeneity of this immunoreactivity was confirmed by two-step HPLC separation. A significant correlation of values was observed between samples measured after extraction and those measured after subsequent HPLC purification. A high correlation was also found with concentrations determined by radioimmunoassay using four different antisera. The values of 24 h excretion of 11-dehydrothromboxane B2 in 10 male volunteers (595 +/- 114 ng/g creatinine, mean +/- SD) as well as the inhibitory effect of acetylsalicylic acid (80 +/- 13%) closely correspond with those reported in the literature. This selective extraction procedure provides a high validity in radioimmunoassay without requiring any further purification step.

Chromatography, High Pressure Liquid↗
PubMed2005

Fluorescent sensing and selective Pb(II) extraction by a dansylamide ion-exchanger.

The (bis)dansylated sulfonamide 1,2-C6H4(NHSO2C10H6-5-N(CH3)2)2 (1) extracted Pb(II) selectively from water into 1,2-dichloroethane via an ion-exchange mechanism and showed fluorescence quenching upon Pb(II) extraction. The distribution ratios for metal extraction (determined by ICP-MS) for Pb(II) were 133-1410 times higher than those for other metal cations [Co(II), Ni(II), Cu(II), Zn(II), and Cd(II)] under identical conditions. Fluorescence quenching was observed upon Pb(II) extraction, which was dependent on Pb(II) concentration. The monodansylated control, C6H5NHSO2C10H6-5-N(CH3)2 (2), showed neither extraction nor quenching, indicating that the fluorescence effects are a direct result of Pb coordination to 1. The observed selectivity for Pb(II) is ascribed to the formation of a low-coordinate binary Pb(II)-Sulfonamido complex in the organic phase.

Cations, Divalent↗
PubMed2006

Simultaneous extraction and fractionation of polycyclic aromatic hydrocarbons and their oxygenated derivatives in soil using selective pressurized liquid extraction.

In this study, a selective pressurized liquid extraction (PLE) method which can extract polycyclic aromatic hydrocarbons (PAHs) and their oxygenated derivatives (oxy-PAHs) from contaminated soil and simultaneously separate them into two fractions was developed. The method uses extraction cells packed with a chromatographic adsorbent and extraction solvents of increasing polarity. Several experiments were conducted on both spiked and authentic contaminated soil samples. Different types of adsorbents, combinations of extraction solvents, and extraction temperatures were tested in order to find a method that could fulfill the purpose of the study. The final method was based on extraction cells packed with 2% deactivated silica gel. The PAHs were extracted with cyclohexane/dichloromethane (9:1) at 120 degrees C, after which the oxy-PAHs where extracted with cyclohexane/dichloromethane (1:3) at 150 degrees C. The PAHs and oxy-PAHs were efficiently separated into two fractions, and only trace amounts of some compounds were found in the inappropriate fraction. The recoveries of the PAHs were mostly above 70% and of the oxy-PAHs, above 90%. The linearity of the method was good, and the calibration curves for most compounds had a regression coefficient better than 0.99 and an intercept close to the origin of coordinates. When the selective PLE method was applied to seven authentic soil samples, the results were found to be in good agreement with those of a reference method based on Soxhlet extraction and silica gel cleanup and also in good agreement with the certified reference values available for one of the soils. The selective PLE method is faster and consumes less solvent than a traditional method based on separate extraction and fractionation steps. The selective PLE method is, therefore, suitable for the concurrent analysis of PAHs and oxy-PAHs during large-scale soil contamination studies. This will provide more information about the soil contamination and the levels of toxicity than an ordinary PAH analysis.

Journal Article↗
PubMed1998

Validated determination of total arsenic species of toxicological interest (arsenite, arsenate and their metabolites) by atomic absorption spectrometry after separation from dietary arsenic by liquid extraction: toxicological applications.

A validated method for the selective extraction of total As species of toxicological interest (arsenite, arsenate and mono- and dimethylated arsenic species) from urine, followed by atomic absorption spectrometric determination, is described. The mechanisms involved in extraction were studied and the extraction method was optimized. The urine sample was acidified with concentrated HCl and KI and sodium hypophosphite were added. Under these conditions, As species were reduced to their corresponding iodide arsines, extracted with toluene and back-extracted with 1 mmol l-1 NaOH solution. Only inorganic arsenic and its metabolites in humans (monomethylarsonic and dimethylarsinic acid) were extracted. Arsenobetaine of dietary origin was not extracted. This method can detect if any As increase in urine originates from inorganic As intoxication or only from dietary non-toxic As species such as arsenobetaine.

Arsenates↗