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Biomedical subjects

A Kettrup

Publications and source records attributed to A Kettrup.

At least 73 records · Page 4Linked to original sources
PubMed2001

Simultaneous determination of sixteen phenylurea herbicides in water by high performance liquid chromatography and solid phase extraction.

A high performance liquid chromatography (HPLC) procedure for simultaneous determination of sixteen phenylurea herbicides in water is described. A Lichrospher 100 RP-18e column and spectrophotometric detection at 240 nm were used. Adequate retention was achieved with a mobile phase of acetonitrile/water solution with gradient elution. The HPLC analysis time was less than 20 min. The herbicides were isolated from water samples by using a single solid phase extraction procedure with C18 solid-phase columns. An enrichment factor of 1,000 was achieved. Recoveries were in the range between 87.8% and 103.7%. The detection limits of the whole procedure achieved were less than one-tenth of the maximum limit permitted by the European Community standard for drinking water.

Chromatography, Gas↗
PubMed2000

Study of the copper distribution in contaminated soils of hop fields by single and sequential extraction procedures.

Hop growing in Bavaria requires the use of copper containing fungicides against mildew, which results in an accumulation of copper in the upper soils to concentrations of up to approximately 450 mg kg(-1). The naturally occurring concentration of copper is approximately 10-15 times lower. Several single and sequential extractions were performed in parallel to the determination of total copper content after aqua regia digestion. By these means copper mobility and retention, its availability to plants as well as its distribution in soils was assessed. Three agricultural soils and two soils from fallow land have been analysed to elucidate whether the copper distribution changes in relation to agricultural activities and to predict environmental risks due to the high copper concentrations. This work also focuses on the difficulties arising from different results when using single and sequential extraction procedures. EDTA, acetic acid, deionised water, ammonium nitrate and calcium chloride were used as single extractants for the functionally defined speciation. EDTA and acetic acid can be regarded as extractants for the plant-available species, while deionised water, NH4NO3 and CaCl2 only release electrostatically weakly bound metals to estimate the mobile species. The extraction behaviour of copper in these procedures is discussed with respect to the quantities extracted from the contaminated and non-contaminated soils. The studies indicate that no vertical copper translocation is observed in the ground, but the main amounts are highly available to plants. Sequential extraction procedures were used for operationally defined speciation, quantifying copper in specific soil phases. The 'five-step extraction scheme' first applied, suggested by the Standard Measurement and Testing Programme of the European Community, overestimated the amounts of copper bound to the residual phase. This was mainly due to the non-specific nature of the reagents for the organic/sulfidic and crystalline iron oxide fraction. A second reason could be the fact that this scheme was developed for sediment and not for soil analysis. Therefore, the sequential extraction has been applied using an adapted method of Zeien and Bruemmer, using different extractants for the two phases. The copper distribution was different, showing that approximately 40-50% of the total copper was bound to the organic fraction and approximately 15-30% could be extracted with the iron oxides. The amounts in the residual fraction were much lower. After comparing the results of the different extraction procedures the environmental behaviour of copper and its risks for plants, micro-organisms and groundwater is discussed in brief.

Agriculture↗
PubMed2000

Analysis of agrochemicals by capillary electrophoresis.

An increasing amount of articles using capillary electrophoresis as an investigation tool for pesticides and environmental pollutants were found over the last few years in analytical chemistry oriented journals. This review covers a wide literature range of the 1990s and concentrates on the analysis of organic agrochemicals (herbicides, fungicides, insecticides, acaricides, etc.) with capillary electrophoresis (capillary zone electrophoresis, micellar electrokinetic chromatography with CE-UV-visible or laser-induced fluorescence detection) as well as with the on-coming hyphenated techniques like capillary electrophoresis-electrospray ionization mass spectrometry. The principal preconcentration methods that allowed real sample analysis with CE are also briefly discussed. The pesticides, the separation methods, the used electrolytes, the detection types, the detection limits and the preconcentration methods were classified and presented in tabulated form as a rapid information tool.

Agrochemicals↗
PubMed2000

Long-term monitoring of arsenic and selenium species in contaminated groundwaters by HPLC and HG-AAS.

The long-term concentration and distribution of species of arsenic and selenium in contaminated groundwaters from Kelheim was monitored. Most of the groundwater wells contained elevated concentrations of iron, manganese and sulfur. Arsenic (III), arsenic (V), selenium (IV) and selenium (VI) were separated using high performance liquid chromatography (HPLC) based on phosphate buffers and collected in fractions. Due to the complex matrix, the fractions were analyzed element-specifically by hydride-generating atomic absorption spectrometry (HG-AAS). The combination of HPLC and HG-AAS was selected due to the authors' intention of developing an easy-to-handle, but nonetheless reliable, method suitable for the long-term monitoring of species distribution in an almost routine way, and taking account of the threshold values of 10 microg/l for each element, indicated by German drinking water regulations. To enhance the reliability of the method, analytical quality control experiments were carried out. When applied to groundwater wells from Kelheim (Germany) they revealed that arsenic (V) and selenium (VI) were the dominating species. The presence of arsenic (III) and selenium (IV) was assumed to be supported by organic matter.

Arsenic↗
PubMed2000

Pentachlorophenol in indoor environments. Correlation of PCP concentrations in air and settled dust from floors.

The investigation of settled dust is a proven and simple screening-method for considering indoor contamination for semivolatile compounds. Here we investigate the correlation of PCP concentrations in air and freshly settled dust from floors. Air and dust samples were taken from 75 rooms in 30 buildings with suspicion of an application of PCP-containing wood preservatives. Sampling was repeated four times within 18 months. PCP air concentrations were found in the range of <0.3-576 ng m-3 (mean value 25.3 ng m-3, median 2.5 ng m-3). PCP dust concentrations were found in the range of 0.083-79 microg g-1 (mean value 3.5 microg g-1, median 1.1 microg g-1. A weak highly significant correlation (P < 0.0001) with a correlation coefficient of R2 = 0.433, of the PCP concentration in dust with the PCP concentration in air, was observed. Measurement of PCP concentrations in dust, therefore, is a suitable screening method for the evaluation of indoor contamination with PCP. Due to the high dispersion of the data it is not possible to calculate PCP concentrations in air from concentrations in dust although a highly significant correlation of the PCP concentrations in air and dust was found.

Air Movements↗
PubMed2000

Determination of basic nitrogen-containing polynuclear aromatic hydrocarbons formed during thermal degradation of polymers by high-performance liquid chromatography-fluorescence detection.

A method for the simultaneous determination of 22 nitrogen-containing polynuclear aromatic hydrocarbons (PAHs) (15 azaarenes and seven amino-PAHs) in the gaseous products of the thermal degradation of polymers is described. After desorption and clean-up using cation-exchange chromatography (PRS cartridge) the samples were analyzed by HPLC-FD. The validation was carried out with real nylon 6 combustion samples. The recoveries of the compounds are in the range of 89-99% for the extraction and 91-100% for the clean up procedure. The detection limits ranged from 7 to 160 pg. The high recovery values, due to the quick and efficient clean-up procedure, resulted in low relative standard deviations (with the exception of acridine and 2-aminoanthracene <5%). The applicability of the method is also investigated for the determination of the N-PAHs in a pyrolysis sample.

Chromatography, High Pressure Liquid↗
PubMed2000

Analysis of cyanogenic glycosides by micellar capillary electrophoresis.

The separation of amygdalin, prunasin and their isomers neoamygdalin and sambunigrin could be achieved with micellar capillary electrophoresis (MEKC). The two isomers were obtained in alkaline conditions and were produced in less than 15 min at pH 11.0. The developed methods showed a good selectivity in the separation of the isomers only in the presence of SDS micelles. The working pH was optimized to allow best resolution and quantitative analysis of these compounds. With a linear calibration over an injection time from 1 to 20 s, the detection limit was found to be in the range of 5 microM (S/N=3; 20 s injection time). Two pH buffer systems (pH 5.2 and pH 9.1) were chosen to confirm the peak attributions of the compounds in the apple and peach seeds samples. Sambunigrin was found in both apple and peach seeds but could not be quantified because of missing standards. Prunasin and amygdalin were not found in the apple sample, while they were quantified in the peach seeds in concentrations of 50 microg/g and 90 microg/g (dry weight), respectively.

Amygdalin↗
PubMed2000

Distribution, transformation, and long-term accumulation of polychlorinated dibenzo-p-dioxins and dibenzofurans in different tissues of fish and piscivorous birds.

The present study monitored 10-year-old fish and piscivorous birds from sites contaminated for many years. The data reflected the results of actual, long-term environmental exposures. The results demonstrate that different tissues of fish have quite different concentrations of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/F). The concentration order of PCDD/F within fish is liver congruent with egg congruent with intestine>kidney congruent with heart>gill congruent with bladder>muscle>brain. The concentration order of PCDD/F within piscivorous birds was liver>egg congruent with heart>muscle congruent with stomach>brain. The results obtained also demonstrate that the accumulation patterns of piscivorous birds and fish are quite different. The tissues of fish and piscivorous birds have different capacities for bioaccumulation and biotransformation of PCDD/F; variable proportions of TEQs were also found throughout their bodies. In fish, toxic equivalency quotient (TEQ): PCDD/F ratios in various tissues ranged from 0.01 to 0.07, whereas in birds the ratios ranged from 0.07 to 0.43. If the concentrations are normalized with lipid content, the results vary less. The effect of different lipid properties is obvious in the case of brain tissue, which is richer in phospholipids.

Animals↗
PubMed2000

River sediment (S-37)--a new analytical quality control material ensuring comparability of chlorinated hydrocarbon analysis during an international environmental study in China.

A sediment reference material (S-37) was prepared as analytical quality control material to be used within an international project on polychlorinated hydrocarbon analysis in two Chinese rivers. The raw material was sampled during a cruise on Yangtse River and transported afterwards to the JRC Ispra for further processing. The material was treated according to the general principles applicable for candidate reference material production. After a thorough homogeneity study of the bulk the material was bottled. A total of 1,080 bottles each containing 50 g of dry sediment powder was obtained. Final homogeneity and stability testing proved the material to be fit for the purpose. Isotope dilution GC/MS was used to establish target values for pentachlorobenzene (1.17 +/- 0.08 ng/g), hexachlorobenzene (3.60 +/- 0.17 ng/g), octachlorostyrene (0.19 +/- 0.01 ng/g), pentachloroanisole (0.52 +/- 0.02 ng/g), alpha-HCH (0.70 +/- 0.05 ng/g), beta-HCH (1.38 +/- 0.18 ng/g), gamma-HCH (0.83 +/- 038 ng/g), 2,4'-DDT (0.36 +/- 0.04 ng/g), 2,4'-DDE (0.29 +/- 0.02 ng/g), 2,4'-DDD (0.49 +/- 0.02), 4,4'-DDT (3.42 +/- 0.47 ng/g), 4,4'-DDD (1.29 +/- 0.17 ng/g), PCB 28 (0.11 +/- 0.01 ng/g), PCB 52 (0.09 +/- 0.003 ng/g), PCB 101 (0.07 +/- 0.003 ng/g), PCB 138 (0.06 +/- 0.003 ng/g) and PCB 153 (0.06 +/- 0.003 ng/g). Furthermore, indicative values for major and minor constituents as well as for polychlorinated dibenzodioxines and -furanes were measured.

China↗
PubMed2000

On the presence of PCDD/Fs and other chlorinated hydrocarbons in the second generation of the European Reference Soil Set--the EUROSOILS.

The second generation of the European Reference Soil-Set, the so-called EUROSOILS, has been introduced recently. The presence of organic micro-pollutants in this new type of reference materials has already been studied for polycyclic aromatic hydrocarbons, triazines, phenylureas and other pesticides. The already large amount of data concerning the level of different contaminants, the elemental composition and matrix properties is completed by a survey by means of GC/MS on the polychlorinated dibenzodioxins/furans (PCDD/Fs) and other chlorinated hydrocarbons. Higher concentrations for 4,4'-DDT in EUROSOIL 2 (10.57 +/- 0.02 ng/g), for dieldrin in EUROSOIL 3 (8.85 +/- 0.87 ng/g) and for heptachlor-epoxide in EUROSOIL 4 (5.86 +/- 0.16 ng/g) could be detected. Sum concentrations for PCDD/Fs were 15.02 ng/kg (EUROSOIL 1), 214.29 ng/kg (EUROSOIL 2), 873.32 ng/kg (EUROSOIL 3), 54.47 ng/kg (EUROSOIL 4) and 119.61 ng/kg (EUROSOIL 5).

Benzofurans↗
PubMed2000

Direct observation of the formation of aromatic pollutants in waste incineration flue gases by on-line REMPI-TOFMS laser mass spectrometry.

On-line REMPI-TOFMS laser mass spectrometry (Resonance Enhanced Multi-Photon Ionization-Time-Of-Flight Mass Spectrometry) was used to monitor combustion and pyrolysis byproducts from industrial combustion processes, including polycyclic aromatic hydrocarbons (PAH) and monochlorobenzene in the flue gas of an industrial 22 MW hazardous waste incineration plant. Sampling at different places in the flue gas stream revealed the complexity of the processes responsible for the formation of the different chemical species, while time resolved measurements depicted the emission dynamics.

Air Pollutants↗
PubMed2000

Estimation of soil adsorption coefficients of organic compounds by HPLC screening using the second generation of the European reference soil set.

The European reference soil set was introduced as common basis for a better comparability of soil sorption data measured within the framework of chemical testing of environmental chemicals. The success of the EUROSOILS, as the set is commonly called, convinced the European Commission's Joint Research Centre to evaluate the possibility of producing a remake of these unique and new type of reference materials maintaining the principal sorption-controlling properties of the soils. In this paper the recently proposed second generation of the EUROSOILS is used to evaluate a HPLC-screening technique for the estimation of soil adsorption coefficients of organic chemicals. It could be shown that the derived correlations between HPLC capacity factors of the test substances and the respective soil adsorption coefficients resulting from batch experiments with the second version of the EUROSOILS agreed with those derived for the first generation of reference soils at a different occasion.

Adsorption↗
PubMed2000

A new method of predicting of gas chromatographic retention indices for polychlorinated dibenzofurans (PCDFs).

A new method has been developed to describe the quantitative relationship between molecular structures of PCDFs and their gas chromatographic retention indices on a 30-m fused silica column coated with DB-5 stationary phase. The regression equation is derived with a multiple correlation coefficient greater than 0.9995. The highest residual is 20 index units. The standard deviation is less than 7 index units. Using this regression equation, the retention indices of PCDFs for which data is not available have also been predicted.

Benzofurans↗
PubMed2000

Copper-catalyzed chlorination and condensation of acetylene and dichloroacetylene.

The chlorination and condensation of acetylene at low temperatures is demonstrated using copper chlorides as chlorinated agents coated to model borosilicate surfaces. Experiments with and without both a chlorine source and borosilicate surfaces indicate the absence of gas-phase and gas-surface reactions. Chlorination and condensation occur only in the presence of the copper catalyst. C2 through C8 organic products were observed in the effluent; PCDD/F were only observed from extraction of the borosilicate surfaces. A global reaction model is proposed that is consistent with the observed product distributions. Similar experiments with dichloroacetylene indicate greater reactivity in the absence of the copper catalyst. Reaction is observed in the gas-phase and in the presence of borosilicate surfaces at low temperatures. The formation of hexachlorobenzene is only observed in the presence of a copper catalyst. PCDD/F were only observed from extraction of the borosilicate surfaces. A global reaction model is proposed for the formation of hexachlorobenzene from dichloroacetylene.

Acetylene↗
PubMed2000

Kinetics of nitromusk compounds degradation in water by ultraviolet radiation and hydrogen peroxide.

The photodegradation of five representative nitromusk compounds in water has been performed in a stirred batch photoreactor with a UV low-pressure immersed mercury lamp, at constant temperature and different doses of hydrogen peroxide. The rate constants have been calculated on the basis of experimental data and a postulated first-order kinetic model. The rate constants, at 298 K and a dose of 1.1746 micromol l(-1) H2O2 ranges from 0.3567 x 10(-3) s(-1) for musk tibetene, to 1.785 x 10(-3) s(-1) for musk ambrette.

Dinitrobenzenes↗
PubMed2000

Peak identification for PCDD/Fs in environmental samples at different temperature programs.

A method has been developed for peak recognition of 136 polychlorinated dibenzo-p-dioxins (PCDDs) and polychlorinated dibenzofurans (PCDFs) at different temperature programs. Their retention behaviours are predicted on the basis of an identification database of retention values (A, B) of gas chromatography. By the retention times of 13C labelled 2,3,7,8-substituted PCDD/F internal standards, the retentions of all PCDDs and PCDFs can be calculated. After comparison with the retentions of practical environmental samples, the predicted values have been proved to be very accurate.

Benzofurans↗