Microtox testing of pentachlorophenol in soil extracts and quantification by capillary electrochromatography (CEC)--a rapid screening approach for contaminated land.

An approach to rapid soil testing which involved the use of simple solvent extraction methods was developed. The analytes of interest were priority pollutants of low water solubility which could not be readily removed from the soil using water. Direct toxicity testing of the soil samples by Microtox showed a high background toxicity which prevented realistic toxicity data from being obtained for the contaminants present. A range of different extraction solutions was used in an attempt to extract the contaminants while eliminating the matrix effects of the soil. It was necessary that the solvents selected for extraction of the soil samples were not of significant toxicity, as this could potentially mask the toxic effects of any compounds extracted from the soil. The extraction efficiencies of solvent systems were evaluated using pentachlorophenol (PCP) as a model compound of known toxicity in the Microtox assay. A rapid and cost-effective method was developed in order to determine the amount of PCP recovered from the soil by the extraction solvents employed. This method consisted of a solid phase extraction (SPE) step followed by quantification using capillary electrochromatography (CEC). Recoveries were greater when a higher proportion of organic solvent (methanol) was used in the extraction process, and lowest when water was used. An extraction based on water could provide information on the potential for leaching of contaminants from the soil into nearby water bodies in an environmental setting. An organic solvent extraction method could indicate how much toxicity soil-dependent organisms might be exposed to through ingestion. Extraction based on 50% (v/v) methanol in water was considered to be the most suitable overall extraction solution for soil screening, given that this permitted extraction of the water-insoluble compound PCP at a level which was clearly toxic in the Microtox assay while also retaining the capability to extract water-soluble contaminants.

The effects of commonly used adulterants on the detection of spiked LSD by an enzyme immunoassay.

The effects of 15 chemicals and household agents on an enzyme immunoassay (EIA) for LSD were investigated. The presence of many of these was detected by pH and specific gravity measurements and by sample inspection. A number of agents caused false positives in the assay at 10% adulteration, but only two produced false positive results at 1%. Adulterated samples spiked with LSD produced no false negatives, demonstrating that none of the adulterants tested were able to conceal the presence of LSD by interfering with the EIA. The assay is shown to be a robust method for the screening of urine for LSD when used in conjunction with sample inspection and a sound confirmatory method.

Development and validation of a nonisotopic immunoassay for the detection of LSD in human urine.

A microplate enzyme immunoassay (EIA) for the detection of lysergic acid diethylamide (LSD) in human urine was developed. The assay kit is designed around an LSD derivative coated on the wall of microplate wells with preservatives and stabilizers. Sample and rabbit anti-LSD are added to the microplate well. The immobilized LSD and LSD present in specimens compete for the opportunity to bind to the anti-LSD antibodies. An anti-rabbit antibody labeled with horseradish peroxidase is used to provide the assay signal, which is inversely proportional to the concentration of LSD in the sample. The assay requires a 25-microL urine sample and three consecutive incubation periods of 60, 30, and 30 min at room temperature. The assay was tested with a variety of drugs, including ergot alkaloids spiked into drug-free urine at up to 100,000 ng/mL without cross-reaction. Nor-LSD was shown to cross-react between 16% and 28%, depending on its concentration. Of the other compounds tested, only ergonovine demonstrated slight cross-reactivity at approximately 0.0008%. The assay is designed to be used with a qualitative cutoff of 0.5 ng/mL. Precision testing at 0.5 ng/mL gave a coefficient of variation (CV) of 6% based on 20 replicates. The CV at 0.375 ng/mL (cutoff, -25%) was 5.2% and at 0.625 ng/mL was 6.6%. Precision at other concentrations within the range of the calibration curve gave similar results both intra- and interassay. Clinical performance of the assay was compared with that of a commercial radioimmunoassay (RIA). Comparable performance was observed with both methods, each screening a total of 458 samples as negative and 17 samples as positive relative to a 0.5 ng/mL cutoff. The EIA found an additional three positive samples that were negative by RIA. The EIA is suitable for the screening of urine samples for the presence of LSD. Preliminary indications are that the assay is also suitable for use with whole blood specimens. The assay can be performed manually or be fully automated and without the need for radioactivity; it can be used in any laboratory.

Development of a stand-alone affinity clean-up for lysergic acid diethylamide in urine.

A total analysis scheme for lysergic acid diethylamide (LSD) from human urine is described. A simple ELISA technique led to the development and optimization of an affinity clean-up cartridge, resulting in high purification factors with a single combined extraction/clean-up step. LSD can be measured with a straightforward HPLC-fluorescence technique, which minimizes operating complexity and process implementation time. The method has been applied to urine containing 0.5 ng ml-1 LDS, and the ability of high-affinity materials to preconcentrate a sample into a small volume should allow the working range of the procedure to be adjusted as required.

Microband electrodes fabricated by screen printing processes: Applications in electroanalysis.

A novel method for the simple and cheap manufacture of microband and multiple microband electrodes is described. The construction technique is based entirely on the screen printing of the surface of alumina tiles with conducting and insulating ink materials. The range of potentials over which the electrodes may be used has been determined by basic electrochemical studies. These electrode systems have been used successfully for the measurement of vitamin C, vitamin B(1) and paracetamol, which illustrates, their potential as useful tools in the field of electroanalysis.