Gas chromatographic determination of the pesticide dodemorph for assessment of occupational exposure.

As part of a health hazard survey of occupational exposure to pesticides in greenhouse growing of ornamentals, analytical methods are developed and validated for measurement of exposure of workers to the fungicide dodemorph. A gas chromatographic method is developed using on-column injection and nitrogen-phosphorus detection for quantification. Methods for the determination of (potential) dermal exposure by the analysis of foliar dislodgeable residues and cotton gloves are validated with respect to background, analytical recovery, stability, limit of detection, and between-day coefficients of variation. Analytical recovery from 'foliar dislodgeable residue solutions' and cotton gloves is more than 95%. Dodemorph in 'foliar dislodgeable residue solutions' and on cotton gloves is stable for at least five and six months, respectively, when stored in the refrigerator. Between-day coefficients of variation are 6% for both matrices. The limit of detection is 3 micrograms per leaf sample and 150 micrograms per pair of gloves. Institute of Occupational Medicine (IOM) samplers, designed for the collection of a defined inspirable fraction of aerosols, are tested for sampling air-borne dodemorph. IOM samplers equipped with glass-fiber or cellulose filters appear unsuitable for reliable sampling of the fungicide because of breakthrough or breakdown during sampling.     

High-performance liquid chromatographic determination of n-methylformamide, a biological index for occupational exposure to dimethylformamide.

This report describes an analytical method for the biological monitoring of workers exposed to N,N-dimethylformamide (DMF), a solvent widely used in the chemical industry. The human main metabolites of DMF are N-hydroxymethyl-N-methylformamide (HMMF) and the minor metabolites N-methylformamide (NMF) and N-acetyl-S-(N-methylcarbamoyl)cysteine. The metabolite selected by the American Conference of Governmental Hygienists for occupational biomonitoring purposes, is NMF measured by gas chromatographic analysis, as during it HMMF may be converted to the minor metabolite NMF. HMMF and NFM can be measured independently using HPLC analysis. The procedure proposed here involves the thermal transformation of the primary metabolite HMMF into the minor metabolite NMF, which is then determined by HPLC. This method makes it possible to determine, using HPLC, both metabolites of DMF by measuring only one peak, thus offering two major advantages: (i) it increases the sensitivity of the test and (ii) it deploys only one reference standard.     

High-performance liquid chromatographic determination of 3,5-dimethylhippuric acid in the occupational exposure to trimethylbenzenes.

A high-performance liquid chromatographic method for the measurement of urinary 3,5-dimethylhippuric acid (3,5-DMHA) in the human biological monitoring of the occupational exposure to trimethylbenzenes has been developed. 3,5-DMHA was extracted from urine with ethyl acetate. The organic phase was dried under vacuum and the resultant product, dissolved in the mobile phase, was analysed by an isocratic system and a programmable photodiode-array detector adjusted to 205 nm. The mobile phase was water-acetonitrile (80:20, v/v) containing 0.1% acetic acid. 3,5-DMHA was chromatographed on a reversed-phase Supelco C18 column (3 microns; 15 cm x 0.46 cm I.D.), and identified by its retention time and ultraviolet spectrum. Quantitation was performed by peak area. The detection limit of the method is 30 ng/ml and the recovery and the accuracy are 96%.     

Gas and liquid chromatographic determination of some metals as their di-isobutyldithiocarbamate chelates

Summary Gas and Liquid Chromatographic Determination of Some Metals as Their Di-isobutyldithiocarbamate Chelates Both reversed-phase liquid chromatography and gas chromatography permit the elution of the di-isobutyldithiocarbamate chelates of nickel(II), copper(II) and cobalt(III) at picogram level. The palladium(II) chelate can be used as internal standard. Gas chromatography can easily be applied to determination of these metals in aqueous samples. In the liquid chromatography, contact between any free ligand remaining after extraction and metal traces in the column packing materials or metal components of the system must be minimized before the determinations commence. The results indicate a need for further study of interferences. Di-isobutyldithiocarbamate appears to be a suitable chelating agent for use in both Chromatographic methods.     

Gas chromatographic determination of impurities in nitromethane

Summary Impurities in commercially available nitromethane have been determined by gas-liquid chromatography using six different column packings. Besides nitromethane, 1-nitropropane, 2-nitropropane, acetonitrile, methanol, small amounts of ethanol and acetaldehyde have been detected. The presence of formaldehyde, ethyl acetate and acetone is probable. Mixtures containing comparable amounts of the four nitroalkanes could be separated on all columns, but plots of logarithms of the retention times vs. carbon number or boiling points of the nitroalkanes or column temperatures were linear only in case of columns packed with Porapak R and Q.     

Gas chromatographic determination of propyphenazone in plasma

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Combined immunological and thin-layer chromatographic method of the determination of morphine

     

Gas chromatographic determination of xanthinol in plasma

The determination of xanthinol in plasma is described. After extraction of the drug, together with the internal standard (papaverine hydrochloride), the extract is evaporated to dryness and the drug is derivatized with acetic anhydride for chromatography. The method is linear for 2–100μg ml^-1 ; the coefficient of variation is 3% and the recovery 80%. The resulting stable solution allows large numbers of samples to be processed with an automatic injector.     

Stability-indicating chromatographic methods for the determination of some oxicams

Two sensitive and selective methods were developed for the determination of some oxicams, namely, lornoxicam (LOX), tenoxicam (TEX), and meloxicam (MEX), in the presence of their alkaline degradation products. The first method is based on the thin-layer chromatographic separation of the 3 drugs from their alkaline degradation products, followed by densitometric measurement of the intact drug spots for LOX, TEX, and MEX at 380, 370, and 364 nm, respectively. The developing systems used for separation are ethyl acetate-methanol-26% ammonia (17 + 3 + 0.35, v/v/v) for LOX and TEX and chloroform-n-hexane-96.0% acetic acid (18 + 1 + 1, v/v/v) for MEX. The linear ranges were 0.25-6.0 microg/spot for LOX and TEX and 0.5-10 microg/spot for MEX, with mean recoveries of 99.80 +/- 1.32, 100.57 +/- 1.34, and 100.71 +/- 1.57%, respectively. The second method is based on the liquid chromatographic separation of the 3 drugs from their alkaline degradation products on a reversed-phase C18 column, using mobile phases of methanol-acetonitrile-acetate buffer, pH 4.6 (4.5 + 0.5 + 5.0, v/v/v) for LOX and MEX and methanol-acetonitrile-acetate buffer, pH 4.6 (1.9 + 0.1 + 3.0, v/v/v) for TEX at ambient temperature. Quantification is achieved by UV detection at 280 nm, based on peak area. The linear ranges were 0.5-20 microg/mL for LOX and TEX and 1.25-50 microg/mL for MEX, with mean recoveries of 99.81 +/- 1.01, 98.90 +/- 1.61, and 100.86 +/- 1.55%, respectively. The methods were validated according to guidelines of the International Conference on Harmonization. The developed methods were successfully applied to the determination of LOX, TEX, and MEX in bulk powder, laboratory-prepared mixtures containing different percentages of degradation products, and pharmaceutical dosage forms.     

Gas chromatographic determination of epichlorohydrin in workplace atmospheres

Summary A new method has been developed for the determination of trace amounts of epichlorohydrin in workplace atmospheres. Collection is peroormed in two bubblers in series both containing dichloromethane. Optimum conditions for sampling and analysis have been established. The lower limit of determination is 0.05 g/mL with an RSD of ±5%.