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Biomedical subjects

W Holak

Publications and source records attributed to W Holak.

15 recordsLinked to original sources
PubMed1979

Differential pulse polarographic analysis of thyroid hormone: determination of iodine, thyroxine, and liothyronine.

A differential pulse polarographic method for the analysis of thyroid and thyroid tablets for total iodine, thyroxine, and liothyronine is described. The procedure for iodine, which is also applicable to individual tablet assay, consists of ashing the sample, coverting iodide to iodate, and analyzing by differential pulse polarography. The procedure for thyroxine and liothyronine involves hydrolysis of the sample with barium hydroxide and isolation and separation of the iodoamino acids using ion exchangers, followed by differential pulse polarographic determination in a supporting electrolyte composed of 0.5 N Na2CO3 in 20% 2-propanol containing 1% tetrabutylammonium bromide. The differential pulse polarographic results for iodine agree with values obtained using the USP XIX procedure, and the quantities of thyroxine and liothyronine found agree with literature values.

Iodine↗
PubMed1977

Temperature-programmable furnace for ashing of foods in trace metal analysis.

The use of programmable furnace in preparing samples for determining cadmium, lead, copper, and zinc by differential pulse anodic stripping voltammetry or atomic absorption spectrophotometry is convenient and time-saving. Recovery data for these 4 metals in various foods (tuna, sardines, and milk) were 93-96% for 0.01-1 ppm cadmium, 96-114% for 0.05-5 ppm lead, 100-108% for 2-10 ppm copper, and 97% for 10 ppm zinc.

Animals↗
PubMed1976

Collaborative study of effect of light on cadmium and lead leaching from ceramic glazes.

A limited interlaboratory study was carried out to determine the effect of lighting conditions on the release of cadmium from ceramic glazes by 4% acetic acid. Cadmium release increased with increased exposure to light. Further interlaboratory study on plates manufactured under controlled conditions showed that if temperature, intensity of illumination, and time of exposure are specified, reproducible results for leaching of both lead and cadmium can be obtained. A modification of the official AOAC method, 25.031-25.034, to increase sensitivity was collaboratively studied by 8 laboratories. Each received 6 solutions of lead in 4% acetic acid (3 sets of blind duplicates at the 0.1, 0.5, and 0.8 mug/ml levels) plus a reagent blank. Average recoveries were 0.1006, 0.5056, and 0.8194 mug/ml, respectively, with coefficients of variation of 11.4, 3.3, and 2.8%, respectively. The proposed modification has been adopted as official first action, and a parameter for exposure to light during extraction has been included in the method.

Cadmium↗
PubMed1976

Drugs. Differential pulse polarography of cacodylate injections.

A method was developed for the analysis of cacodylate injections, using differential pulse polarography for measuring As(III). The cacodylate molecule is decomposed to As(V) by heating with Mg(NO3)2.6H20; As(V) is then chemically reduced to As(III) and polarographed in 1M HCl supporting electrolyte. The method of standard addition is used for quantitation. Recoveries based on the analysis of synthetic cacodylic acid solutions containing approximately 9 mg arsenic/ml ranged from 99.1 to 101.7%.

Arsenic↗
PubMed1975

Collaborative study of the determination of boric acid in caviar by emission spectroscopy.

Caviar samples were spiked at the 0.1 and 0.2% levels and digested with nitric acid in a closed Teflon-lined digestion vessel to prevent volatility losses. The boron was complexed with 2-ethyl-1,3-hexanediol and extracted into methylisobulty ketone. The emission of the boron oxide band was measured in a nitrous oxidehydrogen flame. The mean recoveries at the 0.1 and 0.2% levels for 6 collaborators were 95.7 and 97.1%, respectively.

Boric Acids↗
PubMed1975

Determination of heavy metals in foods by anodic stripping voltammetry after sample decomposition with sodium and potassium nitrate fusion.

A method is described for the simultaneous determination of several heavy metals in foods. The sample is predigested with nitric acid and decomposed completely by heating with a mixture of sodium and potassium nitrates. The resultant melt containing the metals is then dissolved in dilute nitric acid. After the pH is adjusted to an appropriate value, the metals, such as cadmium, copper, lead, and zinc, are determined by anodic stripping voltammetry. The average recoveries of these metals added to 5 commodities were 98, 98,96, and 104%, respectively. The relative standard deviations, based on data from analyses of a commodity containing measurable levels of copper, lead, and zinc, were 12.0, 13.0, and 9.7%, respectively.

Cadmium↗
PubMedDate not supplied

Liquid chromatographic-atomic absorption spectrophotometric method for determination of methyl mercury in seafood: collaborative study.

A previously developed method that uses a simplified sample preparation procedure and atomic absorption detection of liquid chromatographic eluates for the determination of methyl mercury in seafood has been collaboratively studied. The unique feature of the method involves the use of a specially designed interface for the generation of mercury vapor. Methyl mercury is isolated from the blended sample by chloroform elution from a diatomaceous earth-hydrochloric acid column. The organomercury compound is then extracted into a small volume of 0.01M sodium thiosulfate solution. An aliquot of this solution is injected onto a Zorbax ODS column and eluted with methanol-ammonium acetate solution (3 + 2), pH 5.7, containing 0.01% mercaptoethanol. Mercury is detected by flameless atomic absorption spectrophotometry using the interface. The samples analyzed in the study were unspiked swordfish, unspiked and spiked lobster, and unspiked and spiked tuna. The spiked samples contained methyl mercury both above and below the U.S. Food and Drug Administration guideline level of 1 microgram Hg/g. Reproducibility relative standard deviations ranged from 10.5% at 1 microgram Hg/g to 18.2% at about 0.1 microgram Hg/g. Accuracy, measured by comparison to reference values obtained by the Associate Referee, ranged from 94.4 to 99.6%. The method has been adopted official first action.

Animals↗
PubMedDate not supplied

Determination of sulfites in foods by simultaneous nitrogen purging and differential pulse polarography.

An improved technique has been developed for determination of sulfites in food by differential pulse polarography. A Teflon sleeve is fitted to the dropping mercury electrode capillary so that SO2 is purged from the sample and simultaneously detected at peak potential. Bound sulfite in the sample is released at room temperature by addition of base in the absence of oxygen. For some foods, the prepared sample was passed through a Sep-Pak C-18 cartridge to remove naturally occurring sulfur compounds so that only added sulfite is measured. The level of detection was approximately 1 microgram SO2/g. Results agreed with those obtained by the optimized Monier-Williams method for a variety of foods.

Food Analysis↗
PubMedDate not supplied

Interference by tin in AOAC dry-ash voltammetric method for determination of lead and cadmium in canned foods.

When lead and cadmium were determined in samples of canned food by the AOAC anodic stripping voltammetric method, an interference was observed which was believed to be tin(IV). This interference could cause false positive results for lead and cadmium. The electroactivity of tin(IV) was suppressed by increasing the concentration of tartaric acid in the supporting electrolyte from 0.005M to 0.1M after mixing with an equal volume of sample solution.

Cadmium↗
PubMedDate not supplied

Differential pulse polarographic determination of sulfites in foods: collaborative study.

A differential pulse polarographic (DPP) method for the determination of "free" and "total" sulfite in foods was collaboratively studied by 8 laboratories. The collaborators analyzed blind duplicate samples of shrimp, orange juice, peas, dried apricots, and dehydrated potatoes. Collaborators also analyzed the same samples spiked with sulfites at 2 levels, which ranged from 10 to 1100 micrograms added SO2/g. The variability of free SO2 results was excessive for quantitative analysis, but the method can be used for qualitative detection of free SO2. The method for total SO2 determination was suitable for as low as approximately 10 micrograms/g. Recoveries are comparable to those for the official Monier-Williams method at high levels and are superior at low levels. The method has been adopted official first action for determination of total SO2 in the foods studied.

Analysis of Variance↗