Objective of this work was determination of processing contaminant known as 3-MCPD (3-chloropropa-ne-1,2-diol) in its free and bound form in breads with defined parameters of processing. Selected and analysed were 24 samples, which represented two sets of breads produced in bakeries equipped with a continual line. In all cases determinations were carried out for breadcrumb and crust separately. The first set of samples were wheat-rye breads produced chronologically in ten days in the bakery Michelská pekárna, slightly different in temperatures and times of baking. The second set contained 14 samples of wheat-rye breads with a content of rye flour less than 40% differing in the yeast type and acidity. These breads were produced in the bakery Kontinua. The fat content was determined in all samples by Soxhlet extraction. Free and bound 3-MCPD was determined by gas chromatography-mass spectrometry method. Concentration of free 3-MCPD in samples was at interval < 9-54.5 µg/kg. Concentration of bound 3-MCPD was at interval 1.56-23.60 mg/kg of fat (i.e. 5.7-84.9 µg/kg of sample).
The objective of our study was to compare three vastly different analytical methods for measuring urinary metabolites of pyrethroid and pyrethrum insecticides to determine whether they could produce comparable data and to determine if similar analytical characteristics of the methods could be obtained by a secondary laboratory. This study was conducted as a part of a series of validation studies undertaken by the German Research Foundation's Committee on the Standardization of Analytical Methods for Occupational and Environmental Medicine. We compared methods using different sample preparation methods (liquid-liquid extraction and solid-phase extraction with and without chemical derivatization) and different analytical detection methods (gas chromatography-mass spectrometry (single quadrupole), gas chromatography-high resolution mass spectrometry (magnetic sector) in both electron impact ionization and negative chemical ionization modes, and high-performance liquid chromatography-tandem mass spectrometry (triple quadrupole) with electrospray ionization). Our cross validation proved that similar analytical characteristics could be obtained with any combination of sample preparation/analytical detection method and that all methods produced comparable analytical results on unknown urine samples.
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