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Open access

Józef Szkoda, Jan Żmudzki, Agnieszka Nawrocka and Mirosława Kmiecik

Abstract

The aim of the study was to evaluate the contamination of animal muscle, liver, and milk with lead, cadmium, mercury, and arsenic. Determination of the elements was carried out using several techniques of atomic absorption spectrometry. Between 2008 and 2012, samples of muscles and liver from 1305 cattle, 2345 pigs, 758 horses (only muscles), 1721 poultry (chickens, turkeys, geese, ducks), and 736 samples of raw milk were collected. Only 48 (0.7%) samples exceeded the maximum acceptable levels of the elements, especially lead and cadmium. In the case of lead, the highest number of samples exceeding the legal limits was found in muscles of pigs (6), where the maximum value reached 0.376 mg/kg. For cadmium, the highest number of samples (22) with values exceeding legal limits was found in muscles of horses. The cadmium content in muscles of horses, at both the mean (0.052 mg/kg) and median (0.023 mg/kg), was in order of magnitude higher than that observed in cattle and pigs. Small percentage of samples with values exceeding the maximum levels of toxic elements in food of animal origin indicates a low risk for the consumers’ health.

Open access

Anna Gajda, Andrzej Posyniak, Andrzej Bober, Tomasz Błądek and Jan Żmudzki

Summary

A liquid chromatography method with UV detection for determination of oxytetracycline (OTC) in honey has been developed. The samples were extracted with the solution of oxalic acid. The clean-up procedure was performed by solid phase extraction (SPE) using polymeric Strata X and carboxylic acid cartridges. Chromatographic separation was carried out on the Luna C8 analytical column with mobile phase consisting of acetonitrile-0.02 M oxalic acid. The method has been successfully validated according to the requirements of the European Decision 2002/657/EC and this method is used in routine control of oxytetracycline in honey samples. The limit of detection (LOD) and limit of quantification (LOQ) of the presented method were 10 and 12.5 μg/kg, respectively. The developed method has also been verified in quantitative determination of oxytetracycline residues in honey after experimental treatment with this product in bee colonies.

Open access

Henryka Wiśniewska-Dmytrow, Jan Żmudzki, Olga Burek and Katarzyna Pietruszka

Abstract

Between 2003 and 2012, 1413 samples of kidneys, liver, and muscles from swine, cattle, sheep, horses, chickens, turkeys, geese, ducks, and fish were examined for the presence of ochratoxin A. The examination was performed in the framework of “The National Residue Control Programme for Chemical, Biological, and Drug Residue in Animal Tissues and in the Food of Animal Origin”. The mycotoxin was determined by liquid chromatography with fluorescence detection after immunoaffinity column clean up. The limit of quantification was 0.2 μg/kg. Ochratoxin A was found only in swine kidney samples (n = 1092). It was detected in 28.8% of the kidney samples at the concentrations from 0.2 to 29.2 μg/kg. The most of the samples (25.5%) contained OTA at the concentration ranging from 0.2 to 5 μg/kg, which is below the provisional action level for OTA in kidneys, established in Poland at the concentration of 5 μg/kg. Furthermore, 24 (2.2 ) samples had mycotoxin concentrations between 5 and 10 μg/kg and 13 (1.2 ) samples above 10 μg/kg.

Open access

Alicja Niewiadowska, Tomasz Kiljanek, Stanisław Semeniuk and Jan Żmudzki

Abstract

The occurrence and concentrations of organochlorine pesticides and polychlorinated biphenyls (PCBs) were determined in 141 adipose tissue samples of wild boars, roe deer, and red deer from different regions of the country, collected in 2010/2011. The determinations of HCH isomers (α-, β-, and γ-HCH), HCB, DDTs (p,p’-DDT, o,p’-DDT, p,p’-DDE, and p,p’-DDD), and PCBs (six indicator PCB congeners 28, 52, 101, 138, 153, and 180) were carried out using the capillary gas chromatography. The mean concentrations of DDTs expressed on the fat basis ranged from 0.241 mg/kg (wild boar) to 0.032 mg/kg (red deer), and for PCBs from 0.015 mg/kg (wild boar) to 0.010 mg/kg (roe deer). The mean contribution of p,p’-DDE to DDTs and PCB 153, PCB 138, and PCB 180 to PCBs exceeded 80% and 90% respectively, in all game animal samples studied. Higher contents of chlorinated hydrocarbons were detected in game animals originating from industrial regions.

Open access

Barbara Woźniak, Sebastian Witek, Jan Żmudzki and Alicja Kłopot

Abstract

Natural occurrence of thiouracil in bovine and swine urine in Poland was investigated. Under the national residue control programme, 537 urine samples were tested. In 77 samples (14.3%) thiouracil was detected above decision limit CCα (0.91 μg L-1), including eight samples over the recommended concentration of 10 μg L-1. Of the bovine urine samples, 95 and 99 percentiles have thiouracil concentration below 4.50 and 14.85 μg L-1 ,and of porcine samples below 2.35 and 6.80 μg L-1, respectively.

Open access

Alicja Niewiadowska, Tomasz Kiljanek, Stanisław Semeniuk and Jan Żmudzki

Abstract

The occurrence and concentrations of organochlorine pesticides and polychlorinated biphenyls (PCBs) were determined in 158 muscle samples of bream (Abramis brama) and roach (Rutilus rutilus), and 84 samples of sediments collected from 10 river and lake sampling sites in 2011 and 2012. The concentrations of DDTs (p,p’-DDT, o,p’-DDT, p,p’-DDE, and p,p’-DDD), HCH isomers (a-, ß-, and y-HCH), HCB, and PCBs (six indicator PCB congeners 28, 52, 101, 138, 153 and 180) were determined using the capillary gas chromatography. The mean concentrations of DDTs in bream and roach were in the range of 11.2-654 and 4.5-121 ug/kg wet weight respectively, and PCBs were in the range of 1.3-75.9 and 1.1-112 ug/kg wet weight, respectively. Mean concentrations of DDTs and PCBs in sediments were 0.5-270 ug/kg dry weight and ⋋0.1-2.2 ug/kg dry weight respectively. The study showed clear spatial differences in the levels of organochlorine pesticides and PCBs in fish and sediments from different aquatic ecosystems. The highest levels of contaminants were detected in fish and sediments from the Vistula River in vicinity of Cracow. The possible risk to the fish meat consumers and ecological risk were evaluated.

Open access

Tomasz Śniegocki, Jan Żmudzki, Andrzej Posyniak and Bartosz Sell

Abstract

An in-house reference material of chloramphenicol (CAP) in pigs muscle was prepared from the chloramphenicol treated animals. The incurred muscle material was diluted by mixing with blank muscle sample. The concentration of CAP at the level 0.33 μg kg−1 was reached. For the homogeneity study, 10 random samples were analysed and the results were interpreted by Cochran’s test and the sufficient homogeneity test. Additionally, the samples were tested for their stability according to the following scheme: 1, 7, 14, 28, 56, 84, and 112 d. It was confirmed that an appropriate homogeneity and stability of the produced in-house reference material was obtained.

Open access

Barbara Woźniak, Iwona Matraszek-Żuchowska, Stanisław Semeniuk, Alicja Kłopot and Jan Żmudzki

Abstract

Sensitive and selective methods for the screening (GC-MS) and confirmatory analysis (GC-MS/MS) of 17α- and 17β- trenbolone in bovine urine were developed. In the first stage of the analysis, the enzymatic hydrolysis of trenbolone metabolites with glucuronidase AS-HP in acetate buffer (pH 5.2) solution was carried out. Free compounds were extracted from urine with diethyl ether. For the purification of the extract solid phase, extraction with C18 and NH2 columns was applied. The evaporated extract was subjected to two derivatisation steps; the first with MSTFA/I2 solution and second with MSTFA. The separation of the analytes on HP-5 ms capillary column was conducted. The methods were validated according to the Commission Decision 2002/657/EC. For GC-MS method, CCα and CCβ were 0.21-0.36 μg L−1 for 17α- trenbolone and 0.20-0.34 μg L−1 for 17β- trenbolone, while for GC-MS/MS method the values were lower and amounted to 0.15-0.25 μg L−1 for 17α- trenbolone and 0.20-0.34 μg L−1 for 17β-trenbolone. Method recoveries in spiked samples ranged from 86%-111% with standard deviation lower than 25% for both detection techniques.

Open access

Barbara Woźniak, Sebastian Witek, Iwona Matraszek-Żuchowska and Jan Żmudzki

Abstract

A rapid liquid chromatography tandem mass spectrometry method was developed and validated to detect and confirm five thyreostatic drugs: tapazole, thiouracil, methylthiouracil, propylthiouracil, and phenylthiouracil in animal feeding stuff samples. Thyreostats were extracted from feed with methanol, and then degreasing of the extract with petroleum ether was performed, followed by the derivatisation of the compounds with 3-iodobenzylbromide in basic medium (pH 8.0). The derivatives were extracted with diethyl ether and analysed by gradient elution on a Poroshell 120-EC C18 column with triple quadrupole MS detection with turbo spray source in positive ionisation mode. The method was validated in accordance with the Commission Decision 2002/657/EC. For validation level of 10 ļig kg-1, the recovery ranged from 82% to 97.5% for all examined compounds. The repeatability and reproducibility did not exceed the limit of 20% for all analytes. The linearity was good for all thyreostats in the whole range of tested concentrations, as proved by the correlation coefficients greater than 0.99. The decision limits (CCa) ranged from 1.63 ļig kg-1 to 3.95 ļig kg-1, whereas the detection capabilities (CCß) ranged from 2.74 ļig kg-1 to 6.73 ļig kg-1. The developed analysis is sensitive and robust, and therefore useful for quantification and confirmation of thyreostats in residue control programme.

Open access

Iwona Matraszek-Żuchowska, Barbara Woźniak and Jan Żmudzki

Abstract

This paper describes the quantitative method of determination of chosen substances from resorcylic acid lactones group: zeranol, taleranol, α-zearalenol, β-zearalenol, and zearalanone in bovine muscle tissue. The presented method is based on double diethyl ether liquid-liquid extraction (LLE), solid phase extraction (SPE) clean up, and gas chromatography mass spectrometry (GC-MS) analysis. The residues were derivatised with a mixture of N-methyl-N-trimethylsilyltrifluoroacetamide, ammonium iodide, and DL-dithiothreitol (1,000:2:5, v/w/w). The GC-MS apparatus was operated in positive electron ionisation mode. The method was validated according to the European Union performance criteria pointed in Decision Commission 2002/657/EC. The average recoveries of all analytes at 1 μg kg-1 level were located between 83.7% and 94.5% values with the coefficients of variation values <25%. The decision limits (CCα) and detection capabilities (CCβ) for all analytes ranged from 0.58 to 0.82 μg kg-1 and from 0.64 to 0.94 μg kg-1, respectively. The procedure has been accredited and is used as a screening and confirmatory method in control of hormone residues in animal tissues.