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Open access

Tomasz Kiljanek, Alicja Niewiadowska and Stanisław Semeniuk

Abstract

A method for simultaneous determination of 13 organophosphorus pesticide residues in milk samples has been developed and validated. The method is based on the extraction of the sample with acetone and petroleum ether, cleanup by gel permeation chromatography, and solid phase extraction, and determination by gas chromatography with flame photometric detection. The recovery, investigated by analysing blank milk samples spiked with azinphos, chlorfenvinphos, chlorpyrifos, chlorpyrifos-methyl, diazinon, fenitrothion, methacrifos, methidathion, parathion-methyl, pyrazophos, and triazophos at concentrations of 10, 20, and 30 μg/kg, and with parathion and pirimiphos-methyl at concentrations of 25, 50, and 75 μg/kg, ranged from 73.1% to 106.2%. Performance characteristics, such as repeatability and within-laboratory reproducibility expressed as coefficient of variation were less than 20%. Measurement uncertainty was lower than 22% for all validated organophosphorus pesticides. The limits of quantification were 10 μg/kg for all compounds and allowed determination of residues at, or even below, the maximum residue limits set by the European Union. The satisfactory z-score results of international proficiency tests confirm good accuracy, reproducibility, and reliability of the developed method.

Open access

Tomasz Kiljanek, Alicja Niewiadowska and Andrzej Posyniak

Abstract

During the 2000s, the problem of pesticide poisoning of honeybees seemed to be almost solved. The number of cases has decreased in comparison to the 1970s. The problem of acute honeybee poisoning, however, has not disappeared, but instead has transformed into a problem of poisoning from ‘traditional’ pesticides like organophosphorus pesticides or pyrethroids, to poisoning from additional sources of ‘modern’ systemic neonicotinoids and fipronil. In this article, the biological activity of pesticides was reviewed. The poisoning symptoms, incident definitions, and monitoring systems, as well as the interpretation of the analytical results, were also reviewed. The range of pesticides, and the detected concentrations of pesticides in poisoned honeybee samples, were reviewed. And, for the first time, cases of poisoning related to neonicotinoids were reviewed. The latter especially is of practical importance and could be helpful to analysts and investigators of honeybee poisoning incidents. It is assumed that secondary poisoning induced by plant collected materials contaminated with systemic pesticides occurs. Food stored in a hive and contaminated with systemic pesticides consumed continuously by the same generation of winter bees, may result in sub-lethal intoxication. This leads to abnormal behaviour identified during acute intoxication. The final result is that the bees discontinue their social role in the honeybee colony super organism, and colony collapse disorder (CCD) takes place. The process described above refers primarily to robust and strong colonies that were able to collect plenty of food due to effective plant protection.

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

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

Krystyna Pohorecka, Tomasz Kiljanek, Maja Antczak, Piotr Skubida, Piotr Semkiw and Andrzej Posyniak

Abstract

Introduction: Amitraz is a formamide exhibiting both acaricidal and insecticidal activity and is frequently used by beekeepers to protect honeybee colonies against Varroa destructor mites. The aim of this apiary trial was to evaluate the impact of honeybee colony fumigation with amitraz on the level of contamination of honey stored in combs.

Material and Methods: Experimental colonies were fumigated four times every four days with one tablet of Apiwarol per treatment. Honey was sampled from combs of brood chambers and combs of supers one day after each amitraz application and from harvested honey. Amitraz marker residues (as a total of amitraz and metabolites containing parts of molecules with properties specific to the 2,4-DMA group, expressed as amitraz) were evaluated in honey.

Results: All analysed samples were contaminated with amitraz metabolites. 2,4-DMA and DMPF were the most frequently determined compounds. The average concentration of amitraz marker residue in honey from groups where a smouldering tablet was located directly in beehives was significantly higher than that of residue in honey from groups with indirect smoke generation. No significant effect on the honey contamination deriving from the place where it was exposed to smoke (combs of brood chambers and supers) was noted. Amitraz marker residues exceeded the MRL in 10% of honey samples from combs.

Conclusion: Fumigation of beehives with amitraz results in contamination of honey stored in combs.