Determination of heterocyclic aromatic amines (HAs) content in samples of household-prepared meat dishes.

Aminoazaarene content was investigated in 10 meat samples (including pork, beef, turey and chicken) thermally processed at home according to common recipes used by residents of Upper Silesia region in Poland. The clean-up procedure included tandem solid-phase extraction (SPE) using Extrelut-type columns filled with diatomaceous earth, propylsulphonic acid and chemically bounded phase-C18. Identification and quantitative analysis of HAs fraction was carried out using a HPLC system with DAD-type detector. Separation was achieved using TSK-gel ODS 80-TM column and a mixture of 5% acetonitrile and 95% triethylamine phosphate buffer (pH 3.3) as a mobile phase. The results of qualitative determinations were confirmed by GC-MS method. To achieve this, HAs fractions were derivatized to pentafluoropropionic acid (PFPA) amide derivatives. The summary content of five aminoazaarenes determined in investigated meat samples, i.e. 2-amino-3-methylimidazo [4,5-f]quinoline (IQ), 2-amino-3,8-dimethylimidazo[4,5-f]quinoxaline (MeIQx), 2-amino-3,4-dimethylimidazo[4,5-f]quinoline (MeIQ), 2-amino-3,4,8-trimethylimidazo[4,5-f]quinoxaline (4,8-DiMeIQx), 2-amino-1-methyl-6-phenyl-imidazo[4,5-b]pyridine (PhIP) falls within the range of 1.9-77.4 ng/g of sample. The calculated values of theoretically daily human exposure to five determined HAs were in the range of 0.2-7.7 microg per day per person.

Clean-up procedures for the analysis of heterocyclic aromatic amines (aminoazaarenes) from heat-treated meat samples.

The purpose of the study was to determine optimum conditions for the isolation and quantitation of five most biologically active aminoazaarenes [2-amino-3-methylimidazo[4,5-f]quinoline (IQ), 2-amino3,4-dimethylimidazo[4,5-f]quinoline (MeIQ), 2-amino-3,8-dimethyl-imidazo[4,5-f]quinoxaline (MeIQx), 2-amino-3,4,8-trimethylimidazo[4,5-f]quinoxaline (4,8-DiMeIQx), 2-amino-1-methyl-6-phenylimidazo[4,5-b]pyridine (PhIP)]. Some multistep procedures based on ultrasonic extraction, Soxhlet extraction, liquid-liquid extraction and solid-phase extraction (SPE) were tested in order to choose the optimum isolation conditions for aminoazaarenes from fried meat samples spiked with known amounts of standards. According to the tested methods the qualitative-quantitative analysis was performed on the unspiked sample of pork roasted in typical household conditions. The qualitative-quantitative analysis of the aminoazaarenes was performed by a HPLC method. A HPLC Hewlett-Packard HP 1090 liquid chromatograph equipped with a UV diode array detector (DAD) was used. Chemically bonded HPLC columns C8 and TSK-gel ODS 80-T(M) were used under gradient elution conditions. A two-component mixture containing triethylamine-phosphate buffer (pH 3.2 and 3.3) and acetonitrile was used as a mobile phase. The results of the studies showed that a solid-phase extraction procedure using diatomaceous earth (Extrelut, 20 ml), propylsulphonic acid (PRS, 500 mg) and octadecylsilane (C18, 500 mg) columns was the quickest and simplest one. Recoveries of the aminoazaarenes, spiked and isolated from meat samples by the chosen SPE procedure, were as follows: IQ 85%, MeIQ 50%, MeIQx 46%, 4,8-DiMeIQx 62%, PhIP 50%.

Solid-phase microextraction of phthalates from water.

Solid-phase microextraction (SPME) with six different non-polar and polar fibres was used to extract seven phthalate esters from water samples for analysis by gas chromatography-mass spectrometry. With regard to extraction efficiency and repeatability of the extractions, the 70-microm Carbowax-divinylbenzene fibre was especially suitable for the selected phthalates with water solubilities between 4200 mg l(-1) (dimethyl phthalate) and 0.0003 mg l(-1) (di-n-octyl phthalate). Linearity was controlled in the range between 0.02 and 10 microg l(-1). In analysed drinking water samples from Leipzig (Germany) and Katowice (Poland) four of the investigated phthalates [diethyl phthalate, di-n-butyl phthalate, butylbenzyl phthalate and di(2-ethylhexyl) phthalate] were found to be present in concentrations between 0.02 and 0.6 microg 1(-1).

Application of liquid separation techniques to the determination of the main urinary nicotine metabolites.

A rapid procedure for the analysis of the main nicotine metabolites (cotinine, trans-3'-hydroxycotinine) in urine has been worked out. The procedure includes isolation of nicotine and its metabolites from urine by means solid-liquid extraction technique using resin Amberlite XAD-2 and then quantitation by the use of thin-layer chromatography with densitometry (in reflection mode). GC-MS was applied to confirm the results obtained by TLC. The procedure was applied to the analysis of cotinine concentrations in urine samples taken from children living in Upper Silesia region (Poland). Among 444 investigated children we did not find cotinine almost in 60% but in 15% of this population, there were children who could have been exposed to cigarette smoke.

Determination of polycyclic aromatic compounds and heavy metals in sludges from biological sewage treatment plants.

The procedure of the analysis of polycyclic aromatic hydrocarbons (PAHs) and their derivatives in the sludges from biological sewage treatment plants has been worked out. The analysis included isolation of organic matter from sludges, separation of the extract into fractions of similar chemical character, qualitative-quantitative analysis of individual PAHs and their nitrogenated and oxygenated derivatives. Liquid-solid chromatography, solid-phase extraction and semipreparative band thin-layer chromatography techniques were used for the separation. Capillary gas chromatography-mass spectrometry analysis of the separated fractions enabled identification of more than 21 PAHs, including hydrocarbons which contained 2-6 aromatic rings as well as their alkyl derivatives, 10 oxygen derivatives, 9 nitroarenes, aminoarenes and over 20 azaarenes and carbazoles. Using the capillary gas chromatography-flame ionization detection technique the content of 17 dominant PAHs was determined. The content of heavy metals was determined in investigated sludges with the use of atomic absorption spectrometry. The concentrations of the respective metals could be ranked in the order Cd < Co < Ni < Pb < Cr < or = Cu < Mn < Zn < Fe. The sludges were analysed for the first time in Poland in view of their possible utilisation in agriculture and in cultivating dumps of coal mine wastes, taking into consideration the contents of toxic organic pollutants and heavy metals.