Towards the certification of the purity of calibrant reference materials for thyroid hormones: a chicken and egg dilemma.

The certification of the purity of CRMs intended for calibration, where no other certified material already exists for comparison, raises principle questions on how to determine the purity of a "first" calibrant in the calibration hierarchy. We developed and certified two calibration CRMs for their purity in thyroid hormones taking into consideration inorganic residues, residual solvents and organic impurities detectable by HPLC-UV and HPLC-MS. IRMM-468 was certified for a thyroxine (T(4)) mass fraction of 98.6+/-0.7% and IRMM-469 was certified for a 3,3',5-triiodothyronine (T(3)) mass fraction of 97.1+/-0.7%. The approach we used aims to determine the purity of these two CRMs to the best of our knowledge and taking all scientific aspects properly into account for the estimation of an uncertainty related to the stated purity.

Occurrence and determination of pesticides in natural and treated waters.

Pesticides as environmental pollutants are described in detail along with their sources and paths of entry into various elements of the environment. Comprehensive literature data on the concentration of these pollutants in natural and treated waters and wastewaters are discussed. A wide selection of isolation and preconcentration techniques for these pollutants in water is presented and discussed. An emphasis is put on solid-phase extraction. In the case of the authors' work, a more detailed description is given.

Sample preparation for GC analysis of selected pesticides in surface water.

A new isolation procedure for the determination of nitrogen/phosphorous containing pesticides and organochlorine pesticides in water was tested, and statistical evaluation of the recoveries was performed. The procedure, designed specifically for the analysis of semi-volatile compounds in water containing Suspended Particulate Matter (SPM), utilizes a specially designed filtration vessel coupled directly to an SPE cartridge. The studies were based on surface water samples (from the Vistula River) spiked with pesticides. SPM separation and analyte isolation/concentration were carried out in a special filtration vessel. Pesticides were sorbed both on the SPE cartridge and on the suspended matter. The cartridge and the filter with the suspended matter were extracted separately with a solvent, which enabled the determination of analyte distribution between the two. For organochlorine pesticides, between 3 and 60% of the initial amount was found on the filter, while the recoveries in the filtrate ranged from 30 to 98%. Total recoveries of organochlorine pesticides from surface water samples spiked with pesticides using the method described were high, ranging from 90 to 101%. The amounts of nitrogen/phosphorus containing pesticides recovered from the filter were lower than 2%, while those from the filtrate ranged from 69 to 92%. Total recoveries of nitrogen/phosphorus containing pesticides from surface water samples were high, ranging from 71 to 92%.

[Carbamazepine in modern toxicological casuistry at Department of Forensic Medicine of Medical University of Gdansk in the years 1996-2001]. / Karbamazepina we wspólczesnej kazuistyce toksykologicznej Zakladu Medycyny Sadowej Akademii Medycznej w Gdansku w latach 1996-2001.

In this paper the authors presented 20 cases of death of individuals diagnosed at Department of Forensic Medicine of Medical University of Gdansk in the years 1996-2001. In all cases carbamazepine was found in post-mortem material collected from the deceased during autopsy. 14 deaths resulted from intoxication after overdose of drugs for the purpose of committing suicide. In the other cases carbamazepine did not have on influence on the cause of death. The subject of the chemo-toxicological analysis were blood and urine samples and also specimens of the stomach with its contents, liver, kidney, brain and lung specimens collected during autopsy. TLC, GC-FID, GC-MS, TLC-UV were used as diagnostic tools. Determined carbamazepine concentrations fluctuated between 1.5 to 78.6 micrograms/ml in the blood.

[Group intoxication with 2-ethoxyethanol as an ethanol substitute]. / Grupowe zatrucie 2-etoksyetanolem jako zamiennikiem etanolu.

In this paper the authors presented the group 2-ethoxyethanol intoxication of 8 young men aged between 20 to 22. 50-100 ml of pure compound (diluted with water) was administrated as a drink. In this paper symptoms of acute intoxication to this compound were presented. GC-FID and GC-MS were used as diagnostic tools. The obtained results were compared with the data from available literature.