Determinação simultânea de resíduos de etinilestradiol e gestodeno em superfícies de equipamentos de produção / Simultaneous determination of ethynylestradiol and gestodene residues on manufacturing equipment surfaces

Um método de validação de limpeza foi desenvolvido e validado, baseado na amostragem por swab e na determinação cromatográfica simultânea de resíduos de gestodeno e etinilestradiol. O método apresenta limite de quantificação de 0,036µg/mL de etinilestradiol e 0,009µg/mL de gestodeno. Este foi considerado seletivo, preciso, exato e robusto de acordo com as normas da ANVISA. O fator de recuperação para etinilestradiol foi 90,45% e para gestodeno foi 83,52% em superfície de inox e 87,31% para etinilestradiol e 81,21% para gestodeno em superfície emborrachada. O método foi aplicado com sucesso no teste de amostragem por swab de todos os pontos de superfície dos equipamentos. O método de limpeza foi considerado validado...

A cleaning technique validation method was developed and validated, based on swab sampling and simultaneous chromatographic determination of gestodene and ethynyl estradiol residues. The method exhibited limits of quantitation (LOQs) of 0.036µg/mL for ethynyl estradiol and 0.009µg/mL for gestodene. It was considered selective, precise, accurate and robust, according to the standards set by ANVISA, the Brazilian regulatory agency. Mean swab recovery factors were 90.45% for ethynyl estradiol and 83.52 % for gestodene on an inox surface and 87.31% for ethynyl estradiol and 81.21 % for gestodene on a rubberized surface. The method was successfully applied to the assay of actual swab samples collected from all points on equipment surfaces. The cleaning method was validated...

Pesticide monitoring programme of the Ministry of Health of Brazil.

The structure of the recently introduced Brazilian government programme for monitoring pesticide residues in six major agricultural products is described. Residues found from the analysis of samples of tomatoes and strawberries are discussed in detail. The much greater frequency of detection of pesticide residues, many of which are not approved for use in Brazil, in produce being sold on the domestic market, as opposed to that produced for export, is of major concern. It is perceived that this new monitoring programme will become permanent and be used to underpin enforcement actions that will need to be taken to reduce the numbers of incidents of illegal residues occurring, particularly in fresh fruits and vegetables.

Direct determination of gallium on polyurethane foam by X-ray fluorescence.

Gallium chloride is easily extracted from 6M HCl by comminuted polyether-type polyurethane foam. After the extraction step, the gallium absorbed by the PU foam can be quantitatively determined by X-ray fluorescence. A procedure for the direct determination of gallium absorbed by PU foam by XRFS is thus described. Gallium is determined at levels as low as 60 ng/ml (C(L)), with a calibration sensitivity of 424 cps ml/mug, within a linear range 0.1-2.30 mug/ml. The procedure investigated was successfully applied to determination of gallium in aluminum alloys, bauxite and industrial residue samples.

Determination of uranium isotopes by chemical stripping and alpha-spectrometry.

We describe a new method of preparing thin sources for the determination of uranium isotopes by alpha-spectrometry. The sources are produced by extracting the uranium isotopes from 1 M HNO3-4M Al(NO3)3 aqueous solution with polymeric membranes containing trioctylphosphine oxide (TOPO). We demonstrated that the sources are comparable to those obtained by electrochemical procedures using platinum or stainless-steel cathodes.