No abstract

The persistence of methyl bromide (MB) in white rice, brown rice, sultanas, raisins, pumpkin seeds, brazil nuts, groundnuts and walnuts was monitored following laboratory fumigations at different concentration time products and temperatures. A sensitive automated headspace gas chromatographic method with a limit of quantitation of 0.005 mg kg−1 was used to determine MB residues. Nuts and seeds sorbed the highest amounts of MB followed by rice and dried fruit. Measurable MB residues were shown to persist in nuts and seeds for 10 weeks and in dried fruit for four weeks following a fumigation with recommended concentration time products. The data presented suggest MB residues may persist in unprocessed nuts, seeds or dried fruit at the point of consumption using recommended fumigation practices, or particularly following overdosing or multiple fumigations. Crown copyright © 2000 Reproduced with the permission of Her Majesty's Stationery Office

A gas chromatography-mass spectrometry (GC-MS) method was used for the quantitative confirmation of phosphine residues in stored products and processed foods. An established extraction technique was utilized for the preparation of headspace samples, which were analyzed by GC-MS and gas chromatography-nitrogen-phosphorus detection (GC-NPD). Wheat, oats, maize, white rice, brown rice, cornflakes, tortilla cornchips, groundnuts, and raisins were validated, showing excellent agreement between detectors when spiked at levels equivalent to 0.001 and 0.01 mg/kg phosphine and for samples containing incurred residues. The GC-MS method was reproducible and accurate when compared to the GC-NPD method and allowed five samples to be quantified in a working day. Subambient GC-MS oven temperatures were most suitable for phosphine residues ranging from 0.001 to 0.005 mg/kg, and a GC oven temperature of 100 degrees C was appropriate for residues >0.005 mg/kg. The method was sufficiently robust to be evaluated for other similar commodities as the need arises.

A rapid screening method for detecting low levels of tetrachloroethylene (perchloroethylene, PCE) in olive oils has been developed using headspace capillary gas chromatography. Modification of this method allows quantitative results to be obtained down to 0.001 mg kg-1. Results obtained show that olive oil samples received in this laboratory over a two year period have not contained PCE residues in excess of the European Commission guidelines.

An automated gas chromatographic headspace method capable of detecting methyl bromide (MB) down to 0.01 mg kg−1 has been developed and evaluated. The method is suitable for analysing cereals, nuts, seeds and dried fruit. Commodities are extracted with solvent and MB present is derivatised to methyl iodide (MI) which is determined by automated headspace gas chromatography. Results from the method described are compared with those using an established solvent extraction method and show good quantitative agreement. The analytical conditions recommended are likely to be suitable for examination of other commodities for MB residues.