Three groups of eight volunteers were administered stable isotope-labelled phthalate diesters in a single dose and the amount of the corresponding phthalate monoesters excreted in the urine was measured. Amongst the phthalates administered were the symmetrical dibutyl-, di-2-ethyl- and diisooctyl- phthalates along with the unsymmetrical benzylbutylphthalate. The control group received no dose, the low dose group received 168-255 microg of each phthalate and the high dose group received 336 to 510 microg of each phthalate. The excreted phthalate monoesters were measured by LC-MS following hydrolysis of conjugates. The bulk of phthalate monoester was excreted in the first 24 hour period following the dose. For dibutylphthalate, 64% and 73% on a mole basis of the low, and high dose respectively was excreted as monobutylphthalate. For dioctylphthalate (sum of the 2-ethylhexyl and the isooctyl species) the yield was 14 and 12% of the low and high dose excreted as monooctylphthalate. For benzylbutylphthalate, 67% and 78% was eliminated as monobenzylphthalate and only 6% (measured for the high dose only) was eliminated as monobutylphthalate. These conversion factors can be used in future studies to assess exposure to phthalate esters via measuring urinary levels of the monoester metabolites.
Benzophenone may be present in cartonboard food-packaging materials as a residue from UV-cured inks and lacquers used to print on the packaging. It may also be present if the cartonboard is made from recycled fibres recovered from printed materials. A method has been devised to test for benzophenone in cartonboard packaging materials and to test for migration levels in foodstuffs. Packaging is extracted with solvent containing d10-benzophenone as the internal standard. Foods are extracted with solvent containing d10-benzophenone and the extract defatted using hexane. The extracts are analysed by GC-MS. For analysis of food, the limit of detection was 0.01 mg x kg(-1) and the limit of quantification was 0.05 mg x kg(-1). The calibration was linear from 0.05 to 20 mg x kg(-1). The method for food analysis was validated in-house and it also returned satisfactory results in a blind check-sample exercise organized by an independent laboratory. The methods were applied to the analysis of 350 retail samples that used printed cartonboard packaging. A total of 207 (59%) packaging samples had no significant benzophenone (<0.05 mg x dm(-2)). Seven (2%) were in the range 0.05- 0.2 mg x dm(-2), 60 (17%) were from 0.2 to 0.8 mg x dm(-2) and 76 (22%) were from 0.8 to 3.3 mg x dm(-2). A total of 71 samples were then selected at random from the 143 packaging samples that contained benzophenone, and the food itself was analysed. Benzophenone was detected in 51 (72%) of the foods. Two food samples (3%) were in the range 0.01-0.05 mg kg(-1). A total of 29 (41%) were from 0.05 to 0.5 mg kg(-1), 17 (24%) were from 0.5 to 5 mg x kg(-1) and three (4%) food samples exceeded 5 mg x kg(-1). The highest level of benzophenone in food was 7.3 mg x kg(-1) for a high-fat chocolate confectionery product packaged in direct contact with cartonboard, with room temperature storage conditions and with a high contact area:food mass ratio. When the mass fraction of benzophenone migration was calculated for the different contact and storage regimes involved, the attenuation effects of indirect contact and of low temperature storage were cumulative. Thus, there was a sixfold reduction in migration for indirect contact compared with direct contact, a sixfold reduction for chilled/frozen storage compared with ambient storage, and 40-fold reduction for the two contact conditions combined.
The benefits that high-pressure thermal sterilization offers as an emerging technology could be used to produce a better overall food quality. Due to shorter dwell times and lower thermal load applied to the product in comparison to the thermal retorting, lower numbers and quantities of unwanted food processing contaminants (FPCs), for example, furan, acrylamide, HMF, and MCPD-esters could be formed. Two spore strains were used to test the technique; Geobacillus stearothermophilus and Bacillus amyloliquefaciens, over the temperature range 90 to 121 °C at 600 MPa. The treatments were carried out in baby food puree and ACES-buffer. The treatments at 90 and 105 °C showed that G. stearothermophilus is more pressure-sensitive than B. amyloliquefaciens. The formation of FPCs was monitored during the sterilization process and compared to the amounts found in retorted samples of the same food. The amounts of furan could be reduced between 81% to 96% in comparison to retorting for the tested temperature pressure combination even at sterilization conditions of F₀-value in 7 min.
The formation of free monochloropropane-1,2-diol (3-MCPD and 2-MCPD) and its esters (bound-MCPD) was investigated in biscuits baked with various time and temperature combinations. The effect of salt as a source of chloride on the formation of these processing contaminants was also determined. Kinetic examination of the data indicated that an increasing baking temperature led to an increase in the reaction rate constants for 3-MCPD, 2-MCPD, and bound-MCPD. The activation energies of formation of 3-MCPD and 2-MCPD were found to be 29 kJ mol(-1). Eliminating salt from the recipe decreased 3-MCPD and 2-MCPD formation rate constants in biscuits by 57.5 and 85.4%, respectively. In addition, there was no formation of bound-MCPD in biscuits during baking without salt. Therefore, lowering the thermal load or limiting the chloride concentration should be considered a means of reducing or eliminating the formation of these contaminants in biscuits. Different refined oils were also used in the recipe to test their effect on the occurrence of free MCPD and its esters in biscuits. Besides the baking process, the results also confirmed the role of refined oil in the final concentration of these contaminants in biscuits.
UK rye-based cereal products were analysed for six major ergot alkaloids using an in-house-validated liquid chromatography-tandem mass spectrometry (LC-MS/MS) method that distinguished -ine and -inine epimers (isomers). Ergot alkaloids were detected in 25 of 28 samples subject to quantification limits of 1-3 µg kg(-1), including all of eleven rye crispbreads that had up to 340 µg kg(-1). Continental-style rye breads contained up to 121 µg kg(-1). Loaf breads, bread-mix flours, and crackers contained only low levels of alkaloids. Ergotamine, ergocristine, and ergosine were the predominant ergot alkaloids in terms of level and frequency of occurrence. There were no apparent differences in the ergot levels between the organic and non-organic products, although the numbers tested were low. Most rye breads had a ratio of -ines to -inines of about 1.5, and rye crispbreads had lower and more variable -ine to -inine ratios.
COMMON ragwort (Senecio jacobaea) is a widespread invasive weed that is one of the most frequent causes of plant poisoning of horses and other grazing animals, and is responsible for over 90 per cent of the complaints that the UK Department of Environment, Food and Rural Affairs (Defra) receives about injurious weeds. Ragwort has Veterinary Record (2009) 165, 568-569 C. Crews, MSc, MRSC, CChem,
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