Occurrence of bisphenol-F-diglycidyl ether (BFDGE) in fish canned in oil

The levels of bisphenol-F-diglycidyl ether (BFDGE) were quantified as part of a European survey on the migration of residues of epoxy resins into oil from canned fish. The contents of BFDGE in cans, lids and fish collected from all 15 Member States of the European Union and Switzerland were analysed in 382 samples. Cans and lids were separately extracted with acetonitrile. The extraction from fish was carried out with hexane followed by re-extraction with acetonitrile. The analysis was performed by reverse phase HPL C with fluorescence detection. BFDGE could be detected in 12% of the fish, 24% of the cans and 18% of the lids. Only 3% of the fish contained BFDGE in concentrations considerably above 1mg/kg. In addition to the presented data, a comparison was made with the levels of BADGE (bisphenol-A-diglycidyl ether)analysed in the same products in the context of a previous study.     

Method development and analysis of retail foods for annatto food colouring material

Analytical methods for the determination of the permitted food colouring annatto (E160b) have been developed or refined to encompass the wide range of food commodity types permitted to contain it. Specific solvent extraction regimens have been used depending upon the food commodity analysed and HPLC analysis techniques coupled with spectral confirmation have been used for the determination of the major colouring components. Qualitative and quantitative data on the annatto content of 165 composite and two single retail food samples covering a wide range of foods at levels above the limit of quantification (0.1mg kg^-1) is reported. Quantitative results are given for the major colour principals 9'-cis-bixin, 9'-cis-norbixin and trans-bixin. Semi-quantitative results are given for the minor bixin and norbixin isomers monocis- (not 9'-), di-cis- and trans-norbixin, for which authentic reference standards were not available. Repeat analyses (n = 4-9) of 12 different types of food commodity (covering the permitted range) spiked with annatto at levels between 1.7 and 27.7mg kg^-1 gave mean recoveries between 61 and 96%. The corresponding relative SDs (RSD) were between 2.1 and 7.9%.     

Determination of ivermectin and moxidecin residues in bovine milk and examination of the effects of these residues on acid fermentation of milk

Ivermectin (IVM) and moxidectin (MXD) are broad-spectrum antiparasitic drugs not approved for use in dairy animals, although their use in dairy sheep, goats and cattle nevertheless occurs in many parts of the world. The work reported here describes (1) the application of an HPLC method (including milk samples clean-up and chemical extraction) to quantify IVM and MXD residues in bovine milk, and (2) an assessment of the effect of different IVM and MXD concentrations on bovine milk acid fermentation. The latter was carried out using the 'yoghurt test' to determine the minimum IVM and MXD concentrations affecting milk acid fermentation. The sample clean-up, chemical extraction and the validated HPLC method allowed the quantification of IVM and MXD up to 0.1 ng ml^-1 in milk with acceptable validation coefficients. Drug recoveries from fortified milk samples ranged between 72% (CV = 9.1%) and 75% (CV = 13.3%) for MXD and IVM, respectively. Neither IVM nor MXD affected the acid fermentation of bovine milk. In fact, there was no drug-induced changes on milk acidity even at IVM and MXD concentrations as high as 1000 ng ml^-1. These results indicate that the yoghurt biological test is not suitable to evaluate the presence of milk residues for these antiparasitic compounds. Thus, a highly sensitive HPLC technique is the only reliable method for determining the presence of residual concentrations of IVM and MXD in milk and dairy products to assure consumer safety.     

Occurrence of ochratoxin A in black pepper, coriander, ginger and turmeric in India

Ochratoxin A (OA) contamination of black pepper, coriander seeds, powdered ginger and turmeric powder was estimated using indirect competitive ELISA. Samples (1 g) were extracted with 0.5% potassium chloride (KCl) in 70% methanol (5 ml) and diluted subsequently to give two-fold to ten-fold step-wise dilutions in phosphate-buffered saline containing 0.05% Tween 20 and 0.2% bovine serum albumin (PBS-T BSA). For extracts from the spices analysed, ELISA estimates of OA concentrations were compared with those made by HPLC. All estimates were within 1-2 standard deviation of the ELISA values. More than 90% of OA added to spice samples was recovered from samples containing between 5 and 100 microg/kg OA. Extracts of OA-free spice samples contained substances that interfered with ELISA, presumably because of non-specific reactions. This effect was avoided by preparing all the test solutions in extracts of OA-free spice samples. In 126 samples obtained from retail shops, OA was found to exceed 10 microg/kg in 14 (in the range of 15-69 microg/kg) of 26 black pepper samples, 20 (in the range of 10-51 microg/kg) of 50 coriander samples, two (23 microg/kg and 80 microg/kg) of 25 ginger samples and nine (in the range of 11-102 microg/kg) of 25 turmeric samples. This is the first record in India of the occurrence of OA in what are some of the most widely used spices in Indian cooking.     

Caffeine daily intake from dietary sources in Brazil

A survey on the potential intake of caffeine was carried out in Campinas, SP, Brazil, in the summer of 1993. The survey was based on a representative sample of 600 individuals, 9-80 years old, who were asked about their habitual usage of coffee, tea, chocolate products and carbonated beverages. Caffeine levels in the products were determined by high performance liquid chromatography with a UV-visible detector at 254 nm. Individual daily intakes (mg/kg b.w.) of caffeine were calculated from the consumption data generated by the survey and the caffeine content of the analysed products. Of all those interviewed, 81% consumed soft drinks regularly, 75% coffee, 65% chocolate products and 37% tea. Of the analysed products, coffee showed the highest amount of caffeine. The average and median potential daily intake of caffeine by the studied population were, respectively, 2.74 and 1.85mg/kg b.w. Coffee, tea, chocolate products and carbonated beverages accounted for median individual daily intakes of 1.90, 0.32, 0.19, and 0.19mg/kg b.w., respectively. These data show that coffee is the most important vehicle for caffeine intake within the studied population.     

Natural occurrence of aflatoxins in Korean meju

Aflatoxin B₁ (AFB₁) was found in 35 of 60 (58.3%) meju samples with an average concentration of 7.3ng/g by ELISA. Contamination of AFB₁ was confirmed in 25 of 60 samples (41.6%) using HPLC, with an average concentration of 6.9ng/g. Mean recoveries from meju ranged from 107% to 170% for AFB₁ using ELISA at a spiking range of 1 to 50ng/g. Over the same range, recoveries using HPLC were from 70% to 83%. The levels of AFB₁ determined by ELISA and by HPLC demonstrated a close relationship between the two methods (r2 = 0.9324) employed in this study. In order to evaluate the potential health risks of AFB₁ on Koreans consuming meju, we calculated the estimated probable daily intake (PDI) based on the average contamination levels and compared it with the estimated tolerable daily intake (TDI). The PDIs of AFB₁ from kanjang and dwenjang were determined to be 0.04 and 0.21ng/kg bw/day, respectively, and were higher than TDIs.     

Levels Of Linear Alkylbenzenesulfonates (LAS) In Sediments Of The Berre Lagoon (FRANCE)

A method is described to extract, concentrate and determine trace levels of linear alkylbenzenesulfonates (LAS) (a major anionic surfactant) from sediment samples. It consists of an ultrasonic extraction, followed by clean up and enrichment with C18 mini-columns cartridges and determination by HPLC. Both efficiency and accuracy of the method are high, i.e. mean recovery of 85% and repeatability of 2.8% relative standard deviation for five-replicate LAS analyses. The spatial distribution of LAS and their composition of homologues in sediments of the Berre lagoon, the widest lagoon of the Mediterranean littoral, have been studied. The levels of total LAS in sediments range from 0.21 to 5.00?mg=g (dry weight). Results show that LAS principally associated with solids in suspension, and originating from industrial and urban wastewaters, are principally discharged into the Arc and Cadière Rivers then decant in the mouths of these rivers. The maximum concentrations have been monitored in three zones of the site: the Bolmon lagoon, the Vaine lagoon and the northeast part of the Berre lagoon. The distribution of the LAS homologues in the sediments is not the same as that of the commercial LAS. A great percentage of C13-LAS has been observed (>50%).