A capillary electrophoresis method was developed to analyse same food dyes in ice-cream.Sunset yellow (E110), carmoisine (E122), Ponceau 4 R (E124), are permitted in ice-cream by directive 95/45/ce of Commission 26-7-95, but their maximum amount (50 mug/kg) is lower of the limit for the other permitted (150 mug/kg).In this paper we propose a separation on a capillary column (50 cm x 70 mum I.D.) with photodiode array detection: each peak is identified from absorbance spectra and then quantified by external standard.The electrophoresis buffer used was a mixture of 25 mM sodium phosphate and 25 mM sodium borate (1:1) pH 8.The three dyes are separated in a short time, <6 min the standard deviations of the migration times of the peaks range between 0.3% and 0.7%.The limit of detection with a 3:1 signal-to-noise ratio was 5 μg/kg. This capillary zone electrophoresis procedure resulted rapid and sensitive. (C) 2002 Elsevier Science Ltd. All rights reserved.
This paper reports the first group of results on alkylphenol (APE) contamination of seafood in the Adriatic Sea, in the framework of a national project on the quality of this Sea (PRISMA 2). Nonylphenol (NP), octylphenol (OP), and their ethoxylates (NPE and OPE) were detected in edible molluscs, either filter feeders or predators (clams, mussels, cuttlefishes, and squids), caught from 15 harbors along the Italian coast in the Adriatic Sea in 1997. NP was the compound found always at levels much higher than the other APEs in all the examined species. It reached the maximum concentration of 696 ng/g fresh weight in the squids from the central Adriatic Sea. OP generally occurred at levels 30 times lower than NP. OP was found up to a level of 18.6 ng/g in squids from central Adriatic Sea. OPE was the compound always spotted at the lowest concentrations, up to 0.43 ng/g. NPE was always below the detection limit. The pattern of contamination in the three areas examined was different between bivalve and cephalopod species. No exhaustive risk assessment for marine organisms and human health can be conducted on the basis of these results because data are insufficient. Yet, the occurrence of NP suggests a negligible risk for mussels, which represent the only molluscs for which data are adequate. As to the possible human health implications, the consumption of molluscs of the Adriatic Sea implies APE intakes that are some orders of magnitude lower than those responsible for toxic effects in laboratory animals. Despite these apparently low risks for mussels and human health, the reasons for concern still remain because the levels of alkylphenols found in this study indicate a general contamination of the Adriatic Sea even far from the cost. Furthermore, these levels might represent an unacceptable hazard for other marine organisms. Finally, they contribute to the general environmental estrogen pool.
Sixty samples of different types of soft drinks with an aqueous base were analysed (Cola, Cola light, orange, carbonated) for the purpose of evaluating the presence and content of the principal aromatic hydrocarbons responsible for environmental pollution. The analyses were done using the purge and trap technique and gas chromatography combined with mass spectrometry. The deuterated isotopes of the same hydrocarbons were used for quantitative determination by the internal standard technique. Although an examination of the data found does not show values in excess of the limits recommended by the WHO for benzene in drinking water, nevertheless a constant presence of benzene and toluene was found in all the beverages analysed which gives food for thought about a possible cumulative effect, taking the intake of other contaminated foods and environmental pollution into account.
Oils obtained by esterification process of oleins and free fatty acids, by-products of the vegetable oils refining industry, are currently marketed for zootechnical use. Oils labelled as olive, soya and palm oils were sampled on the market and intended for animal nutrition. The fatty acids, sterols and glycerides composition, the acidity value, the peroxide number, and the polar compounds content were investigated to assess the oil's identity, quality and suitability for animal nutrition. The level of mono-glycerides (from 3.0% to 14.2 %) and diglycerides (from 27.4% to 45. 7%) and the high amount of polar compounds (> 50 % for soya and palm oils) showed that the esterification process was incomplete. The high peroxide value (from 7.5% to 17.1 %) and the marked free acidity (> 2.8%) indicated the progress of a heavy lipid oxidation process. The presence of fats of animal origin in palm oil suggested the contamination with exhausted frying oils. Such findings were discussed in the light of risk analysis for animal welfare and food safety.
Evidence of element speciation in biological fluids is scarce and fragmentary in the literature. On the other hand, it is well known that chemical speciation analysis is prone to error due to contamination, modification or breaking up of the metal-organic moiety link during the separation processes, as well as to insufficient detection power for element quantification in the various fractions. Therefore, there is a keen need for sensitive and reliable speciation methods. We explored the analytical capabilities of size exclusion chromatography (SEC) in conjunction with ultrasonic nebulization inductively coupled plasma atomic emission spectrometry (UN-ICP-AES) for the speciation of Ca, Cu, Fe, Mg, Mn and Zn in human milk. We applied the method to assess concentration range and binding pattern of the said elements in the milk of 60 lactating mothers (19-40 years of age) representative of different areas of Italy. The total concentration ranges found were in good agreement with those reported in the literature. These levels were as follows (in ng ml(-1)): Ca, 306 000+/-11 760; Cu, 370+/-30; Fe, 650+/-40; Mg, 23 000+/-510; Mn, 30+/-2; and Zn, 2720+/-70. The influence of factors such as age (over or under 30) and residence area (urban or rural) of the mothers on the total concentration of the elements was also evaluated. Magnesium concentration was higher for mothers >30, while higher Zn levels were found for maternal age <30. Copper was higher in women living in urban areas. Moreover, strong positive Ca-Mg and Fe-Mn associations and significant negative Cu-Zn correlations were found. The chromatographic separation yielded five fractions. The first of these presumably accounted for caseins (alpha(s), beta and k) aggregates; the second peak mainly contained immunoglobulins (Igs); the third could be traced back to human serum albumin (HSA) and lactoferrin (LF); the fourth could be entirely ascribed to alpha-lactalbumin (alpha-La); and the fifth accounted for all substances with relatively low molecular weights, such as non-proteic compounds. As anticipated, the elements investigated showed peculiar associations with the components of the milk. Copper and Fe appeared homogeneously spread over all the organic components. Calcium and Mg preferably bound to low molecular weight compounds. Manganese had a peculiar pattern as it was found in considerable percentage in the first and fifth fractions. As for Zn, the highest percentage was found in the fraction corresponding to alpha-lactalbumin.
A total of 35 samples of commercially obtainable milk were analysed, including whole, semi-skimmed and fully skimmed pasteurised milk and whole and semi-skimmed UHT milk, in order to assess quantitatively the presence and content of certain aromatic hydrocarbons deriving from environmental contamination. The analysis was performed using the purge and trap technique combined with gas chromatography (GC) and using a mass spectrometer (MS) as detector. Deuterated standards of the same aromatic hydrocarbons were used for determination of retention times and for quantitative evaluation. From examination of the data obtained and their subsequent statistical processing it seems clear that, although there are differences between some of the types of milk, the aromatic hydrocarbon content in the samples analysed was at rather modest levels in line with the values reported in the literature.
Virgin olive oil stability to autoxidation is mainly due to phenolic compounds naturally occurring in it, but contrasting data have been published on the effectiveness of the same antioxidant compounds. With thermogravimetric analysis (TGA) it is possible to have an estimation of oil resistance to oxidation, having a measure of weight gain percent due to reaction of sample with oxygen during the oxidation, and of initial and final oxidation temperatures. The following samples were examined: virgin olive oil, olive oil, and olive oil spiked with different amounts of some antioxidants. Tested phenols were p-HPEA, 3,4-DHPEA, 3,4-DHPEA-EA, caffeic acid, oleuropein, and, moreover, BHT and BHA. Data showed that natural antioxidant addition (especially oleuropein, 3,4-DHPEA, and 3,4-DHPEA-EA) could extend the olive oil shelf life and could protect oil from decomposition naturally occurring during thermal treatments (such as cooking process).