Di-(2-ethylhexyl)phthalate (DEHP) and total phthalate ester plasticizer levels were determined in milk, cream, butter and cheese samples from a variety of sources from three European countries (UK, Norway and Spain). Samples of milk (from Norway) obtained at various stages during collection, transportation and packaging operations showed no apparent trends in phthalate contamination with total phthalate levels (expressed as DEHP equivalents) in the raw milk of between 0.12 and 0.28 mg/kg. On processing the DEHP was concentrated in the cream at levels up to 1.93 mg/kg, whereas low fat milk contained from < 0.01 to 0.07 mg/kg. Retail dairy products (from Spain) were contaminated with < 0.01-0.55 mg/kg DEHP with a maximum total phthalate level of 3.0 mg/kg in cream samples. UK pooled milk samples from doorstep delivery (obtained from different regions of the country) contained low levels of DEHP (< 0.01-0.09 mg/kg) and total phthalate (0.06-0.32 mg/kg). Retail UK samples of cheese, butter and other fatty products varied considerably in their levels of contamination, the highest being cheese samples containing 17 mg/kg of DEHP and 114 mg/kg total phthalate. However, the majority of samples contained 0.6-3.0 mg/kg DEHP and 4-20 mg/kg total phthalate. UK cream samples contained levels of 0.2-2.7 mg/kg DEHP and 1.8-19.0 mg/kg total phthalate. The level found in these products was too high to have resulted solely from milk by concentration in the fat phase and must therefore have arisen in other ways.

Evidence is presented for the first time showing that semicarbazide (SEM) is a minor thermal decomposition product of the blowing agent azodicarbonamide (ADC). A novel direct analytical method based on liquid chromatography electrospray ionization tandem mass spectrometry (LC-ESIMS/MS) has been developed to determine SEM in foamed polyvinyl chloride (PVC) seals of metal lids, as well as in commercially available ADC. The direct LC-MS/MS method for gaskets entails extraction of the gaskets in hot water, addition of ((15)N(2)(13)C)-SEM as internal standard, and injection of an aliquot directly into the LC-MS system, achieving good sensitivity (S/N = 348 for 2 ng injected on-column) and monitoring three characteristic mass transitions (m/z 76-->31; 76 -->44; 76-->59). Semicarbazide can be detected in thermally treated ADC, reaching up to 0.93 mmol mol(-1) at 220 degrees C, as determined by the direct LC-MS/MS method. This new method is also compared to the classical derivatization method using 2-nitrobenzaldehyde (2-NBA) that is routinely employed to determine SEM as an indicator of the usage of the antimicrobial drug nitrofurazone, the use of which is not authorized in the European Union (EU). Both methods revealed proportional results, with approx. 3-fold higher levels recorded by the direct SEM approach, probably due to differences in the extraction procedures used. A limited survey of plastic seals from used press twist and twist-off metal lids on food jars (non-foamed and foamed) revealed levels of SEM ranging from 2 to 8689 microg kg(-1)(average = 1593 microg kg(-1), n= 57 determinations).

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An analytical method for the determination of the nylon-6 monomer caprolactam in foods is described. The foodstuff was extracted with ethanol: water (1:2) containing capryllactam as internal standard and the extract was defatted using hexane. The extract was analysed by liquid chromatography coupled with mass spectrometry. The test method was calibrated down to 0.7 mg kg(-1). The repeatability of the method was good, with a relative standard deviation of 9% at the 15 mg kg(-1) level. The method was demonstrated to be accurate in an independent external check sample exercise. The new method was applied to the analysis of 50 retail foodstuffs packaged in nylon-6. Caprolactam was detected and confirmed in nine of the 50 food samples, in the range 2.8-13 mg kg(-1). The presence of caprolactam was indicated in a further 15 samples, in the range 0.8-11 mg kg(-1), but these samples did not meet all of the five confirmation criteria applied. All migration levels (both confirmed and unconfirmed) were below the European specific migration limit for caprolactam, which is 15 mg kg(-1). The average migration for all 50 samples, setting non-detectables at half the limit of detection, was 2.6 mg kg(-1) with a standard deviation of 3.1 mg kg(-1) (n = 50). All samples found to contain detectable levels of caprolactam migration were for applications involving heating the food in the packaging. They were packs of, for example, sausage meat for which the food would have been heat processed in the nylon casing, or they were nylon pouches for heating foods by boiling, microwaving or roasting.

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