No abstract

The 3M Company has developed a sample-ready system (Petrifilm ™ SM) for enumerating bacteria in milk and other food products. The testing unit consists of Standard Methods culture medium coated onto a base film and overlaid with a second film coated with a cold-water-soluble gelling agent and tetrazolium indicator dye. As such, the system is ready to accept samples of product. A pipette or 0.001-ml plate loop continuous pipetting syringe can be used for applying samples. In this study, both methods of sample addition were used and results compared with those of the Standard Plate Count (SPC) and standard Plate Loop (PL) methods for determining bacteria numbers in raw milk. In total, 108 samples were analyzed in duplicate by each of the four methods. The correlation coefficients (r) between the 3M-SPC and SPC, 3M-PL and PL, 3M-PL and SPC and PL and SPC were 0.946, 0.935, 0.941, and 0.974, respectively. Repeatability, as measured by mean log10 variance for duplicate determinations, was essentially the same for the four methods, and in all instances less than 0.005. The mean log10 differences between the SPC and 3M-SPC, and SPC and 3M-PL were, respectively, −0.177 and −0.168. The preceding statistical criteria suggest the Petrifilm™ SM method to be a suitable alternative to the SPC or the PL procedure.

New methodologies based on supercritical fluid extraction (SFE) have been developed for the determination of fat-soluble vitamins in processed foods. The results obtained so far indicate that SFE is well suited to extraction of fat-soluble vitamins from food products, although validation work is required to establish accuracy and precision. The vitamins investigated were A, E and beta-carotene, and the processed foods were UHT milk, milk powder, minced meat, liver paste, infant formula, canned baby food and margarine. Extraction equipment employed analyte collection on either a solid-phase trap or in a solvent. After extraction, the samples were saponified and the vitamins determined using reversed-phase liquid chromatography with ultraviolet or fluorescence detection. Sample throughput was at least 12 samples day(-1), i.e. at least twice the number achievable with a conventional extraction methodology. The detection limits for the vitamins in different processed foods were well below 0.1 microg g(-1). Recoveries (in comparison with vitamin levels obtained using conventional solvent extraction) were close to 100% for experienced personal with access to modern automatic equipment. To reach this level, it was necessary to protect the vitamins with an antioxidant during the different steps of the analysis procedure, to add methanol or ethanol to the extraction cell to facilitate the analyte extraction from the food matrix, and when using a solid-phase trap, to employ a fractionated extraction-elution procedure to prevent breakthrough losses. The developed methods were tested in a validation exercise between five laboratories, which had taken part in the method development, and in an intercomparison between 10 laboratories including laboratories with less experience of vitamin determination. The within-laboratory RSD was generally < or = 11%. The average of the between-laboratory relative standard deviation (RSD) was about 23% in the validation, and increased to about 40% in the intercomparison. Ruggedness tests performed at different steps of the project showed that different types and models of equipment did not give large differences in recoveries. Thus, the increasing RSD can largely be ascribed to differences in experience in vitamin analysis of the participants.