The residual and migration levels of 28 primary aromatic amines (PAAs) in polyurethane and nylon toys were determined using LC-MS/MS, and the migration and residual amounts of PAAs and 15 colorants in textile toys were determined using LC-MS/MS and LC-TOF-MS according to the European Standard EN71. Among 34 polyurethane toy samples, 2,6-diaminotoluene and 2,4-diaminotoluene were detected in the same 12 samples at residual levels ranging from 2.1 to 19.7 and from 7.6 to 39.6 μg/g, respectively. Furthermore, 4,4′-diaminodiphenylmethane (4,4′-MDA) and aniline were detected in 9 samples (from 0.2 to 8.7 μg/g), and one sample (0.4 μg/g), respectively. PAAs were not detected in the 8 samples of nylon toys. As for the migration test into water, only 4,4′-MDA migrated from 3 polyurethane toys at levels ranging from 0.4 to 2.5 μg/g. PAAs did not migrate from the 43 textile toys, but colorants such as Solvent Yellow 1 and Basic Red 9 were detected at the residual level of 0.02 μg/g. The residual levels of PAAs and colorants detected in this study were significantly lower than the limit values established by the European Union regulation.
From fiscal year 2012 to 2014, we surveyed the concentration of radioactive cesium in 39 wild animal meats obtained from 20 wild boars and 19 deer caught in Chiba prefecture, using a germanium semiconductor detector. Four wild boar meats in the fiscal years 2012 and 2013 exceeded the radioactive cesium limit in general foods (100 Bq/kg), whereas none of the deer meats exceeded the limit. The left side of the wild boar that showed a radioactive cesium concentration above 100 Bq/kg was divided into 14 parts. We compared the radioactive cesium concentration in the ham used for the screening test with those in other parts. The concentration was highest in ham, among the edible parts.
Automated rRNA intergenic spacer analysis (ARISA), a method of microbiome analysis, was evaluated for species identification of mushrooms based on the specific fragment sizes. We used 51 wild mushroom-fruiting bodies collected in the centre of Hokkaido and two cultivated mushrooms. Samples were hot-air-dried and DNA were extracted by a beads beating procedure. Sequencing analysis of portions of the rRNA gene (rDNA) provided 33 identifications of mushrooms by genus or species. The results of ARISA identification based on the combination of the fragment sizes corresponding to two inter spacer regions (ITS2 and ITS1) of rDNA within±0.1% accuracy showed that 27 out of the 33 species had specific fragment sizes differentiated from other species. The remaining 6 species formed 3 pairs that showed overlapping fragment sizes. In addition, within-species polymorphisms were observed as 1 bp differences among 32 samples of 13 species. ARISA was applied to investigate a case of suspected food poisoning in which the mushroom was thought to be a toxic Kakishimeji. The morphological identification of the mushroom was ambiguous since the remaining sample lacked a part of the fruiting body. Further, yeast colonies had grown on the surface of the fruiting body during storage. The ARISA fragment size of the mushroom showed 7 bp difference from that of the candidate toxic mushroom. Although ARISA could be a useful tools for estimation of mushroom species, especially in case where the fruiting bodies have deteriorated or been processed, further studies are necessary for reliable identification. For example, it may be necessary to adopt more informative genes which could provide clearer species-specific polymorphisms than the ITS regions.
In this experiment, 351 pesticides and 441 different organic compounds were analyzed by GC/MS, and a database of retention time, retention index, monoisotopic mass, two selected ions, molecular formula, and CAS numbers was created. The database includes compounds such as alcohols, aldehydes, carboxylic acids, esters, ethers and hydrocarbons with unpleasant odors. This database is expected to be useful for health crisis management in the future.
The contents and composition of tetrodotoxin (TTX) and paralytic shellfish toxins (PSTs) in skin, muscle, and internal organs of two samples of marine puffer fish Canthigaster rivulata from Wakayama prefecture, Japan, were analyzed. Liquid chromatography-mass spectrometry (LC-MS) and high-performance liquid chromatography with post-column derivatization and fluorescence detection (LC-FLD) were used for the analysis of TTX and PSTs, respectively. For both samples, TTX and two analogues of PSTs, saxitoxin (STX) and decarbamoyl STX (dcSTX), were detected at levels over the limit of quantization (LOQ) only in the skin. These toxins in the muscle and internal organs were at trace levels, or not detected (ND). TTX contents were 11,000 and 13,000 ng/g (or 35 and 41 nmol/g), while PSTs contents were 168 and 460 ng/g (or 0.63 and 1.72 nmol/g) in the two skin specimens. The compositions of total toxin content were 98.2 and 96.0 mol% TTX and 1.8 and 4.0 mol% PSTs, respectively. Thus, the main contributor to toxin content in C. rivulata skin was TTX and the levels of PSTs toxicity in C. rivulata were very low. When the PSTs contents were converted into mouse unit score from the LC-FLD results, the resulting values of 1.0 and 2.8 MU/g of PSTs in C. rivulata skin were similar to those in Takifugu poecilonotus and Takifugu vermicularis in Japan, as determined in previous studies.
We have developed and validated an inductively coupled plasma-mass spectrometry (ICP-MS) method for the simultaneous analysis of minerals and toxic elements in foods. Food samples were digested by microwave irradiation to prepare solutions for measurement by ICP-MS. Optimal gas mode and internal standard for each element were selected as appropriate. The method was validated for eighteen elements in total using three certified standard reference materials, namely, Typical Japanese Diet, Rice Flour-Unpolished and Infant/Adult Nutritional Formula, according to the guidelines of the Ministry of Health, Labour and Welfare of Japan. The trueness and precision of the method were all within the acceptable limits, except for Na in Rice Flour-Unpolished.