An inter-laboratory study involving 23 laboratories was conducted to validate the government-approved analytical method for the determination of bisphenol A migrating from polycarbonate food processing materials. The obtained values were analyzed statistically using internationally accepted guidelines. Horwitz ratios were calculated based on the reproducibility relative standard deviation (RSD_R), which was estimated from the inter-laboratory study, and predicted RSD_R, which was calculated using the Horwitz/ Thompson equation. The analytical methods used for the migration solutions of water, 20% ethanol, and 4% acetic acid met the performance criteria of less than 2 of HorRat value set by the Codex Alimentarius for analytical method approval, but the analytical method for the migration solution of heptane did not. The results showed that the analytical method for the migration solution of heptane needs to be improved.

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We developed a simultaneous LC-MS/MS determination method for veterinary drugs in muscle of animal and fishery products and milk using sequential extraction with an organic solvent and buffer solution. To enhance the extraction efficiency of both the chelating compound and the hydrophobic compound, freeze ground samples were extracted first with an acetonitrile-methanol (1:1) solution and then with the buffer solution (pH 4.0). The extracts were combined after purification using a hexane/SPE cartridge column. Analytical validations for 65 compounds were done with salmon, shrimp, cattle muscle and milk. The accuracy and precision were within the required ranges of Japanese validation guidelines for a wide range of veterinary drugs (58 compounds in salmon, 51 compounds in shrimp, 63 compounds in cattle muscle, and 63 compounds in milk).

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Food proteins and their constituent peptides can impart huge health benefits in addition to their nutritional attributes. Buckwheat flour hydrolysate was studied for its ability to inhibit the activity of dipeptidyl peptidase-IV (DPP-IV); as shown in in-vitro assays, inhibition of this enzyme can be used for the treatment of type II diabetes. Buckwheat flour hydrolysate prepared with Alcalase^® and Flavourzyme^® showed greater DPP-IV inhibitory activity than the control sample. Buckwheat flour hydrolysate was purified using successive column chromatography. The obtained Val–Pro–Leu (VPL) and Val–Pro–Ile (VPI) were identified using LC-Q-TOF. VPL has been used as a commercial inhibitor of DPP-IV, named Diprotin B. VPI, with an IC₅₀ of 18.0 ± 2.4 μM, exhibited approximately 10-fold greater inhibition of DPP-IV than VPL (200.5 ± 7.5 μM). The DPP-IV inhibitory activity of VPI was maintained at approximately 95% after the in vitro gastrointestinal digestion process. These results suggest that the buckwheat flour hydrolysate has potential value in functional food formulations.

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As basic research for contributing to the determination of conformity with the Positive List (PL) system, chemical substances contained in plastic utensils, containers and packaging were comprehensively analyzed using GC-MS. Total of 131 standard substances of additives listed in the Japanese PL were analyzed to obtain information on mass spectra and retention index (RI). The ratio of calculated RI to library-registered RI showed a good agreement, being 1.0 for most substances. By comparing RI in addition to mass spectra, unknown peaks detected in plastic products could be identified more reliably. Chemical substances contained in plastic products made of polypropylene, polyethylene, polystyrene, and polyethylene terephthalate, which are widely used generalpurpose plastics, were analyzed. As a result, 61 of the 104 substances detected in plastic products were identified and/or estimated, and about half of them were the ones listed in PL. However, the other half were non-listed substances, and most of them were considered to be non-intentionally added substances (NIAS), which are degradation products, impurities, by-products, etc. of plastic and additives.

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Curcumin (Cur) is the main component of turmeric. Cur performs various physiological actions; however, it is poorly soluble in water. Because Cur is barely absorbed by the body, its activity is minimal. We have developed an amorphous formulation of Cur that displays improved water solubility and bioavailability. In this study, we analyzed cancer cell cytotoxicity of amorphous Cur and the conventional formulation (unformulated powders of Cur and commercial formulation of Cur) dispersed in water, to compare the functional expression of Cur. In the cytotoxicity assay against HepG2 cancer cells, amorphous Cur exhibited high cytotoxicity, while the unformulated and commercial Cur exhibited almost no cytotoxicity. These findings contradicted previous reports describing the cancer cell cytotoxicity of commercial Cur. This variation may be due to poorly water-soluble reagents, such as inhibitors, being dissolved in dimethyl sulfoxide (DMSO) prior to dilution with the medium. Thus, we hypothesized that the functional expression of Cur depended on the solvent used for initial dispersion. We evaluated the dispersibility of each Cur formulation in water or DMSO. Visual and microscopic observations revealed that only the amorphous Cur was water-soluble. This likely reflects the presence of crystal particles in unformulated and commercial Cur, which restricted their solubility in water. Conversely, the Cur formulation completely dissolved when dispersed in DMSO. To evaluate the cytotoxicity of each Cur formulation in water or DMSO, HepG2 cancer cells were treated with each formulation. In case of the Cur formulation dissolved in water, only the amorphous Cur showed cytotoxicity; in contrast, all Cur formulations dispersed in DMSO showed cytotoxicity. The collective data demonstrate that the cytotoxicity of Cur against HepG2 cancer cells depends on the solvent used for the initial dispersion. These findings suggest the importance of designing an experimental method according to the purpose of the research.

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The crude drug “Sensoutou” is derived from a whole plant of the toothed clubmoss (Huperzia serrata). In 2021, “Sensoutou” was classified as “raw materials used as non-pharmaceuticals” in Japan and health food products, such as dietary supplements derived from toothed clubmoss, are sold commercially. Huperzine A, an alkaloid isolated from H. serrata, inhibits acetylcholinesterase and is expected to be a therapeutic agent for Alzheimer’s disease. However, there have been reports of health problems caused by foods containing Huperzine A. This study conducted qualitative and quantitative analyses using UHPLC-PDA-MS on 13 health food products related to toothed clubmoss. Qualitative analysis showed that Huperzine A was detected in 10 of the 13 samples. The maximum daily intake of Huperzine A calculated from the results of the quantitative study was between 7.83 and 691.68 μg/day. These products derived from toothed clubmoss may have health risks because the acceptable daily intake of Huperzine A calculated from a previous toxicity study was 3.03 μg/day. Incidentally, in Japan, “Sensoutou” was reclassified from “raw materials used as nonpharmaceuticals” to “raw materials exclusively used as pharmaceuticals” on February 25, 2022.

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Applying the statistical methods on the food analysis data plays important role in the field of food safety, food development, research, and quality control, etc. In this paper, an application example by data science in food analysis using the aroma component data of commercial canned coffee obtained by analysis was introduced. The aroma components of 6 types of fragrance-free products and 6 types of fragrance-added products of canned coffee were analyzed using headspace GC/MS. Analytical data of aroma components contained in coffee was statistically analyzed by R program. Four hundred ninety aroma compounds were extracted by the estimation of GC/MS library search (NIST MS library). Principal component analysis, cluster analysis, False Discovery Rate (FDR) test, etc. were applied to the estimated compounds, and they were classified into two groups, fragrance-added and fragrancefree coffee. Statistical methods are one of the important tools in food analysis as demonstrated by this article, and analytical ability is especially useful for food research and food development.

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