Food Hygiene and Safety Science最新文献

An LC-MS/MS method for the simultaneous determination of chloroacetic acid, dichloroacetic acid and trichloroacetic acid (chloroacetic acids) in mineral water (MW) products was developed by modifying the Japanese official method to determine chloroacetic acids. To prevent ion suppression or enhancement caused by sample matrix in LC-MS/MS analysis, the Japanese official method comprises the cleanup step of analytes using cation exchange resin column. The step is time-consuming and costly, and thus the modified method adopted small-volume injection instead of it to prevent matrix effects on ionization, which enabled rapid analysis at low cost. A validation study was performed on the method using MW products which vary in the degree of hardness and contents of carbonate. The trueness, repeatability and reproducibility of the method were estimated to be within the ranges of 95.3 to 104.3%, 1.1 to 2.9% and 2.4 to 6.4%, respectively. The values of every performance parameter met the criteria in the guidelines announced by the Ministry of Health, Labour and Welfare of Japan. A recovery study was performed on 30 kinds of MW products to examine the applicability of the method, and the recovery rate of all target substances ranged from 91 to 108%. Therefore, the modified method is considered to be suitable for the determination of chloroacetic acids in MW products.

A validation study was performed on the modified analytical method for the determination of amines (triethylamine: TEA and tributylamine: TBA) content in polycarbonate food apparatuses, containers, and packaging, by using a mass spectrometer (MS) and a tandem mass spectrometer (MS/MS) to obtain higher selectivity, after solving problems such as TEA volatilization and TEA and TBA adsorption on the apparatuses. The repeatability, within-laboratory reproducibility and trueness of the LC-MS method was estimated in the range of 1.0-3.4%, 1.5-4.8%, and 96-98% for TEA and of 1.1-2.4%, 2.4-4.4%, and 96-97% for TBA, respectively. The repeatability, within-laboratory reproducibility and trueness of the LC-MS/MS method was estimated in the range of 1.2-3.5%, 1.7-7.3%, and 96-98% for TEA and of 1.1-2.4%, 2.2-5.7%, and 95-97% for TBA, respectively. These results showed that the method is useful as an analytical method for the determination of amines content.

The Codex Standard for Honey adopts diastase activity as an indicator of honey freshness and as a measure to detect overheating during the manufacturing process. However, in some cases a foreign amylase is added to honey to increase its diastase activity. In our previous study, we developed a simple and sensitive method for screening foreign amylases using native polyacrylamide gel electrophoresis followed by activity staining. In this study, to confirm the effectiveness of this method, a collaborative study involving 12 laboratories was conducted in accordance with the AOAC guidelines for qualitative analysis, targeting amylases derived from the Aspergillus and Geobacillus, which were frequently detected in Japan. From the probability of detection (POD) curve confirmed in the preliminary test, three concentrations (low, medium, and high) calculated as diastase numbers were set, and eight samples of each concentration (total of 24 samples) were distributed in a blind manner and evaluated. The results showed that while the POD at the middle level was higher than expected, the method demonstrated sufficient performance to determine the presence or absence of foreign amylase.

Lycorine and galanthamine are toxic alkaloids found in Narcissus. Using HPLC analysis and quantitative NMR analysis, the degrees of purity of these standard reference materials purchased in 2013, 2019, 2021, and 2025 were calculated and compared. The results showed almost no degradation of any component. However, other findings suggest that the lycorine hydrochloride weight changed because of moisture absorption (hydration). This weight change might be avoided by stocking lycorine hydrochloride monohydrate, which is originally hydrated. Maintaining a stock of lycorine and galanthamine reference materials is desirable for facilitating prompt response to food poisoning by Narcissus. Such poisoning incidents have increased rapidly in recent years. If stored properly after purchase according to the method described in the SDS, then the materials will maintain the purity indicated on the label for at least 10 years. They can be used for analysis without other purity measurement.

This study investigated the effective detection methods and contamination status of severe acute respiratory syndrome coronavirus 2 (SARS-CoV-2) on the surface of commercially available vegetables and fruits. SARS-CoV-2 RNA was detected by quantitative real-time RT-PCR. A comparison of swabbing methods using three types of materials and five wiping techniques revealed the highest recovery rate when using a polyester swab, wiping in four directions and suspending the swab in PBS after each swabbing direction. The recovery rate of the method was 8-26% on the surfaces of five different types of commercially available vegetables and fruits. Examination of effective washing for removing SARS-CoV-2 from the surface of eggplants showed that >90% of the virus could be removed by water wiping or scrubbing. A total of 90 commercially available vegetables (45 cucumbers and 45 tomatoes) purchased between June and October 2023 were tested to determine the status of SARS-CoV-2 contamination. Although the virus RNA was detected from only one cucumber purchased in August, the number of infectious viruses could not be determined. Results demonstrated that commercially available vegetables have low risks as a source of COVID-19 infection. Preventive measures such as practicing appropriate respiratory etiquette may contribute to the prevention of SARS-CoV-2 contamination in food products. Furthermore, washing the produce with water and basic infection control measures, including hand hygiene and mask wearing, are essential to reduce the risk of infection through food.

We isolated Phytolaccasaponins B, E and G, which are toxic components of Phytolacca americana. Highly purified products were extracted from Phytolacca americana root extract using silica gel, ODS, diol column chromatography. Using these components as analytical standards, we optimized the LC-MS/MS conditions and established 3 components simultaneous analysis method. In recovery tests, the average recovery ranged from 74 to 119%, with a repeatability of 1.0 to 7.1% RSD. Analyses of a 2018 food poisoning specimen indicated 3 toxic components in the leaves and 2 toxic components in the roots. Those findings suggest that the simultaneous analysis method was useful for a food poisoning specimen. These results show that this method is required for identifying food poisoning caused by Phytolacca americana, even when leftovers are unrecognizable or when the poisoning is caused by plant parts other than the roots.

In this study, a multi-residue method for pesticide residues in green tea leaves was developed using LC-MS/MS and the validity of the developed method was evaluated in accordance with Japanese guidelines. Based on the previously reported method, the amount of acetonitrile used for extraction, amount of hexane-washed distilled water added to the sample, and solid-phase column used for purification were investigated. In the developed method, the pesticides were extracted with 25 mL of acetonitrile after adding 10 mL of the hexane-washed distilled water to the sample and salted out. By cleaning the acetonitrile layer using Inert Sep^® PLS-3 (200 mg/20 mL) and Supelclean^TMENVI-Carb^TMII/PSA (300 mg, 600 mg/6 mL), the effect of the matrix on the green tea leaves was reduced. This method was validated by performing recovery tests at two concentrations (0.01 and 0.1 mg/kg) of 92 pesticides. Of the 92 pesticides, 84 met the criteria. The limit of quantification was 0.01 mg/kg, which is the uniform limit specified by the Food Sanitation Law of Japan. This study presents that the developed method is useful for the analysis of pesticide residues in green tea leaves.

Saxitoxin (STX) and its analogues produced by toxic dinoflagellates in marine environments are known as specific voltage-gated sodium channel blockers and can be detected by the mouse bioassay (MBA) that has been used as the official testing method for paralytic shellfish toxin monitoring systems worldwide. Considering animal welfare issues and improved performance of analytical instruments, it would be better to replace MBA with non-animal testing methods such as LC-MS/MS which have been recently reported for the detection of STXs in shellfish. However, STX itself is regulated by the Act on the Prohibition of Chemical Weapons, so the domestic use of the reference material is required with permission from the relevant government department. Therein, nontoxic enantiomeric STX (ent-STX) was developed as an alternative reference material for STX. In this study, the LC-MS/MS method using ent-STX-fortified scallops homogenate was validated in accordance with a previous report and CODEX-STAN 292-2008. The spiked concentrations of ent-STX were set to the regulatory limits of CODEX (0.8 mg of STX-2HCl equivalents/kg) and approximately half of the limits. The calibration standard solutions were prepared by dilution with solvent and non-toxic scallop extract, respectively, and were used to quantify the toxins by absolute calibration method. As a result of the validation, the results with ent-STX were found falling within all the guideline criteria (the trueness, repeatability, within laboratory re-producibility, and minimum applicable range). Moreover, ent-STX was used to confirm and quantify STX in mussels, scallops and noble scallops. The ent-STX was confirmed to be utilized as reference material. However, it can be sometimes detected an unidentified STX analogue in Japanese bivalve molluscs with retention time close to STX under the qualitative and quantitative selected reaction monitoring (SRM) conditions of STX which are often used in the previous reports. To avoid the assignment of the unidentified STX analogue to STX, appropriate SRM conditions of m/z 300.1>282.0 need to be selected.

In this study, we developed a simultaneous extraction method for 19 food additives, including sweeteners, preservatives, and antioxidants, to enhance testing efficiency across a wide range of processed foods. Samples underwent 2 or 4 extractions with acetonitrile containing 0.05 w/v% ascorbic acid palmitate, facilitated by the addition of water, phosphoric acid, magnesium sulfate, and sodium chloride. The extracts were then diluted and analyzed using instruments tailored to each specific compound. Recovery tests (n=5 or n=3) on 22 samples, encompassing high-protein, oily, and powdered foods, demonstrated satisfactory recovery rates between 76.6% and 111.6% (RSD: 0.1-6.6%). To validate the method, two concentrations-corresponding to the lower limit of quantification and the maximum permissible level-were added to two or three different samples per additives. This validation was conducted by a single analyst over two parallel runs across five days. The results indicated that the lower limit of quantification achieved trueness of 81.7-102.4%, repeatability of 0.3-6.3%, and within-laboratory reproducibility of 1.0-9.7%. Similarly, for the maximum level of use, trueness ranged from 80.6 to 105.5%, repeatability from 0.4 to 2.8%, and within-laboratory reproducibility from 0.6 to 4.3%, all meeting the target criteria. The developed method proves to be a valuable analytical tool, significantly enhancing the efficiency of food additive analysis.

Food allergen analysis using LC-MS/MS has attracted attention in recent years because it can analyze multiple allergens at the same time and has high detection sensitivity and specificity. We have been actively researching for developing this testing method using LC-MS/MS. In this study, we developed the simultaneous detection method for allergens using LC-MS/MS and conducted an interlaboratory validation study in three laboratories to evaluate the effectiveness of the developed method. The study was conducted using two types of model processed foods: rice porridge and pancake. A total of nine allergens were targeted (wheat, egg, milk, peanut, buckwheat, crustaceans (shrimp and crab), walnut, and soybean). The results of the interlaboratory validation study showed that the qualitative and quantitative tests demonstrated good accuracy and, with the exception of a few allergens, exhibited a high level of agreement when compared with other laboratories. This indicates that the developed method is practical as a screening method for simultaneous detection of food allergens and can be applied to foods containing allergens.