A simple determination method of dinoseb and dinoterb in agricultural products, livestock products and seafood by LC-MS/MS was developed. Agricultural samples were extracted with acetone (in the case of rice, soybean and tea leaf, phosphoric acid was added). An aliquot of crude extract was partitioned with hexane and sat. sodium chloride solution. In the case of livestock products and seafood, samples were extracted with a mixture of acetone, hexane, water and sodium chloride, and the organic layer was collected. Clean-up was performed using a PSA mini column. The LC separation was performed on a C18 column with methanol–water (19 : 1) containing 0.005 v/v% acetic acid as a mobile phase, and MS with negative ion electrospray ionization was used for detection. The calibration curve was linear between 0.0005 to 0.04 μg/mL for each compound. Average recoveries (n=5) of dinoseb and dinoterb from 20 kinds of agricultural products, livestock products and seafood fortified at the MRLs were 77–111%, and the relative standard deviations were 2–15%. The limits of quantitation were 0.001 μg/g for both compounds.
The Tokyo Electric Power Company's Fukushima Daiichi nuclear power plant disaster after the Great East Japan Earthquake has caused radioactive contamination in food. Using the market basket method, total diet samples in Tokyo, Miyagi prefecture and Fukushima prefecture were analyzed for cesium-134 and -137 (radioactive cesium) and naturally occurring potassium-40 (radioactive potassium) in order to estimate the committed effective doses of these radioactive materials from food. Doses were calculated on the assumption that “not detected” corresponded to zero or to half the limit of detection (values in brackets). The estimated doses of radioactive cesium in Tokyo, Miyagi and Fukushima were 0.0021 (0.0024), 0.017 (0.018) and 0.019 (0.019) mSv/year, respectively. Although the doses in Miyagi and Fukushima were more than 8 times the dosein Tokyo, they were significantly lower than the maximum permissible dose (1 mSv/year) determined by the Ministry of Health, Labour and Welfare, Japan. The estimated doses of naturally occurring radioactive potassium in these areas were in the range of 0.17–0.20 (0.18–0.20) mSv/year, and there were no significant differences between the areas.
A method for the simultaneous determination of multiple pesticide residues in agricultural products was developed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The sample was extracted with acetonitrile. Co-extractives were removed by GPC/graphitized carbon column SPE, and silica gel/PSA cartridge column SPE. Pesticides in the test solution were determined by LC-MS/MS using scheduled MRM. Recoveries of 124 pesticides from spinach, brown rice, soybean, orange and tomato were tested at the level of 0.1 μg/g, and those of 121 pesticides ranged from 70 to 120% (RSD≤15%). Pesticide residues in 239 agricultural products were investigated by this method, and residues of 49 pesticides were detected in 98 agricultural products.
In this article, we report a novel real-time PCR-based analytical method for quantitation of the GM maize event LY038. We designed LY038-specific and maize endogenous reference DNA-specific PCR amplifications. After confirming the specificity and linearity of the LY038-specific PCR amplification, we determined the conversion factor required to calculate the weight-based content of GM organism (GMO) in a multilaboratory evaluation. Finally, in order to validate the developed method, an interlaboratory collaborative trial according to the internationally harmonized guidelines was performed with blind DNA samples containing LY038 at the mixing levels of 0, 0.5, 1.0, 5.0 and 10.0%. The precision of the method was evaluated as the RSD of reproducibility (RSDR), and the values obtained were all less than 25%. The limit of quantitation of the method was judged to be 0.5% based on the definition of ISO 24276 guideline. The results from the collaborative trial suggested that the developed quantitative method would be suitable for practical testing of LY038 maize.
Performance evaluation methods and criteria for trans-fatty acids analysis using GC-FID were examined. The measurement method constructed in this study was based on the American Oil Chemists' Society (AOCS) official standard methods Ce1h-05. The method for fat extraction from general foods was based on the methods for nutrition labeling notified by the Ministry of Health, Labour and Welfare of Japan and AOAC 996.06. To estimate trueness and precision, fortified samples were analyzed following the established experimental design. Five molecular species of trans-fatty acids that are rarely contained in foods were used for preparing the fortified samples. To estimate precision, more than four degrees of freedom of variance are required. Based on the results, within-laboratory trueness and reproducibility will be set at 90–110% and 10% (RSD%), respectively.
From January to June 2009, a total of 64 gastropod specimens of 15 species were collected from the coastal waters of Okinawa Prefecture, Japan, and examined for toxicity by means of mouse bioassay. Among the specimens tested, 5 species, Nassarius glans, Nassariuscoronatus, Olivaannulata, Oliva concavospira and Zeuxis sp., were toxic. The toxicity scores of N. glans were very high; 39.6–461 MU/g in muscle, and 98.6–189 MU/g in viscera including digestive gland, followed by Zeuxis sp. (12.7 MU/g in whole body), N. coronatus (5.64–11.1 MU/g in whole body), O. annulata (10.8 MU/g in the whole body), O. concavospira (6.65 MU/g in the muscle). Liquid chromatography/mass spectrometry (LC-MS) revealed that the major toxic component was tetrodotoxin (TTX), which accounting for 13–82% of the total toxicity. As for the remaining toxicity in the case of N. glans, 4,9-anhydroTTX, 4-epiTTX and 11-oxoTTX were contributors. Moreover, Niotha albescens showed no toxicity (less than 10 MU/g) in mouse bioassay, but TTX (5.08 MU/g) was detected by LC-MS. Paralytic shellfish poison was not detected in any of the specimens by high-performance liquid chromatography with fluorometric detection (HPLC-FLD).
Herb-drug interactions are mainly mediated by hepatic cytochrome P450 (CYP) enzymes. Here, we examined the effect of three herbs (valerian, salacia and black cohosh) on CYP activity in vivo in mice and in liver microsomes in vitro. Extracts which showed activity in the preliminary tests were then fed to mice at various doses (0, 0.5, 1.5 and 4.5%). Valerian did not show any effect on hepatic CYPs. Black cohosh increased the liver weight, total CYP content and CYP activities (2B and 3A) in a dose-dependent manner (up to 4.5%). Salacia inhibited CYP1A2 activity in liver microsomes in vitro. Also, salacia at the dietary dose of 4.5% suppressed body weight gain, decreased hepatic total CYP content and increased CYP activities (1A1, 2B and 2C). These findings suggest that black cohosh and salacia at high dose affect the activity of hepatic CYPs, and therefore may interact with drugs that are metabolized by CYP.
We investigated the change of radioactive cesium content in food due to cooking in order to estimate the internal radiation exposure due to from radioactive materials in food. Our results revealed that soaking dry shiitake in water decreased the radioactive cesium content by about 50%, compared with that present in uncooked shiitake. Radioactive cesium in beef was decreased by about 10%, 12%, 60–65% and 80% by grilling, frying, boiling and stewing, respectively, compared to uncooked beef. For cooked beef, the decrease in the ratio of radioactive cesium was significantly different among the types of cooking. The decrease ratio of radioactive cesium in boiled and stewed beef was 8 times higher than that in grilled and fried beef.
Enzymatically hydrolyzed guar gum (EHGG), which is used as a thickener or a soluble dietary fiber, is produced by partial hydrolysis of the guar gum (GG) backbone using mannan endo-β-1,4-mannosidase. In this study, we compared and evaluated 3 methods to distinguish EHGG from other polysaccharides used as food additives or monosaccharides. The first method is based on cross-linking reaction of saccharide hydroxyl groups mediated by borate ions. EHGG showed gelation and was distinguished from some soluble polysaccharides, which did not form gels, and also from polysaccharides with low solubility in water. The second method is based on co-gelation with xanthan gum. It was applicable to GG, but not to EHGG. The third method is based on the alcohol precipitation of hydrophilic polymers. EHGG, some soluble polysaccharides and monosaccharides were dissolved in water at the concentration of 10%, while GG and some polysaccharides were not. The 10% solutions thus obtained were mixed with 2-propanol at the ratio of 1 : 1 (v/v). A white precipitate was formed in the EHGG solutions and the tested soluble polysaccharide solutions, while it was not produced in the monosaccharide solutions. This result demonstrated that soluble polysaccharides including EHGG can be distinguished from polysaccharides with low solubility or monosaccharides by the third method.
To validate an LC-MS/MS method for simultaneous determination of deoxynivalenol (DON) and its acetylated derivatives, 3-acetyl-deoxynivalenol (3ADON) and 15-acetyl-deoxynivalenol (15ADON), in wheat using a multifunctional column, an inter-laboratory study was performed in 9 laboratories using one blank wheat sample, three spiked wheat samples (10, 50, 150 μg/kg) and one naturally contaminated wheat sample. The recoveries ranged from 98.8 to 102.6% for DON, 89.3 to 98.7% for 3ADON, and from 84.9 to 90.0% for 15ADON. The relative standard deviations for repeatability (RSDR) and reproducibility (RSDR) of DON were in the ranges of 7.2–11.3% and 9.5–22.6%, respectively. For 3ADON, the RSDR ranged from 5.3 to 9.5% and the RSDR ranged from 16.1 to 18.0%, while for 15ADON, the RSDR ranged from 6.2 to 11.2% and the RSDR ranged from 17.0 to 27.2%. The HorRat values for the three analytes ranged from 0.4 to 1.2. These results validate this method for the simultaneous determination of DON and its acetylated derivatives, 3ADON and 15ADON.