The effects of processing to produce various types of tea or infusion on the levels of pesticide residues in tea were investigated for three insecticides (chlorfenapyr, pyrimiphos-methyl, and clothianidin). Tea plants were sprayed with one of the three pesticides and cultivated under cover. The levels of pesticide residues in tea decreased after processing according to the time and temperature of heating, as well as fermentation. Although significant differences were not observed among the three pesticides in the ratio of decreased of pesticide concentration after processing to green tea, clothianidin, which is a neonicotinoid insecticide and has a lower log Pow value, tended to be transferred more than the other two insecticides into infusions. However, no significant difference in the ratios of clothianidin transferred to infusions was observed among green tea with three different leaf sizes.
To validate an LC-MS/MS method using a strong anion exchange cartridge for simultaneous determination of fumonisin B1, B2 and B3 in corn, an inter-laboratory study was performed in 9 laboratories using one fumonisin-negative corn sample, three spiked corn samples (FB1: 100–1,000 μg/kg, FB2 and FB3: 10–100 μg/kg) and two naturally contaminated corn samples. The recoveries were in the ranges of 79.7–87.2% for FB1, 78.6–103.2% for FB2 and 80.1–92.8% for FB3. The relative standard deviations for repeatability (RSDr) ranged from 3.7 to 8.0% for FB1, from 2.6 to 15.3% for FB2 and from 4.3 to 9.7% for FB3. The relative standard deviations for reproducibility (RSDR) for FB1, FB2 and FB3 were in the ranges of 6.3–10.1%, 5.9–18.7% and 9.3–16.0%, respectively. The HorRat values for all analytes ranged from 0.2 to 0.9. The difference of the trueness between the two kinds of commercially available anion exchange cartridges used in this study was not significant (p>0.05). Surveillance for fumonisins in corn grits was performed using the validated method. All of the samples were contaminated with fumonisins and the mean concentrations for FB1, FB2 and FB3 were 118.1, 37.3 and 17.9 μg/kg, respectively. These results indicated that the method for simultaneous determination of FB1, FB2 and FB3 in corn was successfully developed and validated.
Livers from wild pufferfish, Takifugu rubripes, can be described as having a smooth frontal side and an upper-region that is attached to the hepatic portal vein. Based on this description, the liver can be divided into 10 parts (L1–5 and R1–5), and in this work, the lethal potency of each part was determined by mouse bioassay. Among the raw livers from 58 individuals, all 10 parts of 16 individuals, and some parts of 4 individuals showed mouse lethality, but no toxicity was detected in any part of the liver from 22 individuals. In the livers of 4 individuals that were partially toxic, the lethal potency of the toxic parts was less than 4 mouse units (MU)/g, and no part showed especially high toxicity. The remaining 16 individuals were considered non-toxic based on the assay of only one part. Among 13 frozen livers, all parts of 9 individuals were toxic, while all parts of 4 individuals were non-toxic. Liquid chromatography-mass spectrometry analysis revealed that all parts of a weakly toxic raw liver and a strongly toxic frozen liver had tetrodotoxin as the major toxin. Regarding the 16 raw and 9 frozen livers, whose parts were all toxic, the relative lethal potency of each part to the mean lethal potency of the individual (8.9–709 MU/g) was calculated, and subjected to a two-way analysis of variance with 2 factors (left/right and top/bottom) for each group of livers (raw or frozen). The analysis indicated non-significance among factors and interactions at a significance level of 5% in the frozen livers. However, in the raw livers, although no interaction between the 2 factors was detected, the right-side and the 4th-portion from the top were significantly higher than the left-side and the other portions, respectively. Therefore, we concluded that individual inspection using R4, which is the region that lies below the right-center location of the liver, is suitable for toxicity evaluation of liver to ensure the safe consumption of pufferfish.
Collecting adverse case reports suspected to be due to health foods and evaluation of the causality are important to secure safety, even if the causal relationship between health foods and reported health problem is uncertain. Case reports are mainly collected at three sites: public health centers, practical living information online network system(PIO-NET), and individual companies. The case reports from the three sources are not dealt with consistently. In this study, we investigated and characterized those case reports from the viewpoint of evaluating causality, using the causality association rating methods, namely, the dendritic and pointed methods, which we reported previously. Information in public health centers comprised 20 reports per year; approximately 40% were from health care providers and contained detailed medical data. PIO-NET information comprised 366 reports per year; 80% were self-reports from users, and few medical details were included. Company information covered 1,323 cases from 13 companies; more than 90% were from users and most of them were complaints. Case reports from public health centers and PIO-NET showed that the largerst number of victims were female aged >60, with allergy and gastrointestinal symptoms. When these case reports from the letter two sources were examined using the causality association rating systems, most were rated as “possible” and only a few were rated as “probable”. As specific case reports from different information sources were examined in this study, we were able to identify several points that should be improved in our two rating methods. However, to ensure the safety of health foods, it will be necessary to collect a large number of high-quality case reports for evaluation by a suitable causality rating method, and to integrate those evaluated case reports into a single site.
A method using dispersive and cartridge column solid-phase extraction (SPE) was developed for the simultaneous determination of veterinary drugs in livestock products by LC-MS/MS. The samples were extracted with 85% acetonitrile and cleaned up using dispersive and cartridge column SPE. Recoveries of 70 analytes fortified at the levels of 0.002 μg/g and 0.01 μg/g in cattle, swine and chicken muscles were examined. Among 70 analytes examined, 64 in cattle, 58 in swine and 49 in chicken satisfied the required Japanese validation guideline. The limit of quantitation values of the 70 analytes were 0.001 μg/g or 0.005 μg/g in three kinds of livestock products. This method is suitable to analyze 40 analytes in three kinds of livestock products at levels under the MRL.
It is important to obtain information about ways of removing radioactive cesium from foods in order to reduce internal radiation exposure from food and to ensure the safety and security of food. In this study, we investigated the change of radioactive cesium content in beef due to soaking in seasoning. Our results revealed that soaking beef in liquid seasoning (salt concentration: 8–10%) for 24 h or in miso seasoning (salt concentration: about 9%) for 7 days decreased the radioactive cesium content by about 20% and 55%, respectively, compared with that present in beef before soaking. Furthermore, soaking beef in 10% salt solution for 7 days while changing the salt solution every day or every three days decreased the radioactive cesium content by about 75%, compared with that present in beef before soaking. Because the seasoning is usually discarded after soaking, the procedure of soaking beef in seasoning is a useful method of reducing the burden of radioactive cesium.
In Japan, seafood may be eaten raw or after having been cooked in diverse ways. Therefore, it is important to understand the effect of cooking on the extent of contamination with radioactive materials in order to avoid internal exposure to radioactive materials via seafood. In this study, we investigated the changes in radioactive cesium content in pond smelt cooked in four different ways: grilled, stewed (kanroni), fried and soaked (nanbanzuke). The radioactive cesium content in grilled, kanroni and fried pond smelt was almost unchanged compared with the uncooked state. In contrast, radioactive cesium content in nanbanzuke pond smelt was decreased by about 30%. Our result suggests that soaking cooked pond smelt in seasoning is an effective method of reducing the burden radioactive cesium.
DNA was extracted from sweet corn and its processed products using four DNA extraction methods: the CTAB method, the DNeasy Plant Maxi kit, GM Quicker 3, and Genomic-tip 20/G. DNA was successfully extracted from raw sweet corn and baby corn samples using all four methods. Meanwhile, from frozen, canned, and dry pack products, DNA was well extracted using the DNeasy Plant Maxi kit, GM Quicker 3, and Genomic-tip 20/G, but not enough with the CTAB method. The highest yield of DNA was obtained with Genomic-tip 20/G. The degree of degradation of extracted DNA was observed to increase in the order of raw, frozen, canned, dry pack, and baby corn samples. To evaluate the quality of extracted DNA, real-time PCR analyses were conducted using three maize endogenous genes. The DNAs extracted using GM Quicker 3 had high purity, suggesting that GM Quicker 3 would be the most suitable method for DNA extraction from processed sweet corn products.
A survey of pesticide residues in 313 samples of imported spices and herbs on the Tokyo market from April 1997 to March 2011 was carried out. Thirty-seven kinds of pesticides, including organophosphorus, organochlorine, pyrethroid, carbamate and others, were detected between levels of trace (below 0.01 ppm) and 3.3 ppm from 64 samples. The rate of detection was highest in peel (100%) followed by stem (66.7%), fruit (34.5%), bark (33.3%), flower (31.3%) and leaf (14.7%). No residues were detected in root, seed or whole grass. Organochlorine pesticides were detected in all plant parts. The insecticides were detected in products from all production areas, suggesting that their use is common. Residue levels of these pesticides were calculated as less than 1% of their ADI values, based on the daily intake of spices and herbs. Therefore, these spices and herbs should be safe when consumed in customary amounts.
We examined changes in the quality of drinking water stockpiled under various conditions for emergency use. The results indicated that the change in the quality of the stocked water was influenced mainly by the preservation period and not by the amount of water in the bottle. To maintain water quality, the amount of residual chlorine is less important than using sufficiently sterilized water, bottles and caps in the bottling process. Washing the bottles with a small amount of boiling water was not sufficient to ensure complete inhibition of microbial growth.
Basic principles for simulation of acute reference dose (ARfD) setting were defined based on the work of Solecki et al. (2005). The principles are: (1) Appearance of acute toxicity within 24 h after oral administration. (2) Rationale for setting toxicity that appears or could appear after single oral administration. (3) ARfD setting is assumed to be necessary for all pesticides. (4) ARfD setting is not necessary when the value is at or above the cutoff level. (5) The setting basically applies to the general population. (6) ARfD is set based on the lowest NOAEL among all the available study data concerning endpoints for acute effects. (7) Effects of exposure during critical periods should be considered as endpoints for ARfD setting. (8) The approach for the safety coefficient is the same as that for acceptable daily intake. (9) If available, human data are acceptable as an endpoint for ARfD setting.
A method of rapid analysis of multi-class residual veterinary drugs in milk, fish and shellfish was validated in accordance with Japanese guidelines for the validation of analytical methods for residual agricultural chemicals in food. Using LC-MS/MS, 43 multi-class veterinary drugs, including sulfonamides, quinolones, coccidiostats and antiparasites, could be analyzed in one injection. Analytes were extracted from samples with two kinds of solvent, acetonitrile containing 1 vol% formic acid and anhydrous acetonitrile, and salted out with 4.0 g of magnesium sulfate, 1.5 g of trisodium citrate and 2.0 g of sodium chloride. This method was assessed by performing recovery tests in retail milk and 4 kinds of fresh cultured fish and shellfish (salmon, tiger shrimp, red sea bream and bastard halibut) spiked with the 43 target analytes at the levels of 10 and 100 μg/kg. Using this method, 40 out of 43 drugs satisfied the guideline criteria in milk, 37 drugs in salmon, 42 drugs in tiger shrimp, 41 drugs in red sea bream and 39 drugs in bastard halibut.
In order to ensure compliance of raw bean paste products with the Japanese Food Sanitation Law, we examined the performance characteristics of an analytic procedure based on steam distillation followed by carbonate–pyrazolone assay to determine cyanogenic compounds in raw bean paste. The present method includes a procedure for decomposition cyanogenic glycosides using linamarase due to the possibility that cyanogenic glycoside-hydrolyzing enzymes might be deactivated in raw bean pastes. The performance of the method was evaluated using two types of bean paste spiked with a cyanogenic glycoside (linamarin) corresponding to cyanide ion concentrations of 5 and 10 mg/kg. The trueness of the method was 86–90%, and the repeatability (RSD) was 1.0–2.4%, while the intermediate precision (RSD) was 2.6% to 4.9%. A surveillance of cyanogenic compounds in 28 raw bean pastes manufactured in Japan was then carried out with the validated method. One sample contained 15 mg/kg (as hydrogen cyanide), while the other samples contained less than 5 mg/kg.