Here, we set out to improve our previously developed methylmercury analytical method, involving phenyl derivatization and gas chromatography-mass spectrometry (GC-MS). In the improved method, phenylation of methylmercury with sodium tetraphenylborate was carried out in a toluene/water two-phase system, instead of in water alone. The modification enabled derivatization at optimum pH, and the formation of by-products was dramatically reduced. In addition, adsorption of methyl phenyl mercury in the GC system was suppressed by co-injection of PEG200, enabling continuous analysis without loss of sensitivity. The performance of the improved analytical method was independently evaluated by three analysts using certified reference materials and methylmercury-spiked fresh fish samples. The present analytical method was validated as suitable for determination of compliance with the provisional regulation value for methylmercury in fish, set in the Food Sanitation haw.
A simultaneous determination method was examined for 312 pesticides (including isomers) in muscle of livestock and marine products by GC-MS. The pesticide residues extracted from samples with acetone and n-hexane were purified by acetonitrile–n-hexane partitioning, and C18 and SAX/PSA solid-phase extraction without using GPC. Matrix components such as cholesterol were effectively removed. In recovery tests performed by this method using pork, beef, chicken and shrimp, 237–257 pesticides showed recoveries within the range of 70–120% in each sample. Validity was confirmed for 214 of the target pesticides by means of a validation test using pork. In comparison with the Japanese official method using GPC, the treatment time of samples and the quantity of solvent were reduced substantially.
An accurate and selective analytical method for amantadine, which is used as antiviral drug to treat influenza A virus infection, was developed using LC-MS/MS. Residual amantadine was extracted from 4 kinds of food sample (poultry muscle, liver, gizzard and egg) with acetonitrile–pH 3.0 McIlvaine buffer (7 : 3), then cleaned up with an Oasis® MCX mini-cartridge. An external standard calibration curve was used for quantification, after sample purification by the combination of a reverse-phase strong cation exchange mixed mode cartridge for cleanup and a HILIC column for HPLC. The method was validated by performing recovery tests in accordance with Japanese guidelines for the validation of analytical methods for residual agricultural chemicals in food. Recovery ranged from 79.3% to 91.7%, RSDs of repeatability were under 3.3%, and RSDs of within-laboratory reproducibility were under 8.4%. This new method was applied to samples of poultry and egg purehased in Tokyo, but residual amantadine was not detected at all.
In this study, we developed methods to quantify lead, total arsenic and cadmium contained in various kinds of soft drinks, and we evaluated their performance. The samples were digested by common methods to prepare solutions for measurement by ICP-OES, ICP-MS and graphite furnace atomic absorption spectrometry (GF-AAS). After digestion, internal standard was added to the digestion solutions for measurements by ICP-OES and ICP-MS. For measurement by GF-AAS, additional purification of the digestion solution was conducted by back-extraction of the three metals into nitric acid solution after extraction into an organic solvent with ammonium pyrrolidine dithiocarbamate. Performance of the developed methods were evaluated for eight kinds of soft drinks.
Histopathological findings are important to the understanding of toxicity profiles of pesticides. The liver is often a target organ of chemicals. In the present study, histopathological findings in the liver cited in the pesticides risk assessment reports published by the Food Safety Commission of Japan were classified. The histopathological findings were obtained in repeated-dose 90-day oral toxicity studies of mice, rats and dogs and carcinogenicity studies of rodents. After the classification, a thesaurus was constructed based on the International Harmonization of Nomenclature and Diagnostic (INHAND) Criteria. We recommend the use of INHAND criteria in risk assessment reports to improve mutual understanding between applicants and risk assessors.
Analytical method by HPLC and LC-MS/MS for determining lycorine and galanthamine in processed food was newly developed. In this method, coagulant which has never been used in food analysis was applied on cleanup process. With coagulant approach, removal of interfering substances on determination for analytes was easily achieved. The method using HPLC showed recovery of 95.4–102.9% on both analytes with repeatability of less than 2.9% and reproducibility of less than 2.9%. The method using LC-MS/MS showed recovery of 97.4–107.6% with repeatability of less than 5.7% and reproducibility of less than 5.7%. On HPLC method, limit of quantification for lycorine was 0.004 g/kg and that of galanthamine was 0.006 g/kg. On LC-MS/MS method, limit of quantification for lycorine was 0.0008 g/kg and that of galanthamine was 0.0005 g/kg.
In order to determine trace amounts of lead in copper gluconate by atomic absorption spectrometry (AAS), the authors investigated a separation and pre-concentration procedure using a co-precipitation technique with bismuth. After ashing 2.0 g of the sample by means of a dry process, the ash was dissolved in (1→100) nitric acid and 75 μg of bismuth was added. Lead was co-precipitated by using an ammonium solution controlled to pH 9.5–10.5. The precipitate was left at room temperature for over 15 minutes to age, and then washed with a (3→100) ammonium solution three times. The precipitate was dissolved in (1→100) nitric acid and then analyzed by AAS. The quantification limit of this method was 0.5 mg/kg, and the trueness, repeatability and intermediate precision were 99.6%, 4.2% and 4.2% at the spiked concentration of 0.5 mg/kg, and 94.4%, 2.8% and 4.0% at the spiked concentration of 5.0 mg/kg, respectively. Thus, the present method for trace analysis of lead in copper gluconate was validated.
Pathogenic genes such as stx1, stx2, STh gene, STp gene, LT gene, invE, eae, aggR, afaD, astA, cdt and cnf were investigated in Escherichia coli isolated from cattle during Nov. 2012 and Aug. 2013. Plural pathogenic genes were concurrently detected by multiplex PCR, and screen-positive genes were confirmed and sub-classified by PCR. Among 100 cattle investigated, 180 E. coli strains with diarrheic genes (DEC) were detected in 79 cattle, and 45 of them, isolated from 32 cattle, were Shiga toxin-producing E. coli (STEC). More than 30% of cattle carried astA, cdt, cnf and stx2 in descending order. STh gene, LT gene, invE, aggR and afaD were not detected in this study. Both stx1 and stx2 were concurrently detected from 6 of 45 STEC strains and stx2 alone was detected from 19. Seventeen STEC strains carried STp gene, astA, or cdt along with stx1 or stx2. Additionally, 135 remaining DEC were classified into 18 enterotoxigenic E. coli with STp gene, 25 enteropathogenic E. coli with eae, and 92 other DEC with astA, cdt and cnf. Both O and H serotypes were identified in 48 strains, including O157 : H7, O1H7 and so on. O157 : H7 were identified in 3 strains that carried stx2 and eae together, as found in human pathogenic strains isolated from patients with gastroenteritis and hemolytic-uremic syndrome.
Using six kinds of zinc solution in water and 4% acetic acid as samples, an interlaboratory study was performed to evaluate a zinc (Zn) test method for food-contact rubber products, based on the Japanese Food Sanitation Law. Eighteen laboratories participated, and quantified Zn in six test solutions as blind duplicates using flame atomic absorption spectrometry, induced coupled plasma-optical emission spectrometry or induced coupled plasma-mass spectrometry. Statistical analysis revealed that the trueness, repeatability (RSDr) and reproducibility (RSDr) were 97–103%, 0.7–4.9% and 1.7–8.9% by all measuring methods. The values of the performance parameter fulfilled the target value (trueness: 80–110%, RSDr: 10%, RSDr: 25%). The performance of these methods is sufficient for testing the adherence of samples to the specifications.
July 27, 2015 There had been a system trouble (from July 26‚ 2015 15:25 to July 27‚ 2015 1:00 (GMT)). The service has been back to normal.
July 15, 2015 A new online journal "Mechanical Engineering Letters" has been launched by The Japan Society of Mechanical Engineers (JSME). This publication of such a letter journal is not only a new experience but also a tremendous challenge for the mechanical engineering society.
May 01, 2015 Please note the "spoofing mail" that pretends to be J-STAGE.