Hyogo Prefectural Institute of Public Health and Consumer science

Kōbe-shi, Japan

Hyogo Prefectural Institute of Public Health and Consumer science

Kōbe-shi, Japan
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Matsuoka T.,Hyogo Prefectural Institute of Public Health and Consumer science | Akiyama Y.,Hyogo Prefectural Institute of Public Health and Consumer science | Mitsuhashi T.,Hyogo Prefectural Institute of Public Health and Consumer science
Journal of Pesticide Science | Year: 2011

A multi-residue analytical method for 185 pesticides (including metabolites) in meat products was validated by the guideline of the Japanese Ministry of Health, Labour and Welfare. This method involved extraction with ethyl acetate-cyclohexane (1 : 1) and cleanup by gel permeation chromatography (GPC), and primary secondary amine (PSA) and silica-gel mini-column solidphase extraction (SPE). The target compounds were determined by gas chromatography/mass spectrometry (GC-MS) and liquid chromatography/mass spectrometry (LC-MS). Validation tests were performed on beef, chicken and pork muscles fortified at 0.01 and 0.10 μg/g. Among 185 pesticides tested, 175 in beef, 175 in chicken and 172 in pork were found to conform to the guideline when the solvent standard was used, and 181 in beef, 176 in chicken and 177 in pork when the matrix-matched standard was used. Although significant matrix effects were not observed for most pesticides, use of the matrix-matched standard was preferable for accurate quantitation to the solvent standard. Limits of quantitation (S/N ≥10) were set at 0.01m g/g for all pesticides. The method was applied to the regulatory monitoring of meat products. © Pesticide Science Society of Japan.


Akamatsu S.,Hyogo Prefectural Institute of Public Health and Consumer science | Mitsuhashi T.,Hyogo Prefectural Institute of Public Health and Consumer science
Journal of Separation Science | Year: 2014

This study describes a method for the simultaneous determination of 12 synthetic cannabinoids by MEKC-MS/MS using a volatile surfactant (ammonium perfluorooctanoate) as a constituent of the micellar pseudostationary phase. Although most synthetic cannabinoids comigrated by a CZE method, sufficient separation could be achieved by the proposed method. The best separation was made possible by 50 mM ammonium perfluorooctanoate in 20% v/v acetonitrile/water (apparent pH* 9.0) as the BGE, followed by MS detection using a sheath liquid composed of 5 mM ammonium formate in 50% v/v methanol/water mixed hydro-organic solvent. The standard calibration curve for all analytes showed good linearity (r > 0.99). Satisfactory recoveries, ranging from 89.5 to 101.7%, were obtained. The LODs were 6.5-76.5 μg/g for the target analytes. This method appears to be a useful tool for the identification of synthetic cannabinoids in illegal herbal incense blends. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.


Akamatsu S.,Hyogo Prefectural Institute of Public Health and Consumer science | Mitsuhashi T.,Hyogo Prefectural Institute of Public Health and Consumer science
Journal of Food Composition and Analysis | Year: 2013

A simple capillary electrophoresis-tandem mass spectrometry (CE-MS/MS) method was developed for the analysis of free amino acids in commercial royal jelly (RJ) products containing various kinds of matrices. This method required no concentration step for sample preparation, and all 16 amino acids were determined without derivatization. The CE separation was achieved in an uncoated fused-silica capillary using a 1. M formic acid solution (pH 1.8) as the electrolyte, followed by MS/MS detection after mixing with a sheath liquid comprising 50% (v/v) methanol. The limits of detection (LODs) ranged from 0.61 to 10.5. μg (dry weight)/g for each amino acid. The recoveries for tablets, liquid drinks, and raw materials ranged from 88.3 to 108.6%, and the relative standard deviations (RSDs) were within 10%. The method was applied to 17 commercial RJ products, and the results were compared to those for honey. The relative proportions of free amino acids were specific for each RJ product, and the method was found to be useful in distinguishing not only among the different RJ products but also between RJ and honey. © 2013 Elsevier Inc.


Yoshioka N.,Hyogo Prefectural Institute of Public Health and Consumer science | Akamatsu S.,Hyogo Prefectural Institute of Public Health and Consumer science | Mitsuhashi T.,Hyogo Prefectural Institute of Public Health and Consumer science | Todo C.,Hyogo Prefectural Institute of Technology | And 2 more authors.
Forensic Toxicology | Year: 2014

A simple and rapid method for the determination of nine mushroom toxins, ibotenic acid, propargylglycine, choline, muscimol, muscarine, α-amanitin, β-amanitin, phalloidin, and phallacidin, in mushroom samples has been developed. Mushroom toxins were extracted with 0.5 % formic acid in methanol/water, purified with Oasis HLB cartridges, and analyzed by liquid chromatography-time-of-flight mass spectrometry. The separation was performed on a pentafluorophenylpropyl column, and the mass spectrometer was operated in positive ion mode with electrospray ionization. Calibration curves were linear over the range of 0.01-1 μg/ml (R 2 = 0.999). The detection limits for the toxins in mushroom samples were 0.0098-4.9 μg/g, which were low enough for the investigation of food poisoning cases. The intraday and interday recoveries for blank mushroom extracts fortified with mushroom toxins were 72.5-107 % and 75.9-108 %, and relative standard deviations were <7.9 and 8.2 %, respectively. © 2013 Japanese Association of Forensic Toxicology and Springer Japan.


Akamatsu S.,Hyogo Prefectural Institute of Public Health and Consumer science | Yoshida M.,Hyogo Prefectural Institute of Public Health and Consumer science
Journal of Mass Spectrometry | Year: 2016

This study described a fragmentation pattern of 21 synthetic cannabinoids with an isopropyl group or a tert-butyl group by electron impact ionization quadrupole mass spectrometry and electrospray ionization time-of-flight mass spectrometry in the positive mode. The compounds were categorized into four types according to substituted group such as a terminal amide and ester. The characteristic fragment ion in each group was obtained. The main common fragment ions for the two ionizations were formed by C-N cleavage of the amide group adjacent to the N-hetero rings. Additionally, the fragment ions indicated the difference in the basic structure as well as substituted group, which are useful for estimating the chemical structures of unknown compounds. Copyright © 2015 John Wiley & Sons, Ltd. Copyright © 2015 John Wiley & Sons, Ltd.


Takeda N.,Hyogo Prefectural Institute of Public Health and Consumer science | Matsuoka T.,Hyogo Prefectural Institute of Public Health and Consumer science | Gotoh M.,Hyogo Prefectural Institute of Public Health and Consumer science
Chromatographia | Year: 2010

Immobilized metal ion affinity chromatography (IMAC) was evaluated as a sample pretreatment tool for residual veterinary drugs (VDs) in food. A test of six cations for the IMAC efficiency revealed that Cu 2+ and Fe 3+ were suitable in retaining tetracyclines, quinolones (QLs: fluoroquinolones, acid quinolones), macrolides, β-lactams, and aminoglycosides, but ineffective for sulfonamides and hormones. These results showed the IMAC had great potential for a multiclass multiresidual VDs analysis in a simple and selective way. This methodology was applied on milk analysis for eleven QLs, involving extraction with (1:1) acetonitrile/methanol and IMAC with Fe 3+. Averaged recoveries ranged from 68 to 93% and limits of quantitation from 2 to 26 ng mL -1. Ten commercial milk samples were found to be free from the QLs. © 2010 Vieweg+Teubner Verlag | Springer Fachmedien Wiesbaden GmbH.


Yoshioka N.,Hyogo Prefectural Institute of Public Health and Consumer science | Asano M.,Kobe University | Kuse A.,Kobe University | Mitsuhashi T.,Hyogo Prefectural Institute of Public Health and Consumer science | And 2 more authors.
Journal of Chromatography A | Year: 2011

We developed a simple and rapid method for the simultaneous determination of phosphorus-containing amino acid herbicides (glyphosate, glufosinate, bialaphos) and their major metabolites, aminomethylphosphonic acid (AMPA) and 3-methylphosphinicopropionic acid (MPPA), in human serum. Serum samples were filtrated through an ultrafiltration membrane to remove proteins. The filtrate was then washed with chloroform, and injected into a liquid chromatography-tandem mass spectrometry (LC-MS/MS) system. Chromatographic separation was achieved on a hydrophilic interaction chromatography (HILIC) column. Determination of the target herbicides and metabolites was successfully carried out without derivatization or solid phase extraction (SPE) cartridge clean-up. The recoveries of these compounds, added to human serum at 0.2. μg/mL, ranged from 94% to 108%, and the relative standard deviations (RSDs) were within 5.9%. The limits of detection (LODs) were 0.01. μg/mL for MPPA, 0.02. μg/mL for AMPA, 0.03. μg/mL for both glyphosate and glufosinate, and 0.07. μg/mL for bialaphos, respectively. © 2011 Elsevier B.V.


Akamatsu S.,Hyogo Prefectural Institute of Public Health and Consumer science | Mitsuhashi T.,Hyogo Prefectural Institute of Public Health and Consumer science
Drug Testing and Analysis | Year: 2014

A simple capillary electrophoresis tandem mass spectrometry method was developed for the simultaneous determination of 20 pharmaceutical components such as cathartics and appetite suppressants in dietary supplements for weight loss. This method allowed multidrug target screening and confirmation in differing radically in chemical structure. The separation was achieved on an uncoated fused-silica capillary using 20 mM ammonium formate in 20 % v/v acetonitrile-water (pH 8.0) as the electrolyte, followed by detection mixed with a sheath liquid that consisted of a mixture of 5 mM ammonium formate and 0.1 % v/v formic acid in 50 % v/v methanol-water. Samples were hydrodynamically injected and separated at 30 kV within 25 min. The limits of detection were 1.0-750 μg/g for the target analytes. The method was successfully applied to 12 dietary supplements for weight loss and 3 non-prescription drugs. The proposed method was suitable as the determination and identification of pharmaceutical components in dietary supplements for weight loss. © 2013 John Wiley & Sons, Ltd.


Akamatsu S.,Hyogo Prefectural Institute of Public Health and Consumer science | Mitsuhashi T.,Hyogo Prefectural Institute of Public Health and Consumer science
Food Chemistry | Year: 2012

A simple capillary electrophoretic method was developed for the determination of glucosamine using in-capillary derivatisation. Glucosamine in commercial products was extracted with purified water. The CE separation was achieved on an uncoated fused-silica capillary using a 20 mM borate buffer (pH 9.2) containing 5 mM o-phthalaldehyde (OPA) and 5 mM 3-mercaptopropionic acid (MPA) at 25 kV, followed by UV detection at 340 nm. The detector response was linear (r 2 > 0.999) in the concentration range 10-1000 μg/mL. The limit of detection (LOD) was 1.3 mg/g. Spiked glucosamine recoveries at 50 and 100 mg/g level were 95.1% and 104.3%, respectively. The method was applied to 16 commercial products. The concentrations of glucosamine were 109-705 mg/g, and the ratios of detected glucosamine content to the labelled value were 88.8-124%. No significant bias was observed (r 2 = 0.989, p < 0.01), between results obtained by the proposed CE method and an official colorimetric method (Japanese Health Food & Nutrition Food Association). © 2011 Elsevier Ltd. All rights reserved.


Takeda N.,Hyogo Prefectural Institute of Public Health and Consumer science | Gotoh M.,Hyogo Prefectural Institute of Public Health and Consumer science | Matsuoka T.,Hyogo Prefectural Institute of Public Health and Consumer science
Food Additives and Contaminants - Part A Chemistry, Analysis, Control, Exposure and Risk Assessment | Year: 2011

An efficient LC method was developed for screening the presence of quinolones (QLs) - comprising fluoroquinolones (FQs) and acidic quinolones (AQs) - residues in various livestock and fishery products. Targeted analytes were for nine FQs of marbofloxacin (MAR), ofloxacin (OFL), norfloxacin (NOR), ciprofloxacin (CIP), enrofloxacin (ENR), danofloxacin (DAN), orbifloxacin (ORB), difloxacin (DIF) and sarafloxacin (SAR), and three AQs of oxolinic acid (OXA), nalidixic acid (NAL) and flumequine (FMQ). Samples comprised ten different food products covering five matrices: muscle (cattle, swine and chicken), liver (chicken), raw fish (shrimp and salmon), egg (chicken), and processed food (ham, sausage and fish sausage). This method involved a simple extraction with (1:1) acetonitrile-methanol, a highly selective clean-up with an immobilised metal chelate affinity column charged with Fe 3+, a fast isocratic LC analysis using a short column (20mm ×4.6mm, 3μm) with a mobile phase of (15:85:0.1) methanol/water/formic acid, and fluorescence detection (excitation/emission wavelengths of 295 nm/455 nm for FQs (495 nm for MAR), and 320 nm/365 nm for AQs). Among FQs, pairs of NOR/OFL, ORB/DIF and ENR/DAN were incompletely resolved. A confirmatory LC run with a Mg 2+ containing methanolic mobile phase was also proposed for the samples suspected of being positive. The optimised method gave satisfactory recoveries of 88.5% (56.1-108.6%) and 78.7% (44.1-99.5%) for intra- and inter-day assays with relative standard deviations of 7.2% (0.7-18.4%) and 6.8% (1.4-16.6%), respectively. Limits of quantitation ranged from 0.8 μg kg -1 (DAN) to 6.5 μg kg -1 (SAR). This method was successfully employed to analyse 113 real samples and two positive samples were found: fish sausage (CIP 990 μg kg -1) and shrimp (ENR 20 μg kg -1). © 2011 Taylor & Francis.

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