ABSTRACT
A simple, universal method to quantify soil methylmercury (MeHg) is not available. Here, we developed a solid-phase extraction-based method using gas chromatography mass spectrometry. MeHg was purified from the soil matrix using an optimized solid-phase extraction method, which reduced the use of organic solvents and eliminated the requirement for harmful reagents. The sample limit of quantification was 7.5 ng/g. MeHg recovery in the reference samples was 96.2%-102.6%; the intra- and inter-assay coefficients of variation were 3.4%-7.1% and 4.3%-7.1%, respectively, indicating high validation performance. This analysis method is simple as it can be performed using general-purpose reagents and instruments; has a high degree of trueness and accuracy; could be useful for soil MeHg quantification with improved sensitivity; and can provide reliable data to prevent MeHg contamination and improve food safety.
Subject(s)
Methylmercury Compounds , Gas Chromatography-Mass Spectrometry , Methylmercury Compounds/analysis , Soil/chemistry , Solid Phase ExtractionABSTRACT
The total mercury (T-Hg) and methylmercury (MeHg) concentrations in red snow crabs (Chionoecetes japonicus) caught off the coast of Japan were analyzed. The T-Hg concentration ranged from 0.03 to 0.56â¯mg/kg (mean: 0.21â¯mg/kg) in the raw muscle, and 0.02 to 0.74â¯mg/kg (mean: 0.27â¯mg/kg) in the boiled muscle. The MeHg concentration ranged from 0.04 to 0.54â¯mg/kg (mean: 0.20â¯mg/kg) in the raw muscle. The mean ratio of MeHg to T-Hg was 0.88. The crab body weight was found to significantly correlate with the concentrations of T-Hg (râ¯=â¯0.488) and MeHg (râ¯=â¯0.490) (pâ¯≤â¯0.01). For the general population in Japan, the intake of MeHg from eating red snow crab was estimated to be lower than 0.013â¯mg/week, which was less than one-sixth of the tolerable MeHg intake (0.08â¯mg/week).
Subject(s)
Brachyura/chemistry , Mercury/analysis , Methylmercury Compounds/analysis , Shellfish/analysis , Animals , Brachyura/growth & development , Brachyura/metabolism , Consumer Product Safety , Food Contamination/analysis , Humans , Japan , Mercury/metabolism , Methylmercury Compounds/metabolismABSTRACT
Histamine food poisoning is caused by ingestion of spoiled fish containing high levels of histamine. This paper reports cases in which histamine was detected in Osaka prefecture in fiscal year 2015 in a survey of fish and fishery products on the market and the food poisoning. A suspected case of histamine food poisoning was also evaluated to investigate the cause and minimize further problems. Histamine in food was separated on SPE cartridge columns, and analyzed after derivatization with fluorescamine by means of HPLC-FL. Histamine was detected in some fishery products on the market and in food that had caused poisoning. The samples in which histamine was detected were semi-dried whole round herring (Urumeiwashi-maruboshi), mackerel (Saba) and sardine dumpling (Iwashi-tsumire). These foods were the main causes of histamine food poisoning according to the report of the Ministry of Health, Labour and Welfare, Government of Japan.
Subject(s)
Fish Products/analysis , Fishes , Food Analysis/methods , Food Contamination/analysis , Foodborne Diseases/etiology , Histamine/analysis , Histamine/isolation & purification , Animals , Chromatography, High Pressure Liquid/methods , Fluorescamine , Histamine/adverse effects , Humans , JapanABSTRACT
The applicability of a rapid and easy multiresidue method for determination of pesticide residues in agricultural products by using liquid chromatography/tandem mass spectrometry (LC/MS/MS) was examined. Pesticide residues were extracted with acetonitrile in a disposable tube using a homogenizer, followed by salting out with anhydrous magnesium sulfate and sodium chloride. The extract was purified with a double-layered cartridge column (graphite carbon black/primary-secondary amine silica gel). After removal of the solvent, the extract was resolved in methanol-water and analyzed with LC/MS/MS. Recovery tests of 99 pesticide residues from 7 agricultural products were performed at 20 and 100 ng/g. Throughout all of the agricultural products tested, 47 pesticides exhibited satisfactory recoveries (70-120%) and relative standard deviations (<20%) at both concentrations. The time for processing of 12 samples to test solutions was approximately 2-3 h. This method could be useful for determination of pesticide residues in agricultural products.
Subject(s)
Edible Grain/chemistry , Fruit/chemistry , Pesticide Residues/analysis , Vegetables/chemistry , Chromatography, Liquid , Computer Simulation , Indicators and Reagents , Legislation, Food , Phenyl Ethers , Propionates/chemistry , Reproducibility of Results , Tandem Mass SpectrometryABSTRACT
A simple and rapid test has been developed to quantitatively measure the migration of antimony (Sb) and germanium (Ge) from polyethylene terephthalate (PET) products. The PET product was soaked in 4% acetic acid (2 mL/cm2) for 30 min at 60 degrees C and 95 degrees C. The test solution was analyzed by ICP-MS. Recoveries of spiked Sb (0.025 microg/mL) and Ge (0.05 microg/mL) were 101% and 100%, respectively, with relative standard deviations (RSDs) of 2.3% and 1.7%. In ten successive analyses, Sb and Ge in the 4% acetic acid solution were analyzed with RSDs of 1.7% and 2.2%. Sb and Ge were not subject to interference from other elements simultaneously present in the 4% acetic acid solution. This method is simple, rapid and safe, requiring no pretreatment or use of the hazardous solvent carbon tetrachloride. Therefore, this test is a useful method to analyze Sb and Ge migration from PET products.
