A new analytical method for the simultaneous determination of seven fluoroquinolones, namely, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin, especially in dark-colored honey, has been developed. Fluoroquinolone antibiotics were extracted from samples with MacIlvaine buffer solution (pH 4.0) containing EDTA disodium salt dihydrate. The extracts were treated with both a polymeric cartridge and a metal chelate affnity column preloaded with ferric ion (Fe3+). LC separation with fluorescence detection was performed at 40°C using an Inertsil ODS-4 analytical column (150 × 4.6 mm, 3 µm). The mobile phase was composed of 20 mM/L citrate buffer solution (pH 3.1)–acetonitrile mixture (70 + 30, v/v) containing 1 mM/L sodium dodecyl sulfate. Lomefloxacin was used as an internal standard. The developed method was validated according to the criteria of European Commission Decision 2002/657/EC. Decision limits and detection capabilities were below 2.9 and 4.4 μg/kg, respectively.

An LC-MS/MS method for analysis of cereulide, an emetic toxin produced by Bacillus cereus, was developed. Cereulide was extracted from samples, fried rice, pan-fried noodles, red bean paste and baby formula, with methanol and purified using Oasis HLB cartridges. LC separation was performed on a C18 column with a mixture of formic acid solution and methanol containing ammonium formate as a mobile phase, and the mass spectrometer was operated in the positive electrospray ionization mode. Performance evaluation showed that trueness was higher than 70 and repeatability and reproducibility were within 10. The limits of quantification were lower than 1 ῌg/kg.

A validation study was performed on a multiresidue method for determination of pesticide residues in agricultural products according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. FASRAC Food Automatic Analytical Systems for Residual Agricultural Chemicals automatically performs extraction of pesticide residues from agricultural products with acetonitrile, filtration, constant volume, mixing with the use of air, mixing acetonitrile with buffer solvent, separation, and dehydration with sodium sulfate. The extract was purified with a GC/NH 2 column. For wheat flour and soybeans, a purification step with a C18 column was added before a GC/NH 2 column. After removal of the solvent, the extract was resolved in n-hexane/ acetone solvent for GC-MS/MS analysis. In the case of manual analysis, pesticide residues were analyzed according to official multiresidue methods and purification steps were the same as in FASRAC. Recovery tests were performed with wheat flour, soybeans, spinach and apples, by addition of 302 pesticides at the concentrations 0.01 mg/kg. The results indicate that automatic extraction using FASRAC is superior to manual analysis in trueness, repeatability and within-run reproducibility. Specially, automatic extraction using FASRAC is superior to manual analysis in trueness because it is optimized in various respects, for example reextraction at salting-out.

New automatic pretreatment equipment FASVED; Food Automatic Analytical Systems for Veterinary Drugs was developed. FASVED consists of ten main units: reagent dispenser, homogenizer, transfer hand, lid opening/closing device, centrifugal separator, pipette, shaker, column purification device, centrifugal evaporator and cooling device, and it is capable of freely combining operations by these units. A validation study was performed on two methods for determination of 178 veterinary drugs in livestock products, swine muscle, egg and shrimp, according to the method validation guideline of the Ministry of Health, Labour and Welfare of Japan. The numbers of analytes that satisfied the criteria of the guideline were 148 in swine muscle, 160 in egg and 151 in shrimp.