[Development of an Analytical Method for Simultaneous Determinationof Quinolones and Tetracyclines in Livestock and Fishery Products].

In this study, we developed an analytical method for simultaneous determination of 14 quinolones and 4 tetracyclines in livestock and fishery products using LC-MS/MS. The analytes were extracted from food samples with citrate buffer (containing EDTA)-methanol-acetonitrile (3 : 1 : 1, v/v/v) in the presence of n-hexane, and the extract was purified with an Oasis PRiME HLB cartridge column. It was suggested that this analytical method can also extract analytes from solid samples containing fat by using n-hexane. In addition, using methanol-acetonitrile (3 : 7, v/v) containing 0.1 vol% formic acid as an eluent from the cartridge column, the purification effect could be improved, while minimizing the impairment of the recovery rate. As a result of the validation using six types of food samples, trueness (accuracy) was 70.6%-113.8%, the RSD of repeatability was 9.0% or less, and the RSD of within-laboratory reproducibility was 15.5% or less. Using this approach, the standard values mentioned in the Japanese guideline were successfully met.

Determination of sterigmatocystin in foods in Japan: method validation and occurrence data.

A survey of the contamination of foods by sterigmatocystin (STC) was performed by an analytical method based on LC-MS/MS. STC was extracted from samples with acetonitrile/water (85/15, v/v) and then purified with immunoaffinity columns. The method was validated by a small-scale inter-laboratory study using spiked wheat samples. Mean recoveries of STC were 100.3% and 92.5% from two samples spiked at 0.5 and 5.0 µg/kg, respectively. A total of 583 samples were analysed between 2016 and 2018, and STC was detected in 19.9% of all samples at >0.05 µg/kg (limit of quantification). The foods that were contaminated by STC were wheat flour, Job's tears products, rye flour, rice, buckwheat flour, white sorghum, barley products, azuki bean and corn flour. STC was not found in beer or wine. The occurrence of STC in domestic wheat flour (44.4%), Job's tears products (41.7%) and rye flour (29.9%) accounted for the three highest values. The highest mean concentrations were obtained for Job's tears products (0.3 µg/kg) and rye flour (0.3 µg/kg). The maximum contamination level was present in a sample of rye flour (7.1 µg/kg). Although the contamination levels were low, these results indicate that STC frequently contaminates Japanese retail foods. A continuous survey is required to assess exposure to STC in Japan.

[Analysis of metribuzin and its metabolites in livestock products and seafoods by liquid chromatography-tandem mass spectrometry].

A method for simultaneous determination of metribuzin (MET) and three metribuzin metabolites in livestock products and seafoods by liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed. MET and its metabolites were extracted from a sample with acetonitrile, followed by InertSepC18 and BondElut SAX cartridge cleanup. The LC separation was performed on a C18 column using 0.01 mol/L ammonium formate-acetonitrile-methanol (70 :21 : 9) as the mobile phase and MS detection with both positive and negative ion electrospray ionization. The mean recoveries from 10 livestock products and seafoods were generally >60%, and the relative standard deviations were <20%