[Study of Rapid Simultaneous Determination of 6 Fungicides in Lemon Using Three-Layer Extraction].

A rapid, easy and versatile, simultaneous analytical method based on three-layer extraction was developed for the determination of 6 fungicides in lemon. In this method, degreasing with n-hexane, partitioning into acetonitrile, and purification by the salting-out effect were simultaneously performed after extraction with acetone. It allowed to prepare a test solution without concentrating, transferring, and purification using solid phase extraction column.As a result, 6 fungicides in lemon met the management criteria of the guideline for validity assessment (Ministry of Health, Labour and Welfare in Japan). Thus, the present method could be useful for a rapid determination of fungicides in lemon.

[Usefulness of Dilution for Rapid Simultaneous Determination of Residual Pesticides in Edamame (Immature Soybeans) by LC-MS/MS].

A rapid, easy and versatile, simultaneous analytical method by LC-MS/MS based on extraction of QuEChERS method (EN 15662:2008) was developed for the determination of residual pesticides in Edamame (immature soybeans). In this method, it allowed to prepare a test solution only dilution without purification using solid column. As a result, 202 analytes met the management criteria of the guideline for validity assessment (Ministry of Health, Labour and Welfare of Japan). Thus, the present method could be useful for a rapid simultaneous determination of residual pesticides in green soybean.

[Rapid Determination of tert-Butylhydroquinone (TBHQ) in Foods Using Three-Layer Extraction].

A rapid, easy and versatile analytical method based on three-layer extraction was developed for the determination of tert-butylhydroquinone (TBHQ) in foods. In this method, degreasing with n-hexane, partitioning into acetonitrile, and purification by the salting-out were simultaneously performed after extraction with acetone. It allowed to prepare a test solution without concentrating, transferring, and purification using solid phase extraction column. As a result, TBHQ for a wide variety of 11 foods met the management criteria of the guideline for validity assessment (Ministry of Health, Labour and Welfare of Japan). Thus, the present method could be useful for a rapid determination of TBHQ in foods.

[Usefulness of Dilution for Rapid Simultaneous Determination of Residual Pesticides in Agricultural Products by LC-MS/MS].

A rapid, easy and versatile, simultaneous analytical method by LC-MS/MS based on extraction of QuEChERS method (EN 15662:2008) was developed for the determination of residual pesticides in agricultural products. In this method, it allowed to prepare a test solution only dilution without purification using solid phase extraction column. The method was assessed for 210 pesticide residues in 21 kinds of vegetables and fruits at the fortification levels of 0.01 and 0.1 µg/g according to the method validation guideline (Ministry of Health, Labour and Welfare of Japan). As a result, 194 to 210 analytes met the management criteria of the guideline. Thus, the present method could be useful for a rapid simultaneous determination of residual pesticides in agricultural products.

[Study of Rapid Simultaneous Determination of Residual Veterinary Drugs in Livestock and Fishery Products Using Three-Layer Extraction].

A rapid, easy, versatile, simultaneous analytical method based on three-layer extraction and LC-MS/MS was developed for the determination of residual veterinary drugs in livestock and fishery products. In this method, degreasing with n-hexane, partitioning into acetonitrile, and purification by the salting-out effect were simultaneously performed after extraction with acetone aq. It allowed to prepare a test solution without concentrating, transferring, and purification using solid column. Recoveries of quinolones were improved by adjusting acid concentration and adding EDTA-2Na・2H2O. As a result, 62 analytes for cattle muscle, 63 analytes for cattle fat, 62 analytes for eel, and 65 analytes for salmon met the management criteria of the guideline for validity assessment (Ministry of Health, Labour and Welfare in Japan). Thus, the present method could be useful for a rapid determination of residual veterinary drugs in livestock and fishery products.

[Validation Study of Rapid Analytical Method for Determination of Cyclamate in Various Kinds of Foods by LC-MS/MS].

A rapid, sensitive and selective analytical method by LC-MS/MS was developed and validated for the determination of cyclamate in various kinds of foods. The Preparation of test solutions was performed by heat extraction technique in accordance with an official notification method in Japan. We aimed to reduce the matrix effects in LC-MS/MS only by diluting extracts without clean-up using solid phase column. This method was assessed for 30 kinds of foods fortifying cyclamate at the concentration level of 0.5 µg/g. As a result, trueness was 85.0 to 106.6%, repeatability (RSDr) ranged from 1.7 to 9.4%, and within-laboratory reproducibility (RSDwr) ranged from was 4.1 to 9.7%. These date supported the reliability our method. Thus, this method could be useful for a rapid determination of cyclamate in various kinds of foods.