LC-MS/MSによる鶏組織および鶏卵中アマンタジンの分析法

摘要

抗インフルエンザ薬であるアマンタジンのLC-MS/MSによる確認•定量法を開発した。鶏筋肉，鶏肝臓，鶏砂肝および鶏卵からァセトニトリル-マキルベン緩衝液(pH3.0) 7:3混液で抽出し，Oasis~® MCXにて精製後，LC-MS/MS で測定を行った。精製カラムとして逆相—強陽イオン交換ミックスモードカラム，HPLCカラムとしてHILICカラムを用いることで，4種類の試料いずれにおいても絶対検量線での定量が可能となつた。妥当性評価ガイドラインに従い，添加回収実験を行った結果，4種類の試料について真度79.3～91.7%，併行精度3.3%以下，室内精度8.4%以下の良好な結果が得られた。定量下限値は，鶏筋肉，鶏卵および鶏砂肝では1ng/g，鶏肝臓では10 ng/gとした。%An accurate and selective analytical method for amantadine, which is used as antiviral drug to treat influenza A virus infection, was developed using LC-MS/MS. Residual amantadine was extracted from 4 kinds of food sample (poultry muscle, liver, gizzard and egg) with acetonitrile-pH 3.0 Mcllvaine buffer (7:3)， then cleaned up with an Oasis~® MCX mini-cartridge. An external standard calibration curve was used for quantification, after sample purification by the combination of a reverse-phase strong cation exchange mixed mode cartridge for cleanup and a HILIC column for HPLC. The method was validated by performing recovery tests in accordance with Japanese guidelines for the validation of analytical methods for residual agricultural chemicals in food. Recovery ranged from 79.3% to 91.7%, RSDs of repeatability were under 3.3%, and RSDs of within-laboratory reproducibility were under 8.4%. This new method was applied to samples of poultry and egg purehased in Tokyo, but residual amantadine was not detected at all.