A Quantification and Confirmation Method of Patulin in Apple Juice by GC/MS

摘要

GC／MSを用いてリンゴ果汁中のパノリンを1および5mug／kg（日本の基準値の1／10）ま、そ正確にそれぞれ測ラ己確認できる分析法を確立した．試料中のパノリンを酢酸エチルで抽出し，濃縮後の抽出液にヘキサンを加えて混合し，生成した不溶物をろ過で除去後，固相抽出によりさらに精製した．この低極性状態でのろ過は，妨害物質の除去に非業に有効であった．カラムからの溶出液を減圧乾圏，BSTFAによりトリメチルンリル化後，GC／MSで測定した．定量はSIMモード（m／z：226），確認はSCANモードでマススペクトルを比較することにより行った辚螗垂椁位貐胜希?10～500mug／kg添加で93．4～100％であり，検出，定量および確認限界は，それぞれ0．11および5mug／kgであった．%A sensitive and selective method for quantification and confirmation of patulin in apple juice by GC/MS was developed. By this method, patulin was precisely determined and confirmed down to the level of 1 and 5 mug/kg in samples, respectively Patulinwas extracted with ethyl acetate from a sample and then hexane was added to the concentrated extract solution Significant amounts of insoluble impurities were filtered off, followed by further clean-up by solid-phase extraction with combined silica gel and Florisil cartridges. The filtration step in a low-polarity condition was very effective to remove the impurities in the sample extract solution. The eluate from the cartridges was evaporated to dryness under reduced pressure and patulin was determinedand confirmed by GC/MS after derivatization with 25% TVO-bisftrimethylsilyl) trifluoroacetarnide ethyl acetate solution. Patulin was determined in the selected ion monitoring mode (m/z 226} and confirmed in the SCAN mode (m/z 40-340) The recovery from apple juice spiked with 10-500 mug/kg ranged from 93 4 to 100% The limits of detection and quantification were 0.1 (S/N= 3) and 1 mug/kg (S/N= 30) of patulin in samples, respectively Levels down to 5 mug/ kg of patulin in sample were readily confirmed.