苹果汁中展青霉素的快速气相色谱/质谱测定与确证

Rapid gas chromatography/mass spectrometry determination and confirmation of patulin in apple juice.

作者信息

Marks Heidi S

机构信息

U.S. Food and Drug Administration, Pacific Regional Laboratory Northwest, Bothell, WA 98021, USA.

出版信息

J AOAC Int. 2007 May-Jun;90(3):879-83.

PMID:17580643

Abstract

A gas chromatography/mass spectrometry (GC/MS) method was developed for the quantitative determination and confirmation of patulin extracted from apple juice. Juice is alkalized and extracted with ethyl acetate-hexane, a portion concentrated under N2, then resolubilized in acetonitrile for simple derivatization with bis(trimethylsilyl)trifluoracetamide. Patulin was determined by GC/MS using an electron-impact source and selected ion monitoring of characteristic ions. Spike levels of 20-100 microg/L gave an average recovery of 86%, and 6 ions of sample and standard spectra matched within 10% absolute for confirmation. The limits of quantitation and detection were 10 and 3 microg/L, respectively.

摘要

建立了一种气相色谱/质谱（GC/MS）方法，用于定量测定和确证从苹果汁中提取的展青霉素。将果汁碱化，用乙酸乙酯 - 己烷萃取，一部分在氮气下浓缩，然后再溶解于乙腈中，用双（三甲基硅基）三氟乙酰胺进行简单衍生化。展青霉素通过GC/MS使用电子轰击源和特征离子的选择离子监测进行测定。加标水平为20 - 100μg/L时，平均回收率为86%，样品和标准光谱的6个离子在绝对误差10%以内匹配以进行确证。定量限和检测限分别为10μg/L和3μg/L。