单端孢霉烯族霉菌毒素的质谱研究。II. 气相色谱/负离子化学电离质谱法检测和定量大环单端孢霉烯族毒素

Mass spectral investigations on trichothecene mycotoxins. II. Detection and quantitation of macrocyclic trichothecenes by gas chromatography/negative ion chemical ionization mass spectrometry.

作者信息

Krishnamurthy T, Sarver E W, Greene S L, Jarvis B B

出版信息

J Assoc Off Anal Chem. 1987 Jan-Feb;70(1):132-40.

Abstract

A general, sensitive gas chromatographic/negative ion chemical ionization mass spectrometric (GC/NICIMS) method of analysis was developed for the detection and quantitation of several polar, thermally labile, toxic macrocyclic trichothecenes. The procedure involves the conversion of the molecules to their corresponding alcohols (verrucarols) by alkaline hydrolysis, followed by derivatization of the hydrolysate with heptafluorobutyrylimidazole and analysis by GC/MS technique under negative ion chemical ionization conditions. Nanogram (250 ng) quantities of several macrocyclic trichothecenes with different verrucarol and ester moieties were analyzed successfully with good precision by this procedure. The method was applicable for the accurate determination of at least low ppb levels of these macrocyclic trichothecenes in environmental samples, such as fungal products, fermentation broths, and plant samples. This is the first reported, well developed, sensitive, and applicable method for the detection and quantitation of these compounds in naturally occurring samples.

摘要

开发了一种通用、灵敏的气相色谱/负离子化学电离质谱（GC/NICIMS）分析方法，用于检测和定量几种极性、热不稳定、有毒的大环单端孢霉烯族毒素。该程序包括通过碱性水解将分子转化为其相应的醇（疣孢菌素醇），然后用七氟丁酰咪唑对水解产物进行衍生化，并在负离子化学电离条件下通过GC/MS技术进行分析。通过该程序成功地分析了纳克（250纳克）数量的几种具有不同疣孢菌素醇和酯部分的大环单端孢霉烯族毒素，精密度良好。该方法适用于准确测定环境样品（如真菌产物、发酵液和植物样品）中至少低ppb水平的这些大环单端孢霉烯族毒素。这是首次报道的用于检测和定量天然样品中这些化合物的完善、灵敏且适用的方法。