Mass Spectral Investigations on Toxins. 2. Simultaneous Detection and Quantification of Ultra-Trace Levels of Simple Trichothecenes in Environmental and Fermentation Samples by Gas Chromatographic/Negative Ion Chemical Ionization-Mass Spectrometric Techniques

Abstract

A fast, sensitive, and accurate gas chromatographic/mass spectrometric (GC/MS) method for simultaneously detecting and quantifying several simple trichothecene mycotoxins and related molecules has been developed. The method converts the polar trichothecenes into their volatile, stable heptafluorobutyrl (HFB) esters and follows the conversion with a GC/MS analysis of the derivatives. The derivatives were ionized under chemical ionization conditions, and the negative ions formed during the ionization were monitored. The samples were screened for trichothecene presence by the selected ion monitoring (SIM) mode, and the detected compounds were confirmed either by SIM or total ion monitoring. Two semisynthetic trichothecenes (deoxyverrucarol and 16-hydroxyverrucarol) were investigated and found adequate as internal standards for detecting and quantifying these toxic compounds. Femtograms and low picogram quantities (1-5 pg) of these compounds could be detected and confirmed, respectively, by this procedure. A short cleanup procedure using silica-gel SEP-PAK cartridges was developed and used for the accurate analysis of real-world samples. Several spike and a few real-world samples were analyzed by this method with excellent sensitivity and precision. Keywords: Toxins, Trichothecenes, Mycotoxins, Derivatrization, Negative ion, Chemical ionization, Gas chromatography, Mass spectrometry.

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Document Details

Document Type
Technical Report
Publication Date
Jan 01, 1987
Accession Number
ADA178051

Entities

People

  • Emory W. Sarver
  • Michael B. Wasserman
  • Thaiya Krishnamurthy

Tags

DTIC Thesaurus Topics

  • Abstracts
  • Chemical Reactions
  • Chemical Weapons
  • Chemistry
  • Chlorides
  • Classification
  • Fungi
  • Gas Chromatography
  • Ionization
  • Mass Spectra
  • Mass Spectrometry
  • Measurement
  • Molecules
  • Monitoring
  • Optical Materials
  • Regression Analysis
  • Spectrometry

Fields of Study

  • Chemistry

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  • Analytical Chemistry
  • Environmental Engineering