1. Development of isotope dilution-liquid chromatography/tandem mass spectrometry for the accurate determination of type-A trichothecenes in grains
- Author
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Byungjoo Kim, Mohamed A. Gab-Allah, and Kihwan Choi
- Subjects
Analyte ,Isotope dilution ,Mass spectrometry ,01 natural sciences ,Zea mays ,Trichothecenes, Type A ,Analytical Chemistry ,Matrix (chemical analysis) ,chemistry.chemical_compound ,0404 agricultural biotechnology ,Liquid chromatography–mass spectrometry ,Limit of Detection ,Tandem Mass Spectrometry ,Sample preparation ,Acetonitrile ,Chromatography, High Pressure Liquid ,Triticum ,Carbon Isotopes ,Chromatography ,Chemistry ,010401 analytical chemistry ,Extraction (chemistry) ,Solid Phase Extraction ,Reproducibility of Results ,04 agricultural and veterinary sciences ,General Medicine ,Mycotoxins ,040401 food science ,0104 chemical sciences ,Isotope Labeling ,Edible Grain ,Food Science - Abstract
We report the development of a highly accurate method based on isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) for the simultaneous determination of four major type-A trichothecenes in cereal grains. Uniformly labeled [13C] analogues of the target analytes were used as internal standards. An expedient sample preparation procedure was established. After extraction with acetonitrile/water (84:16; v/v), further clean-up was performed using MycoSep 227 solid-phase extraction cartridges. Unlike the commonly used immunoaffinity columns having strong selectivity for only certain target analytes, the cartridges allowed the simultaneous recovery of all four mycotoxins and efficient elimination of co-extracted matrix interferences. The ID-LC-MS/MS method exhibited very good analytical performance in the concentration range of 10–200 µg/kg; accuracy ranged from 97 to 103% with intra-day and inter-day relative standard deviations of less than 5% and 4%, respectively. Measurement uncertainties were generally below 5%. The applicability of the method was assessed by measuring the target mycotoxins in several samples at sub‐µg/kg levels.
- Published
- 2020