Analytical method for the accurate determination of tricothecenes in grains using LC-MS/MS: a comparison between MRM transition and MS3 quantitation

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• 作者：Chee Wei Lim (1) Jeff_Lim@hsa.gov.sg
  Siew Hoon Tai (2)
  Lin Min Lee (1)
  Sheot Harn Chan (1)
• 关键词：LC ; MS/MS – ; Grains – ; MRM transition – ; MS/MS/MS (MS3) – ; Quantitation – ; Tricothecenes
• 刊名：Analytical and Bioanalytical Chemistry
• 出版年：2012
• 出版时间：July 2012
• 年：2012
• 卷：403
• 期：10
• 页码：2801-2806
• 全文大小：130.2 KB
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• 作者单位：1. Food Safety Laboratory, Applied Sciences Group, Health Sciences Authority, 11 Outram Road, Singapore, 169078 Singapore2. AB SCIEX (Distribution), 10 Biopolis Road, #03-06, Chromos, Singapore, 138670 Singapore
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Analytical Chemistry
  Food Science
  Inorganic Chemistry
  Physical Chemistry
  Monitoring, Environmental Analysis and Environmental Ecotoxicology
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1618-2650

文摘

The current food crisis demands unambiguous determination of mycotoxin contamination in staple foods to achieve safer food for consumption. This paper describes the first accurate LC-MS/MS method developed to analyze tricothecenes in grains by applying multiple reaction monitoring (MRM) transition and MS3 quantitation strategies in tandem. The tricothecenes are nivalenol, deoxynivalenol, deoxynivalenol-3-glucoside, fusarenon X, 3-acetyl-deoxynivalenol, 15-acetyldeoxynivalenol, diacetoxyscirpenol, and HT-2 and T-2 toxins. Acetic acid and ammonium acetate were used to convert the analytes into their respective acetate adducts and ammonium adducts under negative and positive MS polarity conditions, respectively. The mycotoxins were separated by reversed-phase LC in a 13.5-min run, ionized using electrospray ionization, and detected by tandem mass spectrometry. Analyte-specific mass-to-charge (m/z) ratios were used to perform quantitation under MRM transition and MS3 (linear ion trap) modes. Three experiments were made for each quantitation mode and matrix in batches over 6 days for recovery studies. The matrix effect was investigated at concentration levels of 20, 40, 80, 120, 160, and 200 μg kg−1 (n = 3) in 5 g corn flour and rice flour. Extraction with acetonitrile provided a good overall recovery range of 90–108% (n = 3) at three levels of spiking concentration of 40, 80, and 120 μg kg−1. A quantitation limit of 2–6 μg kg−1 was achieved by applying an MRM transition quantitation strategy. Under MS3 mode, a quantitation limit of 4–10 μg kg−1 was achieved. Relative standard deviations of 2–10% and 2–11% were reported for MRM transition and MS3 quantitation, respectively. The successful utilization of MS3 enabled accurate analyte fragmentation pattern matching and its quantitation, leading to the development of analytical methods in fields that demand both analyte specificity and fragmentation fingerprint-matching capabilities that are unavailable under MRM transition.