Identification and quantification of cereulide in cow's milk using liquid chromatography-tandem mass spectrometry

Autor: Akihiko Hirai, Yoko Matsushima, Hiroshi Koike, Kotaro Sekimura, Chieko Nagano, Tetsuya Shindo, Maki Kanda, Hiroshi Hayashi, Yukiko Nakagawa, Takeo Sasamoto, Tsuneo Hashimoto, Yumi Ohba, Junichi Kamiie
Rok vydání: 2018
Předmět:
Zdroj: Food additivescontaminants. Part A, Chemistry, analysis, control, exposurerisk assessment. 35(12)
ISSN: 1944-0057
Popis: In this study, the presence of cereulide in cow's milk was identified and quantified using our validated method with liquid chromatography-tandem mass spectrometry. Cereulide was concentrated using protein acid-precipitation and extracted from the precipitate by using acetonitrile twice. The combination of protein acid-precipitation and extraction sufficiently eliminated the matrix compounds from the milk and a further clean-up step utilising solid-phase extraction could be omitted. For robustly measuring the samples and keeping the MS devices clean, the extraction solution was diluted 10-fold using methanol. Owing to the minimisation of the interferences caused by fragmentation patterns, multiple reaction monitoring information-dependent acquisition-enhanced product ion spectra enabled the characterisation and identification of cereulide. Besides the matrix effect (-4%), an external solvent calibration curve was adapted for accurate quantification. The method was validated using fortified recovery tests, at two concentrations (10 and 50 µg kg
Databáze: OpenAIRE
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