Identification and quantification of cereulide in cow's milk using liquid chromatography-tandem mass spectrometry.
Food Addit Contam Part A Chem Anal Control Expo Risk Assess
; 35(12): 2424-2433, 2018 Dec.
Article
en En
| MEDLINE
| ID: mdl-30475679
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-1), using three samples daily on five different days based on the Japanese guidelines. This new method exhibited good accuracy ranging from 91% to 94%. The relative standard deviations of repeatability ranged from 2% to 5%, and the relative standard deviation of within-laboratory reproducibility ranged from 5% to 6%. These standard deviations satisfied the criteria for the Japanese validation guidelines. The limit of quantification (LOQ) was estimated to be 2 µg kg-1. On the product ion spectra at the LOQ level, the library match was satisfactory with a purity fit value of >70%. The method was applied to 14 raw milk and three milk samples pasteurised using the low-temperature, long-time process and collected in Tokyo. None of the samples was found to contain the target toxin.
Palabras clave
Texto completo:
1
Colección:
01-internacional
Base de datos:
MEDLINE
Asunto principal:
Contaminación de Alimentos
/
Leche
/
Depsipéptidos
Tipo de estudio:
Diagnostic_studies
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Prognostic_studies
Límite:
Animals
Idioma:
En
Revista:
Food Addit Contam Part A Chem Anal Control Expo Risk Assess
Asunto de la revista:
CIENCIAS DA NUTRICAO
Año:
2018
Tipo del documento:
Article
País de afiliación:
Japón
Pais de publicación:
Reino Unido