Journal
ANALYTICAL AND BIOANALYTICAL CHEMISTRY
Volume 405, Issue 26, Pages 8645-8652Publisher
SPRINGER HEIDELBERG
DOI: 10.1007/s00216-013-7277-3
Keywords
Milk; Aflatoxin M-1; Protein precipitation; Dispersive liquid-liquid microextraction; UHPLC-MS/MS
Funding
- Italian Ministry of the University and Research (MIUR) with a FIRB Futuro in Ricerca [RBFR10GSJK]
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A simple, rapid, and sensitive method based on simultaneous protein precipitation and extraction of aflatoxin M-1 (AFM(1)) followed by dispersive liquid-liquid microextraction (DLLME) and ultrahigh pressure liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) analysis was developed for the determination of AFM(1) in milk samples. In order to precipitate the proteins and extract AFM(1) from milk, a sample pretreatment using acetonitrile and NaCl as the extraction/denaturant solvent and salting-out agent, respectively, was optimised. Subsequently, the acetonitrile (upper) phase, containing AFM(1), was used as the disperser solvent in DLLME, and extractant (chloroform) and water were added in turn to the extract to perform the DLLME process. The main parameters affecting the extraction efficiency of the whole analytical procedure, such as acetonitrile volume, amount of salt, type and volume of extractant and water volume, were carefully optimised by experimental design. Under optimum conditions, the developed method provides an enrichment factor of 33 and detection and quantification limits (0.6 and 2.0 ng kg(-1), respectively) below the maximum levels imposed by current regulations for AFM(1) in milk and infant milk formulae. Recoveries (61.3-75.3 %) and repeatability (RSD < 10, n = 3), tested in different types of milk at four AFM(1) levels, met the performance criteria required by EC Regulation No. 401/2006. Moreover, the matrix effect on the signal intensity of the analyte was negligible. The proposed method provides a rapid extraction and an accurate determination of AFM(1) in milk and formula milk using a simple and inexpensive sample preparation procedure.
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