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Rapid analysis of aflatoxin M1 in milk using dispersive liquid-liquid microextraction coupled with ultrahigh pressure liquid chromatography tandem mass spectrometry.
- Source :
-
Analytical and bioanalytical chemistry [Anal Bioanal Chem] 2013 Oct; Vol. 405 (26), pp. 8645-52. Date of Electronic Publication: 2013 Aug 13. - Publication Year :
- 2013
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Abstract
- A simple, rapid, and sensitive method based on simultaneous protein precipitation and extraction of aflatoxin M1 (AFM1) 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 AFM1 in milk samples. In order to precipitate the proteins and extract AFM1 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 AFM1, 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 AFM1 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 AFM1 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 AFM1 in milk and formula milk using a simple and inexpensive sample preparation procedure.
- Subjects :
- Animals
Aspergillus chemistry
Chromatography, High Pressure Liquid economics
Chromatography, High Pressure Liquid methods
Humans
Infant Formula chemistry
Infant, Newborn
Limit of Detection
Liquid Phase Microextraction economics
Tandem Mass Spectrometry economics
Aflatoxin M1 analysis
Carcinogens analysis
Liquid Phase Microextraction methods
Milk chemistry
Milk microbiology
Tandem Mass Spectrometry methods
Subjects
Details
- Language :
- English
- ISSN :
- 1618-2650
- Volume :
- 405
- Issue :
- 26
- Database :
- MEDLINE
- Journal :
- Analytical and bioanalytical chemistry
- Publication Type :
- Academic Journal
- Accession number :
- 23942569
- Full Text :
- https://doi.org/10.1007/s00216-013-7277-3