Determination of Aflatoxin M1 in Milk Powder by Ultrasonic-Assisted Extraction and Dispersive Solid-Phase Clean-up

• Published in: Journal of chromatographic science 2015-07, Vol.53 (6), p.1000-1006
• Main Authors: Manoochehri, Mahboobeh, Asgharinezhad, Ali Akbar, Safaei, Mahdi
• Format: Article
• Language: English
• Subjects: Acetonitrile; Aflatoxin M1; Aflatoxin M1 - analysis; Animals; Chromatography, High Pressure Liquid; Cleaning; Extraction; Leaching; Limit of Detection; Linear Models; Milk; Milk - chemistry; Models, Statistical; Optimization; Reproducibility of Results; Solid Phase Extraction - methods; Solvents; Sonication
• ISSN: 0021-9665; 1945-239X
• DOI: 10.1093/chromsci/bmu131

This work describes the application of ultrasound-assisted dispersive solid-phase extraction (UA-DSPE) as a sample preparation approach for aflatoxin M1 (AFM1) and also its subsequent determination by HPLC–fluorescence detection. A Box–Behnken design in combination with response surface methodology was implemented to determine the variables affecting the extraction procedure. The effects of different variables, including type and quantity of clean-up phase, ultrasonication time, ultrasonication temperature, nature and volume of the leaching solvent, were investigated in the optimization study. Primary secondary amine (PSA) and acetonitrile were selected as the clean-up phase and the leaching solvent, respectively. The obtained optimized values were 30 mg of PSA, 10 min ultrasonication time, 32°C ultrasonication temperature and 10 mL of acetonitrile. Under the optimal conditions, the limit of detection and limit of quantification were 0.0012 and 0.0045 µg kg−1, respectively. The recoveries of the UA-DSPE procedure ranged from 80 to 92%, with relative standard deviations lower than 10% in all cases. Eventually, this method was successfully applied to the extraction of AFM1 in milk powder samples.