simple and reliable liquid chromatography-tandem mass spectrometry method for the determination of aflatoxin M1 in milk

• Published in: Food additives & contaminants. Part A, Chemistry, analysis, control, exposure & risk assessment Vol. 30; no. 2; pp. 381 - 388
• Main Authors: Biancardi, A, Piro, R, Dall’asta, C, Galaverna, G
• Format: Journal Article
• Language: English
• Published: Abingdon Taylor & Francis Group 2013; Taylor & Francis
• Subjects: aflatoxin M; aflatoxin M1; Aflatoxin M1 - analysis; Animals; Biological and medical sciences; Chromatography, Liquid - methods; confidence interval; ethyl acetate; Food Contamination - analysis; Food industries; Food toxicology; Fundamental and applied biological sciences. Psychology; Humans; immunoaffinity chromatography; LC-MS/MS; mass spectrometry; milk; Milk - chemistry; Milk and cheese industries. Ice creams; milk, liquid-liquid extraction; sodium chloride; Spectrometry, Mass, Electrospray Ionization; Tandem Mass Spectrometry - methods; Toxin; LC-MS/MS; aflatoxin M; liquid―liquid extraction; Aflatoxin M1; Liquid liquid extraction; Mycotoxin; Dairy product; Liquid chromatography; Method; Mass spectrometry; Milk
• ISSN: 1944-0057; 1944-0049; 1944-0057
• DOI: 10.1080/19440049.2012.743041

A new chromatographic method is proposed for the analysis of aflatoxin M₁ in milk. The method is based on liquid–liquid extraction followed by LC-MS/MS analysis. Liquid–liquid extraction (LLE) is performed on the defatted milk plus sodium chloride by using ethyl acetate as an extraction solvent. Accuracy and precision were evaluated at the LOQ (15 ng kg–¹) spiked sample as well as with three other different naturally contaminated reference materials. The mean overall recovery (n = 24) was 95% with a confidence interval of 1.9% and a CV% of 4.5%. The performance of the proposed method was compared with that of the Official ISO Method based on the use of immunoaffinity chromatography columns (IAC): LLE protocol could be considered a valid alternative to the LC-IAC. In general it showed better accuracy with lower data dispersion. Moreover, the sample preparation is very simple and straightforward, potentially being applicable as a high-throughput method which, on account of its simplicity and low cost, may be applied to the analysis of a large number of samples in the occasion of outbreaks of large-scale contamination.