Food and Drug Control Department, Faculty of Pharmacy, Tabriz University of Medical Sciences, Tabriz, Iran.
Food and Drug Safety Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.
J Sep Sci. 2021 Apr;44(7):1501-1509. doi: 10.1002/jssc.202001183. Epub 2021 Feb 17.
A new extraction procedure based on combination of a solvent extraction and deep eutectic solvent based dispersive liquid-liquid microextraction has been introduced for the extraction of aflatoxin M from cheese samples. In this method, acetonitrile, deionized water, and n-hexane are added onto the sample and vortexed. Owning to different affinities of the substances in cheese toward the mentioned solvents, an efficient and selective extraction of the analyte is done in the acetonitrile phase. After centrifugation, the acetonitrile phase is removed and mixed with a new hydrophobic deep eutectic solvent prepared from N,N-diethanol ammonium chloride and carvacrol as an extraction solvent. The mixture is injected into deionized water, and a cloudy solution is obtained. Eventually, an aliquot of the organic phase is injected into high-performance liquid chromatography-fluorescence detection. After optimizing the effective parameters with the response surface methodology and a quadratic model, limits of detection and quantification were 0.74 and 2.56 ng/kg, respectively. The obtained extraction recovery and enrichment factor were 94% and 94, respectively. Also, intra- (n = 6) and interday (n = 4) precisions were less than or equal to 8.6% at a concentration of 5 ng/kg. The suggested method was applied to determine aflatoxin M in different cheese samples.
一种新的提取方法，基于溶剂萃取和深共晶溶剂分散液液微萃取的结合，已被引入用于从奶酪样品中提取黄曲霉毒素 M。在这种方法中，将乙腈、去离子水和正己烷加入到样品中并涡旋。由于奶酪中物质对所述溶剂的亲和力不同，分析物在乙腈相中得到有效和选择性的提取。离心后，去除乙腈相并与新的疏水性深共晶溶剂混合，该溶剂由 N,N-二乙醇氯化铵和香芹酚制备而成，作为萃取溶剂。将混合物注入去离子水，得到混浊溶液。最终，将有机相的一部分注入高效液相色谱-荧光检测。通过响应面法和二次模型优化有效参数后，检测限和定量限分别为 0.74 和 2.56 ng/kg。提取回收率和富集因子分别为 94%和 94。此外，在 5 ng/kg 浓度下，日内（n=6）和日间（n=4）精密度均小于或等于 8.6%。该方法已应用于不同奶酪样品中黄曲霉毒素 M 的测定。
