Ouakhssase Abdallah, Chahid Adil, Choubbane Hanane, Aitmazirt Abdelmajid, Addi Elhabib Ait
Research group: Génie des procédés et Ingénierie Chimique, Ecole Supérieure de Technologie d'Agadir, B.P: 33/S, Université Ibn Zohr, Agadir, Morocco.
Laboratoire Régional d'Analyses et de Recherche Agadir/Office National de Sécurité Sanitaire des Produits Alimentaires (LRARA/ONSSA), BP 474, Agadir, Morocco.
Heliyon. 2019 May 10;5(5):e01565. doi: 10.1016/j.heliyon.2019.e01565. eCollection 2019 May.
A LC-MS/MS method has been optimized and validated for the determination of aflatoxins (AFB1, AFB2, AFG1 and AFG2) in maize. Extraction was performed using a modified QuEChERS method with little sample preparation without the need for purification procedure. Determination was performed by high pressure liquid chromatography (HPLC) coupled to tandem mass spectrometry (MS/MS). The acquisition was performed using MassHunter software in Multiple Reaction Monitoring (MRM) mode in positive polarity. Different mobile phases were tested to control the degree of the ionization and good performances were obtained for methanol/water with 5 mM ammonium acetate. MRM experiments were optimized for each aflatoxin in order to generate sensitive transitions. Linearity was demonstrated for the aflatoxins in the range 0.225-1.25 μg/L. Limits of detection (LOD) (0.11 and 0.36 μg/Kg) and limits of quantification (LOQ) (0.36-1.19 μg/Kg) of the aflatoxins are below the maximum permitted levels set by the European Union (EU). Aflatoxins have acceptable recoveries using QuEChERS method in the acceptable range of 50-120% for levels below 1 μg/Kg. Satisfactory recoveries were also obtained in the acceptable range of 70-110% for levels between 1 and 10 μg/Kg except for AFB2. Relative standard deviation (RSD) of recoveries for the intra-day precision and inter-day precision were below 11 %. Selectivity of the method was tested and no spectral interferences were observed in the appropriate retention times. The main advantage of the proposed method is its ease of use and requires a smaller solvent consumption that reduces the time and cost of the analysis.
已优化并验证了一种液相色谱-串联质谱(LC-MS/MS)方法,用于测定玉米中的黄曲霉毒素(AFB1、AFB2、AFG1和AFG2)。采用改良的QuEChERS方法进行提取,样品制备简单,无需纯化步骤。通过高压液相色谱(HPLC)与串联质谱(MS/MS)联用进行测定。使用MassHunter软件在正离子模式下的多反应监测(MRM)模式下进行数据采集。测试了不同的流动相以控制电离程度,对于含有5 mM乙酸铵的甲醇/水体系,获得了良好的性能。针对每种黄曲霉毒素优化了MRM实验,以产生灵敏的跃迁。黄曲霉毒素在0.225 - 1.25 μg/L范围内呈线性。黄曲霉毒素的检测限(LOD)(0.11和0.36 μg/Kg)和定量限(LOQ)(0.36 - 1.19 μg/Kg)低于欧盟设定的最大允许水平。对于含量低于1 μg/Kg的黄曲霉毒素,使用QuEChERS方法的回收率在50 - 120%的可接受范围内。对于含量在1至10 μg/Kg之间的情况,除AFB2外,回收率在70 - 110%的可接受范围内也获得了满意的结果。日内精密度和日间精密度的回收率相对标准偏差(RSD)低于11%。测试了该方法的选择性,在适当的保留时间内未观察到光谱干扰。所提出方法的主要优点是易于使用,且溶剂消耗较少,减少了分析时间和成本。