Department of Analytical Chemistry, Almeria University, Almeria, Spain.
J Chromatogr A. 2011 Jul 15;1218(28):4349-56. doi: 10.1016/j.chroma.2011.05.005. Epub 2011 May 13.
A reliable and rapid method has been developed for the determination of 10 mycotoxins (beauvericin, enniatin A, A1, B1, citrinin, aflatoxin B1, B2, G1, G2 and ochratoxin A) in eggs at trace levels. Ultra-high-pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS) has been used for the analysis of these compounds in less than 7 min. Mycotoxins have been extracted from egg samples using a QuEChERS-based extraction procedure (Quick, Easy, Cheap, Effective, Rugged and Safe) without applying any further clean-up step. Extraction, chromatographic and detection conditions were optimised in order to increase sample throughput and sensitivity. Matrix-matched calibration was used for quantification. Blank samples were fortified at 10, 25, 50 and 100 μg kg(-1), and recoveries ranged from 70% to 110%, except for ochratoxin A and aflatoxin G1 at 10 μg kg(-1), and aflatoxin G2 at 50 μg kg(-1). Relative standard deviations were lower than 25% in all the cases. Limits of detection ranged from 0.5 μg kg(-1) (for aflatoxins B1, B2 and G1) to 5 μg kg(-1) (for enniatin A, citrinin and ochratoxin A) and limits of quantification ranged from 1 μg kg(-1) (for aflatoxins B1, B2 and G1) to 10 μg kg(-1) (for enniatin A, citrinin and ochratoxin A). Seven samples were analyzed and aflatoxins B1, B2, G1, G2, and beauvericin were detected at trace levels.
已开发出一种可靠且快速的方法,可用于测定痕量水平下鸡蛋中的 10 种霉菌毒素(伏马菌素、恩镰孢菌素 A1、A、B1、B1、桔青霉素、黄曲霉毒素 B1、B2、G1、G2 和赭曲霉毒素 A)。超高效液相色谱-串联质谱法(UHPLC-MS/MS)用于在不到 7 分钟的时间内分析这些化合物。使用基于 QuEChERS 的提取程序(快速、简便、廉价、有效、坚固和安全)从鸡蛋样品中提取霉菌毒素,无需进一步的净化步骤。优化了提取、色谱和检测条件,以提高样品通量和灵敏度。使用基质匹配校准进行定量。空白样品在 10、25、50 和 100μg/kg 时进行了加标,回收率在 70%至 110%之间,除了 10μg/kg 时的赭曲霉毒素 A 和黄曲霉毒素 G1,以及 50μg/kg 时的黄曲霉毒素 G2。在所有情况下,相对标准偏差均低于 25%。检测限范围为 0.5μg/kg(黄曲霉毒素 B1、B2 和 G1)至 5μg/kg(恩镰孢菌素 A、桔青霉素和赭曲霉毒素 A),定量限范围为 1μg/kg(黄曲霉毒素 B1、B2 和 G1)至 10μg/kg(恩镰孢菌素 A、桔青霉素和赭曲霉毒素 A)。分析了 7 个样品,痕量水平检测到黄曲霉毒素 B1、B2、G1、G2 和伏马菌素。