College of Material Chemistry and Chemical Engineering, Hangzhou Normal University, Hangzhou, 310036, China.
College of Pharmaceutical Science, Zhejiang University of Technology, Hangzhou, 310014, China.
J Chromatogr A. 2018 Aug 3;1561:1-12. doi: 10.1016/j.chroma.2018.05.031. Epub 2018 May 26.
Mycotoxins are a group of secondary fungi metabolites present in foods that cause adverse effects in humans and animals. The objective of this study was to develop and validate a reliable and sensitive method to determine the presence of fumonisin B1, aflatoxin B1, ochratoxin B, T-2 toxin, ochratoxin A and zearalenone. A rapid, effective process, which involves microwave-assisted dispersive micro-solid phase extraction (MA-d-μ-SPE), has been proposed for the extraction and detection of 6 mycotoxins in peach seed, milk powder, corn flour and beer sample matrixes, for subsequent analysis by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF/MS). Several experimental parameters (type of dispersant, concentration of dispersant, vortex time, type of desorption solvent and pH) affecting the extraction efficiency were systematically studied and optimized. The optimum extraction conditions involved immersing 2.5 μg/mL of nano zirconia (as dispersant) in a 5 mL sample solution. After 2 min of extraction by vigorous shaking, the target analytes were desorbed by 100 μL of chloroform at pH 4.5. The results indicated good linearity in the range of 0.0074-3.6 μg/mL (r ≥ 0.9982), low limits of detection (0.0036-0.033 μg/kg for solid samples and 0.0022-0.017 ng/mL for beer), acceptable reproducibility (relative standard deviation (RSD%) 2.08-2.76% for retention time and 3.51-4.59% for peak area, n = 3), and satisfactory spiked recoveries (84.27-104.96%) for studied mycotoxins in sample matrixes, which demonstrated that MA-d-μ-SPE coupled with UHPLC-Q-TOF/MS is a useful tool for analysis of multi-mycotoxin.
真菌毒素是存在于食品中的一组次级真菌代谢物，会对人类和动物造成不良影响。本研究旨在开发和验证一种可靠、灵敏的方法来检测玉米赤霉烯酮、黄曲霉毒素 B1、伏马菌素 B1、呕吐毒素 B、赭曲霉毒素 A 和展青霉素的存在。本研究提出了一种快速有效的微波辅助分散微固相萃取（MA-d-μ-SPE）方法，用于桃核、奶粉、玉米粉和啤酒样品基质中 6 种真菌毒素的提取和检测，然后采用超高效液相色谱-四极杆飞行时间串联质谱（UHPLC-Q-TOF/MS）进行分析。系统研究并优化了影响萃取效率的多个实验参数（分散剂的类型、分散剂的浓度、涡旋时间、解吸溶剂的类型和 pH 值）。最佳萃取条件为在 5 mL 样品溶液中加入 2.5 μg/mL 的纳米氧化锆（作为分散剂），剧烈摇动 2 min 后，在 pH 4.5 下用 100 μL 氯仿解吸目标分析物。结果表明，该方法在 0.0074-3.6 μg/mL 范围内具有良好的线性关系（r≥0.9982），低检测限（固体样品为 0.0036-0.033 μg/kg，啤酒为 0.0022-0.017 ng/mL），可接受的重现性（保留时间的相对标准偏差（RSD%）为 2.08-2.76%，峰面积的 RSD%为 3.51-4.59%，n=3），以及在所研究的基质中对多种真菌毒素的满意加标回收率（84.27-104.96%），表明 MA-d-μ-SPE 与 UHPLC-Q-TOF/MS 联用是一种分析多真菌毒素的有用工具。
