Tang Zhentao, Han Qingrong, Yu Gang, Liu Fei, Tan Yuzhu, Peng Cheng
Key Laboratory of Southwestern Chinese Medicine Resources Innovative Institute of Chinese Medicine and Pharmacy Chengdu University of Traditional Chinese Medicine Chengdu China.
Key Laboratory of Southwestern Chinese Medicine Resources School of Pharmacy Chengdu University of Traditional Chinese Medicine Chengdu China.
Food Sci Nutr. 2022 Mar 21;10(7):2224-2235. doi: 10.1002/fsn3.2832. eCollection 2022 Jul.
Magnetic solid-phase extraction (MSPE) strategy based on the FeO@PDA/MIL-101(Cr) has been proposed to separate and purify five common mycotoxins in licorice, including aflatoxin B, aflatoxin G, sterigmatocystin, zearalenone, and ochratoxin A. Integrating the MSPE and solid-liquid extraction/partitioning, a modified QuEChERS was established to adapt to the complex licorice samples. The FeO@PDA/MIL-101(Cr) was successfully synthesized and characterized by Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and nitrogen adsorption-desorption isotherms. Sorbents with superior advantages for exclusion of matrix interference and extraction of target analytes in a short time were obtained, according to their ability of magnetic separation, high surface area (287.75 m/g), large pore volume (0.61 cm/g), and nanosized structure with mesopores. Prior to analysis with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS), several key parameters that would affect the sorbents' extraction efficiency were extensively investigated. Under the optimized conditions, the practicality of the developed method for analysis of mycotoxins in licorice samples was confirmed by adequate linearity ( ≥ 0.9967), high sensitivity (LODs and LOQs, respectively, in the ranges 0.01-0.09 and 0.02-0.30 μg/kg), acceptable recovery (78.53%-116.28%), satisfactory reusability, and good interbatch precision of the sorbents (RSDs in the ranges 6.70%-11.20% and 6.02%-10.35%, respectively). The results indicated that the established method was feasible and reliable for the environment-friendly and rapid screening of mycotoxins in complex licorice samples.
基于FeO@PDA/MIL-101(Cr)的磁性固相萃取(MSPE)策略已被提出用于分离和纯化甘草中的五种常见霉菌毒素,包括黄曲霉毒素B、黄曲霉毒素G、杂色曲霉素、玉米赤霉烯酮和赭曲霉毒素A。将MSPE与固液萃取/分配相结合,建立了一种改进的QuEChERS方法以适应复杂的甘草样品。成功合成了FeO@PDA/MIL-101(Cr),并通过傅里叶变换红外光谱(FT-IR)、扫描电子显微镜(SEM)、透射电子显微镜(TEM)和氮吸附-脱附等温线对其进行了表征。根据其磁分离能力、高比表面积(287.75 m/g)、大孔体积(0.61 cm/g)和具有中孔的纳米结构,获得了在短时间内排除基质干扰和萃取目标分析物具有卓越优势的吸附剂。在用超高效液相色谱-串联质谱(UHPLC-MS/MS)分析之前,广泛研究了几个会影响吸附剂萃取效率的关键参数。在优化条件下,所建立的方法用于分析甘草样品中霉菌毒素的实用性通过足够的线性(≥0.9967)、高灵敏度(LOD和LOQ分别在0.01-0.09和0.02-0.30 μg/kg范围内)、可接受的回收率(78.53%-116.28%)、令人满意的可重复使用性以及吸附剂良好的批间精密度(RSD分别在6.70%-11.20%和6.02%-10.35%范围内)得到了证实。结果表明,所建立的方法对于复杂甘草样品中霉菌毒素的环境友好型快速筛查是可行且可靠的。