Institute of Laser Chemistry, Department of Chemistry, Fudan University, Shanghai 200433, China.
Institute of Biomedical and Pharmaceutical Technology, Fuzhou University, Fuzhou 350002, China.
Talanta. 2018 Feb 1;178:1-8. doi: 10.1016/j.talanta.2017.08.030. Epub 2017 Aug 24.
A poly (methacrylic acid-co-divinyl-benzene) [poly (MAA-co-DVB)] monolithic column was specially prepared according to the chemical structures of the three mycotoxins of aflatoxin B1, zearalenone and sterigmatocystin, and used for in-tube solid-phase microextraction (in-tube SPME) of the selected mycotoxins. The poly (MAA-co-DVB) monolithic column was characterized in detail, and exhibited effective hydrophobic, π-π, and hydrogen bonding interactions towards the target analytes. By coupling the poly (MAA-co-DVB) monolithic column-based in-tube SPME with high-performance liquid chromatography, a simple, sensitive and matrix effect-free method for determination of mycotoxins was developed. Some important parameters related to extraction efficiency were optimized systematically. Under the optimal conditions, the enrichment factors for the three mycotoxins ranged from 71.9 to 98.7. Recoveries of mycotoxins in rice grains with three spiked concentration levels were in the range of 78.0-102.8%, with satisfactory relative standard deviations (n = 4) of 2.96-4.74%. Good linearity was obtained with correlation coefficients larger than 0.99, and the detection limits (S/N = 3) of the three mycotoxins were between 0.69 and 2.03μgkg. The developed poly (MAA-co-DVB) monolithic column based in-tube SPME-HPLC method was successfully used to sensitively determine trace mycotoxins in practical samples of rice grain without interference peaks, indicating that it is promising for the detection of trace mycotoxins in complex grain samples.
一种聚（甲基丙烯酸-co-二乙烯基苯）[聚（MAA-co-DVB）]整体柱是根据黄曲霉毒素 B1、玉米赤霉烯酮和桔青霉素这三种真菌毒素的化学结构专门制备的，并用于所选真菌毒素的管内固相微萃取（in-tube SPME）。详细表征了聚（MAA-co-DVB）整体柱，其对目标分析物表现出有效的疏水性、π-π 和氢键相互作用。通过将聚（MAA-co-DVB）整体柱基管内 SPME 与高效液相色谱法相结合，开发了一种简单、灵敏且无基质效应的真菌毒素测定方法。系统优化了与萃取效率相关的一些重要参数。在最佳条件下，三种真菌毒素的富集因子范围为 71.9-98.7。在三种加标浓度水平的稻谷中的真菌毒素回收率在 78.0-102.8%之间，相对标准偏差（n=4）为 2.96-4.74%，令人满意。具有大于 0.99 的相关系数，三种真菌毒素的检测限（S/N=3）在 0.69-2.03μgkg 之间。开发的基于聚（MAA-co-DVB）整体柱的管内 SPME-HPLC 方法成功地用于灵敏地测定稻谷实际样品中的痕量真菌毒素，没有干扰峰，表明它有望用于复杂谷物样品中痕量真菌毒素的检测。
