Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., Evin, Tehran 1983969411, Iran.
Department of Analytical Chemistry and Pollutants, Shahid Beheshti University, G. C., Evin, Tehran 1983969411, Iran.
Food Chem. 2022 Nov 1;393:133350. doi: 10.1016/j.foodchem.2022.133350. Epub 2022 May 31.
This study employed thin-film solid-phase microextraction procedure as a simple, sensitive, green, and solvent-free method for the co-extraction of multi-classes herbicides from cereal samples before HPLC-UV analysis. To provide an efficient sorbent, electrospun nanofibers of the crosslinked polyacrilonitril/ϒ-cyclodextrin-metal-organic framework (PAN/ϒ-CD-MOF) were successfully fabricated and assessed as a new thin-film adsorbent. Under the optimal conditions (desorption solvent: acetonitrile, desorption time: 5 min, sample solution pH: 7.0, salt concentration: 15% (w/w), and extraction time: 15 min), good linearity in the range of 2.5-1250.0 ng/mL (r ≥ 0.992) was obtained. The detection limits were 0.75-2.50 ng/mL. The extraction recoveries and relative recoveries were 64.9-75.7% and 92.9-106.1%, respectively. The method showed good precision as the relative standard deviations were ≤ 6.3%. Finally, the developed method was applied efficiently for trace analysis of the herbicides in wheat, rice, and barley samples. Generally, the proposed method provided a simple, sensitive, environmentally friendly, and relatively fast approach.
本研究采用薄膜固相微萃取程序作为一种简单、灵敏、绿色且无溶剂的方法，用于在 HPLC-UV 分析前从谷物样品中共同提取多类除草剂。为了提供一种有效的吸附剂，成功制备了交联聚丙烯腈/γ-环糊精-金属有机骨架（PAN/γ-CD-MOF）的静电纺纳米纤维，并将其评估为一种新的薄膜吸附剂。在最佳条件下（解吸溶剂：乙腈，解吸时间：5 分钟，样品溶液 pH 值：7.0，盐浓度：15%（w/w），萃取时间：15 分钟），在 2.5-1250.0ng/mL 的范围内获得了良好的线性关系（r≥0.992）。检测限为 0.75-2.50ng/mL。萃取回收率和相对回收率分别为 64.9-75.7%和 92.9-106.1%。该方法表现出良好的精密度，相对标准偏差≤6.3%。最后，该方法有效地应用于小麦、大米和大麦样品中除草剂的痕量分析。总的来说，所提出的方法提供了一种简单、灵敏、环保且相对较快的方法。
