A novel green microextraction supramolecular (SUPRA)-based method for simultaneous preconcentration of seven pesticides, acetamiprid, azoxystrobin, bifenthrin, carbendazim, chlorpyrifos, imidacloprid, and tebuconazole, in water samples and cereal flours with further determination by HPLC-DAD was developed. The method uses 113 µL of 1-decanol as amphiphilic extractor and 500 µL of tetrahydrofuran as disperser solvent. To perform the method optimization, a 2⁵ factorial design and Doehlert design combined with Derringer–Suich desirability function and response surface methodology were used. The microextraction of the pesticides was carried out at pH 6.3 in the presence of 5% NaCl (w/v), low vortex-assisted extraction time (30 s) and it was provided high preconcentration factors (3.6–266.1), and low LOQs (8.98–29.92 µg L⁻¹). The intra-day (n = 10) and inter-day (n = 10) precision assessed as the percentage of relative standard deviation (%RSD) for concentrations of 50.0 and 200.0 µg L⁻¹ varied from 1.7 to 4.1%. The method was successfully applied to determine pesticides in river and lake water samples using external calibration curves. Considering the property of restricted access materials of SUPRAs, the microextraction method was also applied to the direct treatment of solid samples of wheat, oat, and rice flours. High recovery values in the range of 80–112% were obtained, thereby proving the absence of possible interference from matrix components.

Graphical Abstract

中文翻译：

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开发一种绿色水诱导的限制进入超分子溶剂微萃取方法，可显着改进水样和谷物面粉中各种极性农药的测定

开发了一种基于绿色微萃取超分子 (SUPRA) 的新型方法，用于同时富集水样和谷物粉中啶虫脒、嘧菌酯、联苯菊酯、多菌灵、毒死蜱、吡虫啉和戊唑醇 7 种农药，并通过 HPLC-DAD 进一步测定。该方法使用 113 µL 1-癸醇作为两亲萃取剂，使用 500 µL 四氢呋喃作为分散溶剂。为了进行方法优化，使用了 2 ⁵因子设计和 Doehlert 设计，并结合了 Derringer-Suich 合意性函数和响应面方法。农药的微萃取在 pH 6.3、5% NaCl (w/v) 存在下、低涡旋辅助萃取时间 (30 s) 下进行，并提供高预浓缩因子 (3.6–266.1) 和低 LOQ （8.98–29.92 µg L ^-1）。日内 ( n  = 10) 和日间 ( n = 10) 精度评估为浓度为 50.0 和 200.0 µg L ^-1的相对标准偏差 (%RSD) 的百分比，变化范围为 1.7% 至 4.1%。该方法成功应用于利用外标曲线测定河流和湖泊水样中的农药。考虑到SUPRA限制性材料的特性，微萃取方法也被应用于小麦、燕麦和米粉固体样品的直接处理。获得了 80-112% 范围内的高回收率，从而证明不存在基质成分的可能干扰。

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