Background

Extensive use of high-efficiency pyrethroid pesticides as pest-control agents lead to remarkable adsorption and release of these materials in soil and aquatic environment which could have serious adverse effects on water and food chain quality as well as human health. In this study, a molecularly imprinted polymer was synthesized and used as a selective sorbent in the sample preparation procedure in order to facilitate sensitive and quantitative exposure assessment of insecticide permethrin.

Methods

Molecular imprinted nanoparticles were prepared by precipitation polymerization technique using 1:4:20 mmol ratio of the template, functional monomer, and cross-linker, respectively, as well as 80 mL of chloroform as progen solvent. The obtained nanoparticles were characterized by field emission scanning electron microscopy (FESEM) and Fourier transform infrared spectrometry (FT-IR). The optimization of critical variables in the MISPE process was done using the central composite design (CCD) of the response surface methodology.

Results

Quadratic regressional models were developed to correlate the response and independent variables and the analysis of variance (ANOVA) verified the excellent fitting of proposed models for experimental data. Optimum conditions for the highest MISPE yield were selected as follow: sorbent mass of 7.71 mg, sample pH 5.58 and 5.68 for cis and trans-permethrin, respectively, sample flow rate of 0.6 mL/min, as well as 5 and 3.94 mL of methanol/acetic acid at the flow rate of 2 mL/min as elution solvents for cis and trans-permethrin, respectively. Under optimized conditions, the linear range was obtained 20–120 μg/L (R2 = 0.99) and the detection limits were 5.51 and 5.72 μg/L for cis and trans-permethrin, respectively. Analysis of real samples demonstrated the high extraction efficiency of designed protocol ranging from 93.01 to 97.14 with the relative standard deviation (RSD) less than 4.51%.

Conclusions

The satisfactory results confirmed the reliability and efficiency of the proposed method for trace analysis of permethrin isomers in biological and environmental samples.

中文翻译：

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用于氯菊酯选择性暴露评估的分子印迹纳米粒子的合成：响应面法优化。

背景

高效拟除虫菊酯农药作为害虫防治剂的广泛使用导致这些物质在土壤和水环境中的显着吸附和释放，可能对水和食物链质量以及人类健康产生严重的不利影响。在本研究中，合成了一种分子印迹聚合物，并将其用作样品制备过程中的选择性吸附剂，以促进对杀虫剂氯菊酯的敏感和定量暴露评估。

方法

分子印迹纳米粒子通过沉淀聚合技术制备，分别使用 1:4:20 mmol 的模板、功能单体和交联剂，以及 80 mL 氯仿作为前体溶剂。通过场发射扫描电子显微镜（FESEM）和傅里叶变换红外光谱（FT-IR）对获得的纳米颗粒进行表征。使用响应面方法的中心复合设计 (CCD) 对 MISPE 过程中的关键变量进行了优化。

结果

开发了二次回归模型来关联响应变量和自变量，方差分析 (ANOVA) 验证了所提出的模型对实验数据的出色拟合。选择最高 MISPE 产率的最佳条件如下：吸附剂质量为 7.71 mg，顺式和反式氯菊酯的样品 pH 值分别为 5.58 和 5.68，样品流速为 0.6 mL/min，甲醇为 5 和 3.94 mL /乙酸以 2 mL/min 的流速分别作为顺式和反式氯菊酯的洗脱溶剂。在优化条件下，顺式和反式氯菊酯的线性范围为 20–120 μg/L (R2 = 0.99)，检测限分别为 5.51 和 5.72 μg/L。对真实样品的分析证明了设计方案的高提取效率，范围从 93.01 到 97。

结论

令人满意的结果证实了所提出的生物和环境样品中氯菊酯异构体痕量分析方法的可靠性和效率。