开发一种简单快速的溶剂辅助分散固相萃取法,用于痕量检测水、水果、蔬菜和农业土壤样品中的三唑类杀菌剂

Zolfaghar Aladaghlo, Ali Sahragard, Alireza Fakhari
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摘要

开发了溶剂辅助分散固相萃取(SA-DSPE)方法来测定三唑类杀菌剂(TFs)。在 SA-DSPE 技术中,在样品溶液中加入 1000 μL 作为分散溶剂的乙醇和少量作为吸附剂的苯偶酰,会产生浑浊的溶液。萃取完成后,对混合物进行离心,以分离出苯偶酰。接着,将苯偶酰溶解在乙醇中,然后用气相色谱-火焰离子化检测器对所得溶液进行分析。该方法在最佳条件下(吸附剂:苯齐尔,苯齐尔用量:2% w/v,溶液 pH 值:7.0,分散溶剂:乙醇),对 TFs 的定量具有较高的线性(R2 > 0.9963)和重复性(相对标准偏差 % < 4.3):7.0,分散溶剂:乙醇,乙醇体积:1000 μL,离心时间:3 分钟,萃取温度:25°C:3 分钟,萃取温度:25°C,离子强度:不加盐)。该方法的检出限、定量限和预浓缩因子分别为 0.3-0.9 纳克/毫升、1.0-3.0 纳克/毫升和 419-426。最后,利用该验证方法测定了各种实际样品(包括水、水果、蔬菜和农业土壤)中的 TFs,相对回收率为 93.0% 至 104%。
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Development of a simple and fast method named solvent‐assisted dispersive solid phase extraction for trace detection of triazole fungicides in water, fruit, vegetable, and agricultural soil samples
Solvent‐assisted dispersive solid‐phase extraction (SA‐DSPE) approach was developed to measure triazole fungicides (TFs). In the SA‐DSPE technique, the addition of 1000 μL of ethanol as a disperser solvent, along with a small quantity of benzil as a sorbent to the sample solution, led to a cloudy solution. After completion of the extraction, the mixture was subjected to centrifugation to isolate benzil. Next, benzil was dissolved in ethanol, and the resulting solution was subsequently analyzed by a gas chromatography‐flame ionization detector. This method demonstrated high linearity (R2 > 0.9963) and repeatability (relative standard deviation % < 4.3) for the quantification of TFs under the optimal conditions (sorbent: benzil, amount of benzil: 2% w/v, pH of solution: 7.0, disperser solvent: ethanol, volumes of ethanol: 1000 μL, centrifuge time: 3 min, extraction temperature: 25°C, and ionic strength: without salt addition). The proposed SA‐DSPE yielded detection limits, quantification limits, and preconcentration factors within the ranges of 0.3–0.9 ng/mL, 1.0–3.0 ng/mL, and 419–426, respectively. Finally, the validated method was employed to determine TFs in a diverse range of real samples, encompassing waters, fruits, vegetables, and agricultural soils, with relative recoveries ranging from 93.0% to 104%.
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