Department of Analytical Chemistry, Faculty of Pharmacy, Cumhuriyet University, 58140 Sivas, Turkey.
Department of Analytical Chemistry, Faculty of Pharmacy, Erciyes University, 38039 Kayseri, Turkey.
Molecules. 2019 Dec 17;24(24):4621. doi: 10.3390/molecules24244621.
A sensitive, rapid, reliable, and easily applicable method based on magnetic solid phase extraction (MSPE) combined with HPLC-PDA was developed for monitoring propoxur (PRO) and fenitrothion (FEN) pesticides in environmental water samples. The effect of major experimental variables on the extraction efficiency of both the pesticides was investigated and optimized systematically. For this purpose, a new magnetic material containing decanoic acid on the surface of particles was synthesized and characterized by XRD, FT-IR, SEM, EDX, and TGA analysis in detail. The simultaneous determination of pesticide molecules was carried out by using a Luna Omega C18 column, isocratic elution of acetonitrile (ACN): Water (70:30 /) with a flow rate of 1.2 mL min. After MSPE, the linear range for pesticide molecules (r > 0.9982) was obtained in the range of 5-800 and 10-800 ng mL, respectively. The limit of detections (LOD) are 1.43 and 4.71 ng mL for PRO and FEN, respectively while RSDs % are below 3.5%. The applicability of the proposed method in four different environmental samples were also investigated using a standard addition-recovery procedure. Average recoveries at two spiking levels were over the range of 91.3-102.5% with RSD < 5.0% ( = 3). The obtained results show that decanoic acid grafted magnetic particles in MSPE combined with HPLC-PDA is a fast and simple method for the determination of PRO and FEN in environmental water samples.
建立了一种基于磁固相萃取（MSPE）结合高效液相色谱-光电二极管阵列检测（HPLC-PDA）的灵敏、快速、可靠且易于应用的方法，用于监测环境水样中的丙溴磷（PRO）和fenitrothion（FEN）农药。系统地研究和优化了主要实验变量对两种农药萃取效率的影响。为此，合成并详细表征了一种新的磁性材料，其表面含有癸酸。通过 XRD、FT-IR、SEM、EDX 和 TGA 分析。采用 Luna Omega C18 柱，以乙腈（ACN）：水（70:30/）为流动相，流速为 1.2 mL min，进行等度洗脱，实现了农药分子的同时测定。经 MSPE 后，两种农药分子的线性范围分别为 5-800 和 10-800 ng mL，相关系数（r）均大于 0.9982。PRO 和 FEN 的检出限（LOD）分别为 1.43 和 4.71 ng mL，相对标准偏差（RSD）%均低于 3.5%。采用标准加入-回收法考察了该方法在四种不同环境水样中的适用性。两个加标水平的平均回收率在 91.3-102.5%之间，RSD < 5.0%（n = 3）。结果表明，MSPE 中接枝癸酸的磁性粒子与 HPLC-PDA 结合是一种快速、简单的方法，可用于测定环境水样中的 PRO 和 FEN。
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