Environmental Engineering Department, Civil Engineering Faculty, Yildiz Technical University, Davutpaşa, Esenler, 34220, İstanbul, Turkey.
Department of Chemistry, Faculty of Art and Science, Yildiz Technical University, Davutpaşa, Esenler, 34220, İstanbul, Turkey.
Environ Monit Assess. 2020 Jan 2;192(2):72. doi: 10.1007/s10661-019-8061-4.
This study presents the use of Quick Easy Cheap Efficient Rugged and Safe (QuEChERS) as an effective sample cleaning procedure and switchable solvent liquid phase microextraction (SS-LPME) as a preconcentration tool for the determination of fenazaquin by gas chromatography mass spectrometry (GC-MS) at ultratrace levels. After a thorough optimization process, 0.50 mL of switchable solvent, 1.5 mL of 1.0 M sodium hydroxide, and 15 s of vortexing were determined as optimum conditions of the SS-LPME method. The limit of detection (LOD) and limit of quantitation (LOQ) determined using the optimum method (SS-LPME/GC-MS) were 0.05 and 0.18 ng/mL, respectively. Compared with direct GC-MS determination of fenazaquin, the optimum method yielded about 800-fold enhancement in detection power of GC-MS. The method was applied to lake, irrigation canal, well, and wastewater samples. In order to test the method's applicability on fresh tomato samples, a QuEChERS method was used before applying the SS-LPME method. Matrix-matched calibration standards were used to enhance the accuracy of fenazaquin quantification in spiked tomato samples to obtain recovery results close to 100%.
本研究采用快速、简便、廉价、有效、耐用、安全(QuEChERS)作为有效的样品净化程序,采用可切换溶剂液相微萃取(SS-LPME)作为浓缩工具,结合气相色谱质谱(GC-MS)在痕量水平下测定芬扎喹。经过彻底的优化过程,确定 0.50 mL 可切换溶剂、1.5 mL 1.0 M 氢氧化钠和 15 s 涡旋为 SS-LPME 方法的最佳条件。使用最佳方法(SS-LPME/GC-MS)确定的检测限(LOD)和定量限(LOQ)分别为 0.05 和 0.18 ng/mL。与直接 GC-MS 测定芬扎喹相比,最佳方法使 GC-MS 的检测能力提高了约 800 倍。该方法已应用于湖泊、灌溉渠、水井和废水样品。为了测试该方法在新鲜番茄样品上的适用性,在应用 SS-LPME 方法之前,使用 QuEChERS 方法对其进行处理。采用基质匹配校准标准来提高在加标番茄样品中定量测定芬扎喹的准确性,以获得接近 100%的回收率结果。