Yıldız Technical University, Faculty of Art and Science, Department of Chemistry, 34210, Davutpasa, Esenler, Istanbul, Turkey.
Turkish Academy of Sciences (TÜBA), Vedat Dalokay Street, No: 112, 06670, Çankaya, 06690, Ankara, Turkey.
Environ Monit Assess. 2023 Aug 18;195(9):1063. doi: 10.1007/s10661-023-11575-1.
This study presents a highly sensitive and accurate analytical strategy for the determination of fenuron in wastewater samples using gas chromatography-mass spectrometry (GC-MS). Simultaneous derivatization and spray-based fine droplet formation-liquid phase microextraction (SFDF-LPME) method was developed and performed to achieve low detection limits. The parameters of the derivatization and SFDF-LPME method were optimized by univariate approach to improve sensitivity and selectivity. Under the optimum SFDF-LPME-GC-MS conditions, the limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.15 and 0.49 mg/kg, respectively. In addition, the linear range was calculated as 0.51-24.50 mg/kg. Recovery studies were carried out on wastewater samples to determine the accuracy of the developed method and its applicability to real sample matrix. Matrix matching calibration strategy was applied to eliminate/reduce any possible interference effects caused by the complexity of the wastewater matrix and to increase the accuracy of the analytical results. Percent recovery results varied between 85.9 and 120.9% with small percent relative standard deviation values. These results were satisfactory in terms of the accuracy and applicability of the proposed method for wastewater samples.
本研究提出了一种使用气相色谱-质谱联用（GC-MS）测定废水中菌脲的高灵敏度和准确的分析策略。开发并采用同时衍生化和喷雾式细液滴形成-液相微萃取（SFDF-LPME）方法，以实现低检测限。通过单变量方法优化了衍生化和 SFDF-LPME 方法的参数，以提高灵敏度和选择性。在最佳的 SFDF-LPME-GC-MS 条件下，检测限（LOD）和定量限（LOQ）分别为 0.15 和 0.49 mg/kg。此外，线性范围计算为 0.51-24.50 mg/kg。在废水样品中进行了回收研究，以确定所开发方法的准确性及其对实际样品基质的适用性。采用基质匹配校准策略消除/减少废水基质复杂性可能引起的任何干扰影响，提高分析结果的准确性。回收率结果在 85.9%至 120.9%之间变化，相对标准偏差值较小。这些结果在废水样品中提出的方法的准确性和适用性方面令人满意。
