Necmettin Erbakan University, Environmental Engineering Department, Konya, Turkey.
Acta Pharm. 2018 Sep 1;68(3):313-324. doi: 10.2478/acph-2018-0024.
A novel micro-extraction technique for a rapid and sensitive analysis of diclofenac (DCF) in water samples has been developed. DCF was derivatized and extracted simultaneously using vortex-assisted liquid-liquid micro-extraction (VALLME) prior to gas chromatography with mass spectrometry detection. The effects of extraction solvent volume, extraction and derivatization time and ionic strength of the sample were studied using 23 factorial experimental design. The optimum extraction conditions were as follows: 200 μL of chloroform, 25 μL of N-methyl-N-trimethylsilyl-trifluoroacetamide (MSTFA) derivatization reagent, vortex extraction and derivatization time 5 min at 3000 rpm. The extraction recovery for different fortification levels was 98 %. Also, the proposed micro-extraction method exhibited results comparable with the solid phase extraction of real water samples. The proposed one-step VALLME and derivatization method is simpler and faster than the conventional extraction and derivatization methods used for the determination of DCF in real water samples.
一种新型的微萃取技术，用于快速灵敏地分析水样中的双氯芬酸（DCF）。在气相色谱-质谱检测前，采用涡旋辅助液-液微萃取（VALLME）对 DCF 进行衍生和萃取。使用 23 因子实验设计研究了萃取溶剂体积、萃取和衍生时间以及样品离子强度对萃取的影响。最佳萃取条件如下：200 μL 氯仿，25 μL N-甲基-N-三甲基硅基三氟乙酰胺（MSTFA）衍生试剂，3000 rpm 涡旋萃取和衍生 5 min。不同加标水平的萃取回收率为 98%。此外，所提出的微萃取方法与实际水样的固相萃取结果相当。与用于实际水样中 DCF 测定的常规萃取和衍生方法相比，一步 VALLME 和衍生方法更简单、更快。
