Su Örneklerinde 4-Nonylfenolün Tayini için Dispersif Sıvı-Sıvı Mikroekstraksiyon-Gaz Kromatografisi-Kütle Spektrometrik Bir Yöntem

Year 2023, Volume: 23 Issue: 5, 1103 - 1111, 30.10.2023

Sabahattin Deniz

https://doi.org/10.35414/akufemubid.1341412

Abstract

Bu çalışmada çevre dostu, basit ve oldukça hassas bir teknik olan dağılma sıvı-sıvı mikroekstraksiyon
(DLLME) yöntemi, sucul ortamlarda 4-nonylfenolün ayırma ve analizi için geliştirilmiştir. Ekstraksiyon
işlemi, 1-undekanol-su dağılma sıvı-sıvı sistemi kullanılarak 4-nonylfenolün izolasyonunu içermiştir. 1
undekanol ve asetonitril miktarı ile sulu çözeltinin iyonik şiddeti gibi mikroekstraksiyon verimliliğini
etkileyen temel değişkenler hassas bir şekilde ayarlanmıştır. Ayrıca, Gaz Kromatografisi-Kütle
Spektrometresi (GC-MS) cihazının kromatografik parametreleri de hassas analiz için optimize edilmiş ve
4-nonylfenol analizi 2-1000 µg/L aralığında lineer kalibrasyon eğrisi kullanılarak gerçekleştirilmiştir, bu
sayede hızlı bir 6 dakikalık alıkonma süresi elde edilmiştir. Yöntem, 0.05 µg/L tespit limiti ve 188 ön
zenginleştirme faktörüne sahiptir. Analit geri kazanım oranları %96 ile %103 aralığındadır ve göreceli
standart sapma %3'ün altındadır. Geliştirilen prosedür, musluk suyu ve nehir suyu örneklerinin
incelenmesi için etkili bir şekilde değerlendirilmiştir.

Keywords

4-Nonilfenol, GC-MS, Sıvı-sıvı mikroekstraksiyon, Ön zenginleştirme

A Dispersive Liquid-Liquid Micro Extraction-Gas Chromatography-Mass Spectrometric Method for The Determination of 4-Nonylphenol in Water Samples

Abstract

In this study an environmentally-friendly, uncomplicated, and responsive method involving dispersive
liquid-liquid microextraction (DLLME) was presented for the isolation and analysis of 4-nonylphenol in
aquatic environments. The extraction process employed the undecanol–water dispersive liquid-liquid
system to isolate 4-nonylphenol. Essential variables impacting the efficiency of microextraction, such
as the quantities of 1-undecanol and acetonitrile, as well as the ionic strength of the aqueous solution,
were fine-tuned. Furthermore, the chromatographic parameters of the Gas Chromatography-Mass
Spectrometer (GC-MS) were optimized for precise analysis, and the analysis of 4-nonylphenol was
conducted using a linear calibration curve spanning 2-1000 µg/L, achieving a rapid 6-minute retention
time. The method exhibited a detection limit of 0.05 µg/L and a preconcentration factor of 188. Analyte
recovery rates ranged from 96% to 103%, having a relative standard deviation below 3%.The applied
procedure was effectively evaluated for its suitability in examining tap water and river water samples.

Keywords

4-Nonylphenol, GC-MS, Liquid-liquid microextraction, Preconcentration

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