Magnetic Solid-Phase Extraction Combined with Dispersive Liquid-Liquid Microextraction Followed by HPLC for Determination of Four Aromatic Amines Released from Azo Dyes in Paper Samples

Abstract

A novel extraction technique combining dispersive liquid-liquid microextraction (DLLME) with magnetic solid-phase extraction (MSPE) is presented for pre-concentration of four primary aromatic amines (PAAs) released from azo dyes in paper samples prior to high performance liquid chromatography (HPLC). n-Octanol was used as the extractant and hydrophobic oleic acid modified Fe 3 O 4 nanoparticles (Fe 3 O 4 @OA NPs) as an efficient adsorbent was applied to retrieve the PAAscontaining n-octanol in the DLLME step. Because of the rapid mass transfer associated with the DLLME and MSPE steps, fast extraction could be achieved. The main parameters affecting the efficiency of MSPE-DLLME procedure of PAAs were investigated and optimized. Under optimum conditions, the recoveries ranged from 79.6 to 88.5% and the limits of detection (LODs) were in the range of 0.21-1.16 ng mL-1 (S / N = 3). The intra-day precision (relative standard deviation (RSD)) was below 7.8% and inter-day RSD was less than 11%.