Investigation of the performance of cross-linked poly(acrylic acid) and poly(methacrylic acid) as efficient adsorbents in SPE columns for simultaneous preconcentration of tricyclic antidepressants in water samples

Abstract

A solid phase extraction-based (SPE) procedure for simultaneous preconcentration of five tricyclic antidepressants (TCAs), amitriptyline hydrochloride (AMT), nortriptyline hydrochloride (NOR), doxepin hydrochloride (DOX), imipramine hydrochloride (IMI), and clomipramine hydrochloride (CLO) from water samples with determination by HPLC-DAD is proposed. Polymers were characterized by FT-IR, SEM, and thermogravimetric analysis. SPE-based methods were carried out by the preconcentration of 320.0 mL of TCAs at pH 7.0 (buffered with 0.01 mol L⁻¹ phosphate buffer) through 70.0 mg of adsorbent packed into a SPE cartridge, followed by elution with 1.0 mL of ACN : MeOH : acetic acid solution (45 : 45 : 10% v/v). Higher preconcentration factors were obtained ranging from 117.9 to 372.2 and 207.1 to 396.1 by using poly(MAA-co-EGDMA) and poly(AA-co-EGDMA), respectively, yielding lower limits of detection (0.03 to 0.12 μg L⁻¹) and (0.03 to 0.15 μg L⁻¹). These outcomes show satisfactory detectability of SPE-based methods, with slightly better performance using poly(MAA-co-EGDMA). On the other hand, poly(AA-co-EGDMA) was able to preconcentrate TCAs in the presence of humic acid (7.0 mg L⁻¹) without interference. The precision of methods assessed as RSD (%) was very similar, ranging from 1.7% to 16.3% for poly(MAA-co-EGDMA) and 1.7% to 13.4% for poly(AA-co-EGDMA). SPE cartridges packed with the polymers showed high reusability (52 cycles of preconcentration and elution) without losing adsorption efficiency. The methods were applied to determine TCAs in tap, lake, and stream water samples and the accuracy was attested by addition and recovery tests (86.7–116.0%), with determined nortriptyline ranging from 0.48 to 0.52 μg L⁻¹ in lake water samples.