Ahmad Lutfi Anis
Faculty of Applied Sciences, Universiti Teknologi MARA, 94300 Kota Samarahan, Sarawak, Malaysia

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Selective Determination of Acidic Drugs in Water Samples Using Online Solid Phase Extraction Liquid Chromatography with Alginate Incorporated Multi-Walled Carbon Nanotubes as Extraction Sorbent Nurzaimah Zaini @ Othman; Nor Suhaila Mohamad Hanapi; Nor’ashikin Saim; Wan Nazihah Wan Ibrahim; Ahmad Lutfi Anis
Indonesian Journal of Chemistry Vol 20, No 5 (2020)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | Full PDF (20.631 KB) | DOI: 10.22146/ijc.43703

Abstract

A rapid and effective method is developed for selective determination of five selected acidic drugs (salicylic acid, naproxen, diclofenac, ibuprofen and mefenamic acid) in water samples by using online solid phase extraction (Online-SPE) prior to liquid chromatography diode array detector (LC-DAD) analysis. In this study, Alginate incorporated multi-walled carbon nanotubes (Alg-MWCNT) beads were prepared and utilized as solid phase extraction sorbent. Optimization of online SPE-LC operating parameters such as valve switching time, composition of acetonitrile and buffer pH was conducted using Box-Behnken Design of Response Surface Methodology (RSM) to evaluate the interactive effects of these three variables. Under the optimized conditions (valve switching time: 1.5 min, composition of acetonitrile: MSA, 60:40 and buffer pH: pH 2), the method showed good linearity (1–500 μg L−1) with coefficient of determination (R2) of 0.9971–0.9996 and low limits of detection ≤ 0.018 µg L–1. The method showed high relative recoveries in the range of 75–110% for river water and tap water samples, respectively with RSDs of ≤ 7.8 (n = 3). This method was successfully applied to the determination of acidic drugs in river and tap water samples. In addition, Alg-MWCNT sorbent offered high degree of selectivity and efficiency for online SPE-LC-DAD analysis.
Pre-Concentration and Determination of Tetracyclines Antibiotics Residues in Water Samples Using RGO/Fe3O4 Nanocomposite as Extraction Sorbent Ungku Amirul Arif Ungku Abdullah; Nor Suhaila Mohamad Hanapi; Wan Nazihah Wan Ibrahim; Nursyamsyila Mat Hadzir; Nurzaimah Zaini; Ahmad Lutfi Anis; Noorfatimah Yahaya
Indonesian Journal of Chemistry Vol 21, No 5 (2021)
Publisher : Universitas Gadjah Mada

Show Abstract | Download Original | Original Source | Check in Google Scholar | DOI: 10.22146/ijc.64414

Abstract

Existing methods used in tracing Tetracyclines' antibiotics (TCAs) residues which pose serious environmental problems, consume high amounts of organic solvents, are time-consuming, and are relatively expensive. A simple and effective magnetic solid-phase extraction (MSPE) based on reduced graphene oxide/magnetite (RGO/Fe3O4) nanocomposite sorbent was successfully developed for preconcentration and extraction of TCAs residues from water samples. The analytes were determined by high-performance liquid chromatography with a diode-array detector (HPLC-DAD). The synthesized nanocomposite was characterized using Fourier-transform infrared spectroscopy (FTIR), X-ray diffractometry (XRD), and field emission scanning electron microscopy (FESEM). Sample pH, amount of adsorbent, sample volume, extraction time, desorption time, and desorption solvent were evaluated and optimized. Under optimized conditions, the method demonstrated good linearity over the concentration range of 0.05–1.0 mg L–1 with the coefficient of determination (R2) ≥ 0.9978. Limit of detection (LOD) and limit of quantification (LOQ) were 0.006–0.011 mg L–1 and 0.019–0.036 mg L–1, respectively. The accuracy and precision of the developed method were proven by good analyte recovery (89.77–106.33%) and acceptable precision with relative standard deviation, RSD ≤ 5.54%. The results showed that magnetic solid RGO/Fe3O4 could be a suitable adsorbent in the preconcentration and extraction of TCAs in water samples.