The Malaysian Journal of Analytical Sciences Vol 17 No 2 (2013): 262 – 271

 

 

 

TANDEM SOLID PHASE EXTRACTION FOR THE DETERMINATION OF PHARMACEUTICALS IN WASTEWATER

 

(Pengekstrakan Fasa Pepejal Secara Penggabungan Katrij Untuk Analisis Farmaseutikal

Dalam Air Sisa Buangan)

 

Licaberth Ismail*, Rozita Osman, Norashikin Saim

 

Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor

 

*Corresponding author: lica.ismail@yahoo.com

 

 

 

Abstract

In this study, a simple and rapid tandem solid phase extraction (SPE) was developed for the analysis of seven pharmaceuticals (acetaminophen, caffeine, carbamazepine, diclofenac, naproxen, ibuprofen and metoprolol) in wastewater sample. The novel aspect of coupling SPE cartridge in tandem is the ability to simplify the SPE procedure (sample introduction step) as no single sorbent was able to retain and concentrate all selected compounds since these compounds are of different physicochemical properties. A tandem SPE cartridges using Oasis HLB and octadecyl bonded silica (C₁₈) was found to be efficient with the advantages of minimizing sample volume and reducing analysis time. Using this approach, carbamazepine, diclofenac, naproxen and metoprolol were trapped in the Oasis HLB while acetaminophen, caffeine and ibuprofen were trapped in the second cartridge (C₁₈). The instrumental limits of detection (LOD) ranged from 0.01 to 0.04 μg/L and satisfactory recoveries were obtained between 76% to 104%.  The calibration curves were linear from 0.1 to 5.0 µg/mL, with correlation coefficients (R²) in the range of 0.995 to 0.999. The developed method was applied to the analysis of pharmaceuticals in wastewater samples. The amount of pharmaceuticals detected in wastewater samples varied from 0.4 to 24.5 mg/L.

 

Keywords: pharmaceuticals, solid phase extraction, Oasis HLB, wastewater

 

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