MALAYSIAN JOURNAL OF CHEMISTRY (MJChem)

MJChem is double-blind peer reviewed journal published by the Malaysian Institute of Chemistry (Institut Kimia Malaysia) E-ISSN: 2550-1658

Optimisation and Validation of a Headspace-Solid Phase Micro Extraction GCMS using Central Composite Design for Determination of Polyaromatic Hydrocarbons in Water Samples

Muhammad Umar Nazhan Muhamad Muhaidi
Universiti Teknologi MARA
Nor Suhaila Mohamad Hanapi
Universiti Teknologi MARA
Nurzaimah Zaini
Universiti Teknologi MARA
Ahmad Lutfi Anis
Universiti Teknologi MARA
Wan Nazihah Wan Ibrahim
Universiti Teknologi MARA

DOI: https://doi.org/10.55373/mjchem.v25i3.440

Keywords: Headspace solid phase microextraction; response surface methodology; central composite design; polycyclic aromatic hydrocarbons; water samples

Abstract

A headspace solid phase microextraction (HS-SPME) method coupled with gas chromatography- mass spectrometry (GC-MS) was developed for the determination of selected polyaromatic hydrocarbons (PAHs) in water samples. Two extraction parameters i.e. extraction time and temperature were investigated using central composite design (CCD) of response surface methodology. The regression line fitted well with the data with an r2 value of 0.9048. The lack of fit test gives the highest value of the Sum of Squares of 1.786x1013 with a probability F value of 13.31, showing a significant quadratic model. Under the optimal condition, the method provided good linearity, with a concentration range of 2.0-10.0 mgL-1 with coefficients of determination, r2 ≥ 0.9993 and good limits of detection, which is (0.287-0.999 mgL-1) and limits of quantification (0.958-1.21 mgL-1). The results also showed good relative recoveries ranging from 60 to 103% with acceptable reproducibility (RSDs ≤ 0.67%, n = 3). The study’s results revealed that the HS-SPME-GC-MS method is easy, feasible, and selective for the trace analysis of fluorene and phenanthrene in water samples.

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Published 29 June 2023


Issue Vol 25 No 3 (2023): Malaysian Journal of Chemistry

Section