Sains Malaysiana 45(5)(2016): 803–810

Detection of Gliclazide in Aqueous Samples using Liquid Chromatography/Time-of-Flight/Mass Spectrometry

(Penentuan Gliklazida dalam Sampel Akues Menggunakan Kromatografi Cecair/Masa Penerbangan/Spektrometri Jisim)

FOUAD FADHIL AL-QAIM^1,2, MD PAUZI ABDULLAH¹, JALIFAH LATIP¹, WAN MOHD AFIQ WAN MOHD KHALIK¹, NURFAIZAH ABU TAHRIM¹, NURUL AUNI ZAINAL ABIDIN¹ & MOHAMED ROZALI OTHMAN^1,3*

¹School of Chemical Sciences and Food Technology, Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor Darul Ehsan, Malaysia

²Department of Chemistry, Faculty of Sciences for Women, Babylon University, P.O. Box 4, Hilla

Iraq

³Centre for Water Research and Analysis (ALIR), Faculty of Science and Technology, Universiti Kebangsaan Malaysia, 43600 Bangi, Selangor Darul Ehsan, Malaysia

Diserahkan: 20 Mei 2015/Diterima: 19 November 2015

ABSTRACT

The big challenge for the detection of pharmaceutical residues in water samples is the type of ionization mode in terms of positive or negative ionization which plays an important role to identify and quantify the analytes using liquid chromatography/mass spectrometry. An analytical method was applied to analysis of gliclazide (diabetic drug) in surface water and wastewater from sewage treatment plants and hospitals. The proposed analytical method allows simultaneous isolation and concentration procedure using solid phase extraction (Oasis HLB) prior to separation using high-performance liquid chromatography. The detection and confirmation was achieved by applying time-of-flight analyzer. The limits of quantification were as low as 1.4 ng/L (deionized water), 4 ng/L (surface water), 27 ng/L (hospital influent), 10 ng/L (hospital effluent), 6 ng/L (sewage treatment plant effluent) and 21 ng/L (sewage treatment plant influent), respectively. On average, good recoveries of higher than 87% were obtained for gliclazide in the studied samples. The proposed method successfully determined and quantified gliclazide in surface water and wastewater. The results showed that gliclazide is a persistent compound in sewage treatment effluents as well as in the recipient rivers. Gliclazide was detected in all samples and the highest concentration was 130 ng/L in influent of sewage treatment plant.

Keywords: Effluent hospital; gliclazide; positive ionization; solid phase extraction

ABSTRAK

Antara cabaran besar untuk mengesan sisa farmasi dalam sampel air menggunakan kromatografi cecair/spektrometri jisim adalah jenis mod pengionan, dengan pengionan positif atau negatif memainkan peranan yang penting untuk mengenal pasti dan menilai kandungan analit. Suatu kaedah analisis telah diaplikasikan untuk menganalisis gliklazida (ubat diabetik) dalam air permukaan dan juga air buangan dari loji rawatan kumbahan dan hospital. Kaedah analisis yang digunakan membolehkan prosedur pengasingan dan pemekatan dijalankan serentak menggunakan pengekstrakan fasa pepejal (Oasis HLB), iaitu teknik pemisahan dengan menggunakan kromatografi cecair berprestasi tinggi. Pengesanan dan pengesahan telah dicapai dengan menggunakan penganalisis masa penerbangan. Had kuantifikasi adalah serendah 1.4 ng/L (air ternyahion), 4 ng/L (air permukaan), 27 ng/L (influen hospital), 10 ng/L (efluen hospital), 6 ng/L (efluen loji rawatan sisa kumbahan) dan 21 ng/L (influen loji rawatan kumbahan). Secara keseluruhannya, peratusan perolehan semula yang baik diperoleh untuk gliklazida dalam sampel yang dikaji iaitu melebihi nilai 87%. Kaedah yang dicadangkan berjaya menentukan secara kuantitatif kandungan gliklazida dalam air permukaan dan air sisa buangan. Hasil kajian menunjukkan bahawa gliklazida adalah sebatian kekal dalam efluen rawatan kumbahan dan juga di dalam sungai. Gliklazida telah dikesan dalam kesemua sampel dan kepekatan maksima ialah 130 ng/L dalam influen loji rawatan sisa kumbahan.

Kata kunci: Efluen hospital; gliklazida; pengekstrakan fasa pepejal; pengionan positif

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*Pengarang untuk surat-menyurat; email: rozali@ukm.edu.my