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-QAIM1,2, MD PAUZI ABDULLAH1, JALIFAH LATIP1, WAN MOHD AFIQ WAN MOHD KHALIK1, NURFAIZAH ABU TAHRIM1, NURUL AUNI ZAINAL ABIDIN1 & MOHAMED ROZALI OTHMAN1,3*
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
Received: 20 May 2015/Accepted: 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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*Corresponding author; email: rozali@ukm.edu.my |