Development of Analytical
Method for Detection of Some Pharmaceuticals in Surface
Water
Fouad Fadhil Al-Qaim1,2,
Md Pauzi Abdullah1,3*, Mohamed Rozali Othman1,3,
Jalifah Latip1 and Wan Mohamed Afiq1
1School of Chemical Sciences
and Food Technology, Faculty of Science and Technology,
Universiti
Kebangsaan
(UKM), 43600 Bangi, Selangor.
Malaysia, 2Chemistry Department, Faculty of
Sciences for Women, Babylon University, PO Box 4, Hilla,
Iraq, 3Centre for Water Research and Analysis
(ALIR), Faculty of Science and Technology,
Universiti
Kebangsaan (UKM), 43600 Bangi, Selangor.
Malaysia.
*For correspondence:
Email:
mpauzi@ukm.my
Tel: +060193295636
Received: 25 April 2013
Revised accepted: 12 July
2013
Tropical Journal of
Pharmaceutical Research, August 2013; 12(4):
609-616
http://dx.doi.org/10.4314/tjpr.v12i4.25
Abstract
Purpose: To develop and validate a simple
method using solid – phase extraction along with liquid
chromatography–time of flight mass spectrometry for the
analysis of pharmaceuticals in surface water of Tangkas
River, Malaysia.
Methods: Liquid chromatography (LC) was
performed on a Dionex Ultimate 3000/LC 09115047 (USA)
system equipped with a vacuum degasser, a quaternary
pump, an autosampler and UV-Vis diod array detector.
Chromatography was performed on a Thermo Scientific C18
(250 mm x 2.1 mm, i.d.: 5µm) column. The injection
volume was 20 µL. All compounds (hydrochlorothiazide,
gliclazide, diclofenac-Na and mefenamic acid) were
analysed in negative ion (NI) mode and eluted off the
column with a mobile phase consisting of (A) 0.1% formic
acid (FA) in deionised water (DIW) and (B) 40%
acetonitrile (ACN) in methanol (MeOH) at 0.3 ml/min.
Mass spectrometry was performed on a time of flight (TOF)
instrument.
Results: The linearity range, 5 - 500 ng/mL,
provided a determination coefficient (R2) >
0.99 for all compounds. The limit of detection (LOD)
ranged from 65 - 136 ng/L while recovery ranged from 45
- 111.2 % in the river water. Two pharmaceutical
compounds were detected in the surface water samples:
diclofenac sodium and mefenamic acid at concentrations
of 340 and 545 ng/L, respectively.
Conclusion:
The developed method is linear in the range 5 - 500 ng/mL,
and precise and acceptable recoveries were obtained. In
addition, this method is suitable to identify and
quantify trace concentrations of diclofenac sodium and
mefenamic acid in surface water.
Keywords: Diclofenac, Mefenamic acid,
Electrospray Ionization, Mass spectrometry, Solid phase
extraction (SPE), Tangkas river, Collision energy.
