Malaysian Journal of Analytical Sciences Vol 20 No 4
(2016): 726 - 734
DOI:
http://dx.doi.org/10.17576/mjas-2016-2004-04
DETERMINATION OF PRAZOSIN
AND SIMVASTATIN IN LANDFILL LEACHATE USING LIQUID CHROMATOGRAPHY-TIME OF
FLIGHT-MASS SPECTROMETRY
(Penentuan Prazosin dan
Simvastatin di dalam Larut Lesap Mengunakan Kromatografi Cecair-Masa
Penerbangan-Spektrometri Jisim)
Zainab Haider Mussa1,2,
Fouad Fadhil Al-Qaim1,3*, Md Pauzi Abdullah1,4, Mohamed
Rozali Othman1,4
1School
of Chemical Sciences and Food Technology, Faculty of Science and Technology,
Universiti Kebangsaan Malaysia, 43600 UKM
Bangi, Selangor, Malaysia
2Faculty
of Pharmacy
3Department
of Chemistry, Faculty of Sciences for Women
University of Babylon, PO Box 4, Hilla,
Iraq
4Centre
for Water Research and Analysis (ALIR), Faculty of Science and Technology,
Universiti Kebangsaan Malaysia, 43600 UKM
Bangi, Selangor, Malaysia
*Corresponding author: fouadalkaim@yahoo.com
Received: 13
January 2016; Accepted: 27 March 2016
Abstract
Human pharmaceuticals have been shown to occur in
considerably high amounts in sewage treatment plant (STP) effluents and surface
waters. So far there is no data available on the occurrence of prazosin and
simvastatin in leachate sample in Malaysia. Thus, this study is the first
report to analysis of prazosin and simvastatin in leachate samples by using
solid phase extraction-liquid chromatography-time of flight-mass spectrometry
(SPE-LC-TOF-MS). The proposed method included isolation and reconstitute
procedure. The linearity range was achieved at 1.5 -
3000 μg/L and 0.8 – 125 μg/L for prazosin and simvstatin, respectively with a
determination coefficient (R2) > 0.99. The limit of quantification
(LOQ) for prazosin and simvastatin was calculated at 2.1 and 0.5 ng/L in deionised water
(DIW), meanwhile it was recorded at 3.5 and 2.4 ng/L for prazosin and simvastatin in effluent sample, respectively. Two pharmaceutical
compounds were detected in the leachate samples: prazosin and simvastatin at
concentrations levels of 3850 and 415 ng/L, respectively.
Keywords: prazosin, simvastatin, leachate, solid phase
extraction, pharmaceutical pollution
Abstrak
Farmaseutikal manusia telah hadir di dalam effluen
loji sisa rawatan dan air permukaan. Sehingga kini, tiada data kajian yang
merekodkan kehadiran prazosin dan simvastatin dalam sampel larut lesap di
Malaysia. Maka, kajian ini merupakan laporan pertama tentang analisis terhadap
prazosin dan simvastatin di dalam sampel larut lesap mengunakan pengekstrakan
fasa pepejal-kromatografi cecair-masa penerbangan-spekrometri jisim
(SPE-LC-TOF-MS). Kaedah yang dibangun meliputi langkah pemisahan dan nilai
isian semula. Julat kelinearan dicapai antara 1.5 – 3000 μg/L dan 0.8 – 125 μg/L masing-masing
bagi prazosin dan simvastatin dengan nilai pekali (R2) > 0.99. Had kuantifikasi
(LOQ) bagi prazosin and simvastatin dihitung pada aras
2.1 dan 0.5 ng/L di dalam air ternyahion manakala direkod masing-masing pada aras 3.5 dan 2.4 ng/L di dalam sampel efluen. Dua jenis sebatian
farmaseutikal ini dikesan in dalam sampel larut lesap pada aras kepekatan
masing-masing adalah 3850 and 415 ng/L.
Kata kunci: prazosin, simvastatin, larut lesap, pengekstrakan
fasa pepejal, pencemaran farmaseutikal
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