Malaysian
Journal of Analytical Sciences Vol 21 No 1 (2017): 95 - 104
DOI:
http://dx.doi.org/10.17576/mjas-2017-2101-11
DETERMINATION OF CAFFEINE IN SURFACE WATER USING
SOLID PHASE EXTRACTION AND HIGH PERFOMANCE LIQUID
CHROMATOGRAPHY
(Penentuan Kafien di Permukaan Air
Mengunakan Pengekstrakan Fasa Pepejal dan Kromatografi Cecair Prestasi
Tinggi)
Fouad Fadhil Al-Qaim1,2*, Siti
Hasmah Jusof1, Md Pauzi Abdullah1,3, Zainab Haider Mussa1,
Nurfaizah Abu Tahrim1, Wan Mohd Afiq Wan
Mohd Khalik1, Mohamed Rozali Othman1,3
1School of Chemical Sciences and Food Technology,
Faculty of Science and Technology,
Universiti
Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia
2Chemistry Department, 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 UKM Bangi, Selangor, Malaysia
*Corresponding author: fouadalkaim@yahoo.com
Received: 9
April 2016; Accepted: 8 October 2016
Abstract
A
new analytical method development based on solid phase extraction (SPE)
combined with high performance liquid chromatography (HPLC) was carried out.
The optimum working conditions were obtained based on selection of 250 mL
sample loading, 0.25 µL methanol as reconstitution solvent, 100% methanol as
mobile phase and 270 nm as the optimum wavelength. Good linearity was obtained
in the range of 0.015 – 400 mg/L and the regression coefficient, R2,
was 0.995. Limit of detection and quantification were calculated at LOD = 0.06
µg/L and LOQ = 0.2 µg/L respectively. Repeatability and robustness has showed
good performance with low relative standard deviation less than 3.29% and 3.50%
respectively. Time-of-flight mass spectrometry (TOF/MS) instrument was used to confirm
that caffeine is definitely present in surface water with level of concentration
ranged from 31.7 to 50.1 µg/L. All results were analyzed statistically using one-way
ANOVA, Tukey with interval confidence 95% and P-value 0.05.
Keywords: caffeine,
stimulant, emerging pollutant, water quality, time of flight/mass spectrometry
Abstrak
Pembangunan kaedah analisis baru berasaskan pengekstrakan
fasa pepejal bersama kromatografi cecair prestasi tinggi (KPCT) telah
dijalankan. Kaedah optimum diperolehi berdasarkan tetapan iaitu 250 mL muatan
sampel, 0.25 µL metanol sebagai pelarut, 100% methanol sebagai fasa bergerak
dan 270 nm panjang gelombang yang optimum. Nilai kelinearan baik diperolehi
pada julat kepekatan 0.015 – 400 mg/L dan nilai pekali regresi, R2
ialah 0.995. Had pengesanan dan kuantifikasi dihitung masing – masing pada LOD
= 0.06 µg/L and LOQ = 0.2 µg/L. Kebolehulangan dan keteguhan kaedah menunjukkan
prestasi baik dengan nilai sisihan piawai relatif yang rendah iaitu masing –
masing kurang daripada 3.29% dan 3.50%. Spektrometri jisim masa penerbangan
(TOF/MS) digunakan untuk mengesahkan kehadiran kafein di permukaan air dengan
aras kepekatan antara julat 31.7 hingga 50.1 µg/L. Keputusan dianalisa
mengunakan pendekatan statistik seperti ANOVA satu hala, Tukey dengan aras
keyakinan 95% and nilai p 0.05.
Kata kunci: kafein,
perangsang, pencemar baru, kualiti air, spektrometri jisim/masa penerbangan
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