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Sains Malaysiana 45(10)(2016):
1453–1459 Determination of Polycyclic Aromatic
Hydrocarbons in Beverage by Low Density Solvent Based-Dispersive
Liquid-Liquid Microextraction-High Performance Liquid Chromatography-Fluorescence
Detection (Penentuan Hidrokarbon Polisiklik Aromatik
dalam Minuman dengan Pengekstrakan Cecair-Cecair Serakan Berdasarkan
Pelarut Berketumpatan Rendah-Kromatografi Cecair Prestasi Tinggi-Pengesanan
Pendarfluor) SAW HONG
LOH1,2*,
YU
TING
CHONG1,
KHAIRUN
NISA
NOR
AFINDI1
& NORSHIMA ABDULLAH KAMARUDDIN1 1School of Marine
and Environmental Sciences, Universiti Malaysia Terengganu, 21030
Kuala Terengganu, Terengganu Darul Iman, Malaysia 2Institute of Marine
Biotechnology, Universiti Malaysia Terengganu, 21030 Kuala Terengganu,
Terengganu Darul Iman, Malaysia Diserahkan: 17 Ogos 2015/Diterima:
16 Februari 2016 ABSTRACT A simple and fast dispersive
liquid-liquid microextraction (DLLME) technique using organic
solvent lighter than water has been developed for the extraction
of selected polycyclic aromatic hydrocarbons in green tea, chrysanthemum
tea and coffee beverage. The 1-octanol and acetonitrile were pre-mixed
and injected into the sample solution. After dispersing, the cloudy
solution was subjected to centrifugation to separate the solution
into 2 phases, where the micro-droplet of 1-octanol was clearly
floated on the top layer. The 1-octanol extract was then diluted
and injected into high performance liquid chromatography-fluorescence
for the quantitative analysis. The technique offered rapid analysis
as the 1-octanol was homogeneously dispersed in the sample solution
thus speeding the analytes diffusion. Under the optimized extraction
conditions, the technique achieved trace detection limits in the
range of 0.001 to 0.3 μgL-1 for the targeted analytes,
namely phenanthrene, fluoranthene and benzo[a]pyrene. The method
was successfully applied to the spiked green tea, chrysanthemum
tea and coffee beverage samples with good average relative recoveries
obtained in the range of 86.7 to 103.0%. The utilization of low
density organic solvent as extraction solvent has allowed for
easier operation and eliminated the use of hazardous halogenated
solvent that is commonly applied in DLLME.
Keywords: Beverage; dispersive
liquid-liquid microextraction; high performance liquid chromatography-fluorescence
detection; low density solvent; polycyclic aromatic hydrocarbons ABSTRAK Suatu teknik pengekstrakan
cecair-cecair serakan (DLLME) yang mudah dan cepat menggunakan
pelarut organik berketumpatan lebih rendah daripada air telah
dibangunkan untuk mengekstrak hidrokarbon polisiklik aromatik
terpilih dalam minuman teh hijau, teh kekwa dan kopi. 1-oktanol
dan asetonitril dipracampur dan disuntik ke dalam larutan sampel.
Selepas penyerakan, larutan yang kabur tertakluk kepada pengemparan
untuk mengasingkan larutan kepada 2 fasa, dengan titisan mikro
1-oktanol terapung dengan jelas pada lapisan atas. Ekstrak 1-oktanol
seterusnya dicairkan dan disuntik ke dalam kromatografi cecair
prestasi tinggi-pendarfluor untuk analisis kuantitatif. Teknik
ini menawarkan analisis yang cepat kerana 1-oktanol diserakkan
dengan homogen dalam larutan sampel yang seterusnya mempercepatkan
resapan analit. Dalam keadaan pengekstrakan yang optima, teknik
ini mencapai had pengesanan dalam lingkungan 0.001 to 0.3 μgL-1 untuk analit sasaran, iaitu fenantrena,
fluorantena dan benzo[a]pirena. Kaedah ini berjaya diaplikasikan
kepada sampel minuman teh hijau, teh kekwa dan kopi yang dipakukan
dengan analit sasaran dengan perolehan semula purata yang baik
dalam lingkungan 86.7 to 103.0%. Penggunaan pelarut organik berketumpatan
rendah telah membolehkan operasi yang lebih mudah dan menyingkirkan
penggunaan pelarut berhalogen yang berbahaya dan biasa digunakan
dalam DLLME. Kata kunci: Hidrokarbon polisiklik aromatik; kromatografi cecair
prestasi tinggi-pengesanan pendarfluor; minuman; pelarut berketumpatan
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