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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 Received: 17 August 2015/Accepted:
16 February 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;
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2-10. *Corresponding author; email: lohsh@umt.edu.my
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