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Sains Malaysiana 55(8)(2026): 1363-1371
http://doi.org/10.17576/jsm-2026-5508-11
Analisis Residu 2-Fenilfenol dan 4-Fenilfenol dalam Buah Sitrus
Menggunakan Kaedah Pengekstrakan Mikro Cecair-Cecair Tersebar (DLLME) dan
Spektrofotometri Ultraungu-Boleh Nampak (UV-VIS)
(Analysis of 2-Phenylphenol and 4-Phenylphenol Residues in Citrus Fruits
Using Dispersed Liquid-Liquid Micro-Extraction (DLLME) and Ultraviolet-Visible
Spectrophotometry (UV-VIS)
NUR ALIFFAH ANISSA BINTI MOHD FAUZI,
NADHIRATUL-FARIHIN BINTI SEMAIL* & FAIQ HAFIY BIN ROZEMAN
Jabatan Sains
Kimia, Fakulti Sains dan Teknologi, Universiti Kebangsaan Malaysia, 43600 UKM
Bangi, Selangor, Malaysia
Received: 18 May 2026/Accepted: 16 August 2026
Abstrak
Antioksidan fenol merupakan antara unsur yang banyak terdapat dalam buah-buahan yang memberikan pelbagai manfaat kesihatan kepada pengguna. Bagi menentukan kandungan dan taburan 2- dan 4-fenilfenol dalam lima jenis jus buah sitrus, satu kaedah yang pantas, sensitif serta mesra alam iaitu pengekstrakan mikro cecair-cecair secara serakan (DLLME) telah digunakan di bawah keadaan optimum pH 5, 1.5 g NaCl, 1.5 mL isopropanol sebagai pelarut penyebar dan 1.2 mL diklorometana sebagai pelarut pengekstrak. Analisis preliminari menggunakan kromatografi lapisan nipis (TLC) dengan menggunakan toluena dan aseton (8:2) sebagai pelarut fasa bergerak telah dijalankan bagi penvisualisasi 2 dan 4-fenilfenol di bawah cahaya ultraungu. Namun begitu, disebabkan kedua-dua analit mempunyai kepekatan yang sangat rendah, ia tidak dapat dikesan melalui kaedah TLC. Ujian DPPH tidak menunjukkan perubahan
warna yang signifikan, yang menunjukkan bahawa kepekatan antioksidan dalam
sampel sitrus mungkin terlalu rendah untuk dinilai secara berkesan menggunakan
kaedah ini tanpa proses prapekatan sampel. Oleh itu, kaedah kuantifikasi menggunakan
DLLME dan spektrofotometer UV-Vis pada panjang gelombang 245 dan 287 nm telah dijalankan. Jus lemon menunjukkan kepekatan 2- dan 4-fenilfenol yang tertinggi antara kelima-lima sampel buah dengan nilai 0.0212 dan 0.0371 mg/mL masing-masing bagi 2 dan 4-fenilfenol. Keputusan menunjukkan kedua-dua analit mempunyai pekali kolerasi linear (R²) 0.9917 dan 0.9899. Had pengesanan (LOD) dan had pengkuantifikasian (LOQ) masing-masing adalah 0.00119 dan 0.00408 bagi 2-fenilfenol manakala 0.00127 dan 0.00436 bagi 4-fenilfenol. Peratusan penghasilan semula adalah dari 85.92 sehingga 105.5% bagi 2-fenilfenol dan 90.30 sehingga 114.8% bagi 4-fenilfenol dengan sisihan piawai relatif harian (RSD) 0.1977 hingga 0.5189. Kaedah ini telah berjaya digunakan untuk analisis sampel sebenar jus buah dan membuktikan bahawa teknik ini adalah teknik yang ringkas, pantas dan praktikal serta mesra alam.
Kata kunci: Antioksidan fenol; buah sitrus; DLLME; UV-Vis; TLC
Abstract
Phenolic antioxidants
are among the many compounds found in fruits that offer various health benefits
to consumers. To determine the content and distribution of 2- and 4- phenylphenol in five types of citrus fruit juices, a rapid,
sensitive, and environmentally friendly method, dispersive liquid-liquid
microextraction (DLLME) was employed under optimized conditions: pH 5, 1.5 g of
NaCl, 1.5 mL of isopropanol as the disperser solvent, and 1.2 mL of
dichloromethane as the extractant solvent. A preliminary analysis was conducted
using thin-layer chromatography (TLC) with toluene and acetone (8:2) as the
mobile phase solvent to visualize 2- and 4-phenylphenol under ultraviolet
light. However, due to the very low concentrations of both analytes, they could
not be detected by TLC. The DPPH assay also did not exhibit a significant
colour change, suggesting that the antioxidant compounds in the citrus sample
may be present at concentrations too low for effective detection using this
method without prior sample pre-concentration. Therefore, quantification was
carried out using UV-Vis spectrophotometry at wavelengths of 245 and 287 nm.
Lemon juice showed the highest concentrations among the five fruit juice
samples, with values of 0.0212 and 0.0371 mg/mL for 2- and 4-phenylphenol,
respectively. The results showed that both analytes had linear correlation
coefficients (R²) of 0.9917 and
0.9899. The limits of detection (LOD) and quantification (LOQ) were 0.00119 and
0.00408 for 2-phenylphenol, and 0.00127 and 0.00436 for 4-phenylphenol,
respectively. The recovery percentages ranged from 85.9 to 105.5% for
2-phenylphenol and 90.3 to 114.8% for 4-phenylphenol, with daily relative
standard deviations (RSD) ranging from 0.1977 to 0.5189. This method was
successfully applied to the analysis of real fruit juice samples and
demonstrated that it is a simple, rapid, practical, and environmentally
friendly technique.
Keywords: Citrus
fruit; DLLME; phenolic antioxidant; TLC; UV-Vis
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*Corresponding author; email:
nadhiratulfarihin@ukm.edu.my
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