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Sains Malaysiana 50(1)(2021): 109-121
http://dx.doi.org/10.17576/jsm-2021-5001-12
Optimization
of Effervescent Tablet-Assisted Dispersive Liquid-Liquid Microextraction with Central Composite Design for Preconcentration of
Stimulant Drug
(Pengoptimuman Tablet Berbuak Berbantukan Sebaran Pengekstrakan Mikro Cecair-Cecair dengan Reka Bentuk Komposit Berpusat untuk Kepekatan Awalan Dadah Stimulan)
NURLIYANA TAZULAZHAR, SAW HONG LOH, MARINAH MOHD ARIFFIN
& WAN MOHD AFIQ WAN MOHD KHALIK*
Faculty
of Science and Marine Environment, Universiti Malaysia Terengganu, 21030 Kuala Nerus, Terengganu Darul Iman, Malaysia
Diserahkan: 18 Mei 2020/Diterima: 6 Julai 2020
ABSTRACT
The
extraction efficiency of stimulant drug, namely caffeine, was investigated
using a 23 central composite design. The values of optimum
extraction condition were set at 468 µL of 1-dodecanol, 1 piece of effervescent
tablet, and 22 °C of extraction temperature. An enrichment factor was
calculated as 72 for 80 mL water sample. The run time was conducted in less
than 6 min using a non-polar C18 column and an isocratic mobile
phase (methanol: water of 40:60 (v/v)) at a controlled flow rate of 1 mL min-1.
A good linear response was achieved in the range of 0.01-0.50 µg mL-1 (R2 > 0.998). Detection and quantification limits were calculated
at 0.009 and 0.015 µg mL-1, respectively. The average recoveries at
two spiking concentration levels were within the range of 75-105% with RSD <
2% (n = 3). Real samples namely beverages which contained caffeine and river
water were tested using the proposed method, and the results ranged 0.021-0.56
µg mL-1. The eco-scale score and green analytical procedure index
confirmed the greenness profile of the proposed method through a calculated
score of 88 and has 6 green criteria, respectively.
Keywords:
Pharmaceutically active compound; response surface methodology; stimulant drug
ABSTRAK
Keberkesanan pengekstrakan bagi jenis dadah perangsang,
iaitu kafein telah dikaji menggunakan 23 reka bentuk komposit
berpusat. Pada keadaan optimum, nilai parameter ditetapkan pada 468 µL 1-dodecanol, 1 tablet berbuak dan 22 °C suhu
pengekstrakan. Faktor pengayaan dihitung pada nilai 72 bagi 80 mL sampel air.
Waktu eksekusi dijalankan kurang dari 6 minit menggunakan turus tak berkutub C18 dan fasa bergerak isokratik (metanol: air pada 40:60 (v/v)) pada kadar aliran
terkawal 1 mL min-1. Respons kelinearan yang baik telah dicapai dalam julat
0.01-0.50 µg mL-1 (R2> 0.998). Had pengesanan dan
pengkuantitian telah dihitung masing-masing pada 0.009 dan 0.015 µg mL-1. Purata perolehan semula pada
dua aras kepekatan sampel dipaku berada dalam julat 75-105% dengan nilai RSD
< 2% (n = 3). Analisis sampel sebenar iaitu minuman yang mengandungi kafein
dan air sungai telah diuji dengan kaedah yang dicadangkan dan keputusan yang
dihitung berada dalam julat 0.021-0.56 µg mL-1. Skor skala-eko dan
indeks prosedur analitis hijau telah mengesahkan profil hijau bagi kaedah yang
dicadangkan masing-masing dengan nilai skor yang dihitung ialah 88 dan 6
kriteria hijau.
Kata kunci: Dadah perangsang; kaedah gerak balas permukaan; sebatian aktif farmaseutis
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*Pengarang untuk surat-menyurat; email: wan.afiq@umt.edu.my
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