Malaysian Journal of Analytical Sciences Vol 25 No 3 (2021): 432 - 445

 

 

 

 

CO₂-EFFERVESCENT TABLET-ASSISTED DISPERSIVE LIQUID-LIQUID MICROEXTRACTION WITH CENTRAL COMPOSITE DESIGN FOR PRE-CONCENTRATION OF ACETAMINOPHEN DRUG: METHOD DEVELOPMENT, VALIDATION AND GREEN ASSESSMENT PROFILE

 

(Tablet Berbuak-CO₂ Berbantukan Sebaran Pengekstrakan Mikro Cecair-Cecair dengan Reka Bentuk Komposit Berpusat untuk Kepekatan Awalan Dadah Acetaminophen: Pembangunan Kaedah, Validasi dan Profil Penilaian Hijau)

 

Priya Murugan, Sarveishwhary Rajendran, Saw Hong Loh, Marinah Mohd Ariffin, Wan Mohd Afiq Wan Mohd Khalik*

 

Faculty of Science and Marine Environment,

Universiti Malaysia Terengganu, 21030 Kuala Nerus, Malaysia

 

*Corresponding author:  wan.afiq@umt.edu.my

 

 

Received:  15 April 2021; Accepted: 2 June 2021; Published:  27 June 2021

 

 

Abstract

This study discovered the extraction procedure of acetaminophen from water samples using the effervescent tablet-assisted dispersive liquid-liquid microextraction (DLLME) method. The effervescent tablet that is composed of sodium dihydrogen phosphate (proton donor) and sodium carbonate (CO₂ source) was formulated using the wet granulation technique. In this study, high performance liquid chromatography coupled with ultraviolet visible detection (HPLC-UV) was used for qualitative and quantitative analysis of the targeted analyte. The chromatographic separation was conducted in less than 6 min (R_t 5.10 min) using a non-polar C₁₈ column and an isocratic elution (methanol: water of 40: 60 (v/v)) at a controlled flowrate of 1 mL min^-1. Optimum wavelength was set at 264 nm. Main variables that influenced the extraction efficiency namely the amount of extraction solvent (X₁), the number of tablets consumed (X₂) and the effect of extraction temperature (X₃) were tested during optimization work. Operation setting for extraction procedure was optimized using a 2³ full factorial central composite design, CCD (STATISTICA Version 10). The values of optimum extraction condition were set as 215 µL of extraction solvent, 5 pieces of tablets and 47 °C extraction temperature. Under optimal condition, a good linearity with determination coefficient R² = 0.995 was obtained. Extraction recoveries at spiked concentrations (500 ng mL^-1 and 100 ng mL^-1) were recorded ranging from 83% to 94.1%. The detection and quantification limits of the proposed method were calculated at 8.62 ng mL^-1 and 28 ng mL^-1, respectively. In terms of the precision method, the relative standard deviation was recorded ˂ 5%. Real analysis samples were performed, which fortified with commercial drugs dissolved in 80 mL of deionized water. The concentration levels were determined at 5.60 mg L^-1 (sample A) and 5.47 mg L^-1 (sample B) respectively.

 

Keywords:  analgesic drug, CO₂-effervescence, central composite design, liquid phase microextraction

 

 

Abstrak

Kajian ini meneroka prosedur pengekstrakan bagi acetaminophen dari sampel air mengunakan kaedah tablet berbuak berbantukan sebaran pengekstrakan mikro cecair-cecair (DLLME). Tablet berbuak terdiri dari sodium dihidrogen fosfat (penderma proton) dan sodium karbonat (sumber CO₂) di formulasi mengunakan teknik penggranulan basah. Dalam kajian ini, kromatografi cecair berprestasi tinggi gabungan pengesan ultralembayung nampak (HPLC-UV) telah digunapakai bagi analisis kuantitatif dan kualitatif terhadap analit sasaran. Pemisahan kromatografi berlaku dalam masa kurang 6 min (R_t 5.10 min) mengunakan turus tak berkutub C₁₈ dan elusi isokratik (metanol: air 40:60 (v/v)) pada kawalan aliran 1 mL min^-1. Panjang gelombang optimum ditetapkan pada 264 nm. Pemboleh ubah utama yang mempengaruhi keberkesanan pengekstrakan seperti jumlah pelarut pengekstrak (X₁), bilangan tablet yang digunakan (X₂) dan kesan perubahan suhu (X₃) diuji semasa kerja pengoptimuman. Tetapan operasi bagi prosedur pengekstrakan bagi pengoptimuman mengunakan reka bentuk komposit berpusat, CCD (STATISTICA versi 10). Nilai yang diperolehi bagi keadaan optimum ialah pelarut pengekstrakan 215 µL, 5 biji tablet dan tetapan suhu 47 °C. Kelinearan yang baik dengan pekali regresi R² = 0.995 telah diperolehi pada keadaan optimum. Perolehan semula pengekstrakan pada kepekatan yang dipaku (500 ng mL^-1 dan 100 ng mL^-1) telah merekodkan nilai julat 83%-94.1%. Had pengesanan dan pengkuantitian bagi kaedah yang dibangunkan dihitung masing-masing pada 8.62 ng mL^-1 dan 28 ng mL^-1. Bagi aspek kejituan kaedah, sisihan piawai relatif telah direkodkan < 5%. Analisis sampel sebenar telah dijalakan dengan penambahan dadah komersial yang dilarut dalam 80 mL air ternyah ion. Kepekatan telah ditentukan masing-masing pada 5.60 mg L^-1 (sampel A) dan 5.47 mg L^-1 (sampel B).

 

Kata kunci:  dadah analgesik, CO₂-berbuak, reka bentuk komposit berpusat, pengekstrakan mikro fasa cecair

 

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