Malaysian Journal of Analytical Sciences Vol 24 No 1 (2020): 53 - 61

 

 

 

 

APPLICATION OF MICROWAVE-ASSISTED EXTRACTION COUPLED WITH DISPERSIVE LIQUID-LIQUID MICROEXTRACTION FOR THE DETERMINATION OF POLYCYCLIC AROMATIC HYDROCARBONS IN VEGETABLES

 

(Aplikasi Pengekstrakan Berbantukan Mikrogelombang Gandingan dengan Pengekstrakan Mikro Cecair-Cecair Serakan bagi Penentukan Hidrokarbon Aromatik Polisiklik dalam Sayur-Sayuran)

 

Chai Mee Kin¹*, Tan Yeong Hwang¹, Wong Ling Shing²

 

¹College of Engineering,

Universiti Tenaga Nasional, Jalan Ikram-Uniten, 43000 Kajang, Selangor, Malaysia

²Faculty of Health and Life Science,

INTI International University, Persiaran Perdana BBN, Putra Nilai, 71800 Nilai, Negeri Sembilan, Malaysia

 

*Corresponding author:  mkchai@uniten.edu.my

 

 

Received: 20 November 2019; Accepted: 21 January 2020

 

 

Abstract

Microwave-assisted extraction (MAE) coupled with dispersive liquid-liquid microextraction (DLLME) followed by gas- chromatography flame ionization detector (GC-FID) for the determination of 13 PAHs in vegetable samples was developed in this study. The analytical performances of the optimized DLLME and MAE-DLLME including limit of detection (LOD), limit of quantification (LOQ), precision, accuracy, relative extraction recovery and relative extraction factor were validated and compared. The LOD of DLLME and MAE-DLLME were in the range of 0.040-0.400 and 0.0200-0.080 µg/L, respectively. For DLLME, precision and accuracy were 1.22-7.50% (RSD) and 71.77% to 90.93%, respectively; while for MAE-DLLME, were 0.77%-3.07% (RSD) and 83.65-98.42%, respectively. The relative extraction recovery was improved from 70.81% – 85.41% in DLLME to 85.79% - 99.61% in MAE-DLLME. The relative enrichment factors were ranged from 126-156 and 165 to 202 for DLLME and MAE-DLLME, respectively. The volume of extraction solvent was reduced from 50 µL to 30 µL in MAE- DLLME. The overall analytical performances of MAE-DLLME is better than DLLME. The application of proposed MAE- DLLME in real samples was also investigated and discussed.

 

Keywords: dispersive liquid-liquid microextraction, microwave-assisted extraction, polycyclic aromatic hydrocarbons, extraction solvent

 

Abstrak

Pengekstrakan berbantukan mikrogelombang (MAE) gandingan dengan pengekstrakan mikro cecair-cecair serakan (DLLME) yang diikuti dengan gas kromatografi-pengesan nyalaan ion (GC-FID) bagi penentukan 13 jenis hidrokarbon aromatik polisiklik (PAHs) dalam sampel sayur-sayuran telah dibangunkan dalam kajian ini. Analisis prestasi optimum DLLME dan MAE-DLLME seperti had pengesanan (LODs), kepersisan, kejituan, perolehan semula pengekstrakan secara relatif dan faktor-faktor pengayaan secara relatif telah disahkan dan dibandingkan. Had pengesanan (LODs) bagi DLLME dan MAE-DLLME adalah dalam lingkungan 0.040-0.400 dan 0.0200-0.080 μg/L, masing-masing. Bagi DLLME, kepersisan dan kejituan adalah dalam lingkungan 1.22-7.50% dan 71.77-90.93%, masing-masing; manakala bagi MAE-DLLME, adalah dalam lingkungan 0.77-3.07% dan 83.65-98.42%, masing-masing. Perolehan semula pengekstrakan secara relatif telah ditingkatkan daripada 70.81-85.41% pada DLLME hingga 85.79 - 99.61% pada MAE-DLLME. Faktor-faktor pengayaan secara relatif adalah 126-156 dan 165-202 bagi DLLME dan MAE-DLLME, masing-masing.  Jumlah  pengekstrakan pelarut yang digunakan telah dikurangkan daripada 50 μL di DLLME kepada 30 μL di MAE-DLLME. Prestasi keseluruhan analisis MAE-DLLME adalah lebih baik daripada DLLME. Penggunaan MAE-DLLME dalam analisis sampel sebenar juga disiasat dan dibincangkan.

 

Kata kunci: pengekstrakan mikro cecair-cecair serakan, pengekstrakan berbantukan mikrogelombang, hidrokarbon aromatik polisiklik, pelarut pengekstrakan

 

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