Malaysian Journal of Analytical Sciences Vol 24 No 6 (2020): 882 - 892

 

 

 

 

DETERMINATION OF PHENANTHRENE AND FLUORANTHENE IN RICE SAMPLES BY ACTIVATED CARBON-BASED DISPERSIVE SOLID PHASE MICRO-EXTRACTION COUPLED WITH GAS CHROMATOGRAPHY-FLAME IONIZATION DETECTOR ANALYSIS

 

(Penentuan Phenantrena dan Fluorantena dalam Sampel Beras Menggunakan Pengekstrakan Mikro Fasa Pepejal Berserak Berasaskan Karbon Diaktifkan Bersama Analisis Pengesan Pengionan Nyalaan-Kromatografi Gas)

 

Nurul Nadjwa Nahrowi1, Boon Yih Hui2, Mohamad Shariff Shahriman1, Noorfatimah Yahaya2, Nur Nadhirah Mohd Zain2, Saliza Asman3, Md Firoz Khan1, Kavirajaa Pandian Sambasevam4, Vuanghao Lim2, Muggundha Raoov1,5*

 

1Department of Chemistry, Faculty of Science,

Universiti Malaya, 50603 Kuala Lumpur, Malaysia

2Integrative Medicine Cluster, Advanced Medical & Dental Institute,

Universiti Sains Malaysia, 13200 Pulau Pinang, Malaysia

3Department of Physics and Chemistry, Faculty of Applied Sciences and Technology, Pagoh Education Hub,

Universiti Tun Hussein Onn Malaysia, 84000 Pagoh, Muar, Johor, Malaysia

4School of Chemistry and Environment, Faculty of Applied Sciences,

Universiti Teknologi MARA, Negeri Sembilan Branch, Kuala Pilah Campus, 72000 Kuala Pilah, Negeri Sembilan, Malaysia

5Universiti Malaya Centre for Ionic Liquids (UMCIL), Department of Chemistry, Faculty of Science,

Universiti Malaya, 50603 Kuala Lumpur, Malaysia

 

*Corresponding author:  muggundha@um.edu.my

 

 

Received: 12 August 2020; Accepted: 20 October 2020; Published:  10 December 2020

 

 

Abstract

A simple dispersive solid phase micro-extraction (DSPME) based on activated carbon (AC) was performed for the determination and separation of carcinogenic polycyclic aromatic hydrocarbons (PAHs), namely phenanthrene and fluoranthene, in selected white, brown and parboiled rice samples. The extraction was coupled with gas chromatography-flame ionization detector (GC-FID) for analysis. Under the optimized conditions [amount of adsorbent (5 mg), sample volume (40 mL), type (dichloromethane), and volume of desorption solvent (300 µL)], calibration curves were found to be linear for the concentration between 10 and 1000 µg kg-1 with coefficient of determination (R2) from 0.9938 to 0.9955. The limit of detection (LOD) and limit of quantification (LOQ) were in the range of 0.11 - 0.15 µg kg-1 and 0.33 - 0.46 µg kg-1, respectively. Relative standard deviation (RSD) was less than 8.02% and 5.48% for intra-day (n = 5) and inter-day (n = 5) for the present method, respectively. High pre-concentration factor (2587 - 2866) and satisfactory recoveries (90.23 - 115.63%) were also achieved. The proposed method was found to be simple, rapid and reliable for the monitoring of PAHs in rice samples.

 

Keywords:   dispersive solid phase micro-extraction, activated carbon, polycyclic aromatic hydrocarbons, rice samples

 

Abstrak

Pengekstrakan mikro fasa pepejal berserak (DSPME) yang mudah berasaskan karbon diaktifkan (AC) telah dijalankan untuk penentuan dan pengasingan hidrokarbon polisiklik aromatik (PAHs) yang boleh menyebabkan barah iaitu phenantrena dan fluorantena dalam sampel beras putih, perang dan pra-rebus yang terpilih. Pengekstrakan dijalankan bersama dengan - kromatografi gas - pengesan pengionan nyalaan (GC-FID) untuk analisis. Dalam keadaan optimum [jumlah penyerapan (5 mg), jumlah isipadu sampel (40 mL) dan jenis serta jumlah isipadu pelarut penyerapan (diklorometana, 300 µL)], keluk penentukuran didapati bergerak lurus untuk kepekatan antara 10 dan 1000 µg kg-1 dengan pekali penentuan (R2) daripada 0.9938 hingga 0.9955. Had pengesanan (LOD) dan had kuantifikasi (LOQ), masing-masing dalam julat 0.11 - 0.15 µg kg-1 dan 0.33 - 0.46 µg kg-1. Berdasarkan kaedah yang sekarang, sisihan piawai relatif (RSD) menunjukkan masing-masing kurang daripada 8.02% dan 5.48% untuk hari yang sama (n=5) dan antara hari (n=5). Faktor prakepekatan tinggi (2587 - 2866) dan pemulihan yang memuaskan (90.23 - 115.63%) juga dapat dicapai. Kaedah yang dicadangkan didapati mudah, cepat dan boleh dipercayai untuk pemantauan PAH dalam sampel beras.

 

Kata kunci:     pergekstrakan mikro fasa pepejal dispersif, karbon diaktifkan, hidrokarbon polisiklik aromatik, sampel beras

 

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