Malaysian Journal of Analytical Sciences, Vol 28 No 3 (2024): 694 - 710

 

MEMBRANE-PROTECTED MICRO-SOLID PHASE EXTRACTION OF CARCINOGENIC AROMATIC AMINES IN WATER SAMPLES PRIOR TO GC-FID ANALYSIS

 

(Pengekstrakan Fasa Pepejal Mikro Yang Dilindungi oleh Membran untuk Amin Aromatik Karsinogenik dalam Sampel Air dengan Analisis GC-FID)

 

Anjalee Pushpika Patabendi1, Mohamad Shariff Shahriman1, Hemavathy Surikumaran2, Nur Nadhirah Mohamad Zain3, Noorfatimah Yahaya3, Faizah Mohammad Yunus1, Usman Abdullahi Usman4, Kavirajaa Pandian Sambasevam5,6*, and Muggundha Raoov1*

 

1Department of Chemistry, Faculty of Science, Universiti Malaya, 50603 Kuala Lumpur, Malaysia

2Faculty of Bioeconomic, Food and Health Sciences, Universiti Geomatika Malaysia, 54200 Kuala Lumpur, Malaysia

3Department of Toxicology, Advanced Medical & Dental Institute, Universiti Sains Malaysia, 13200 Pulau Pinang, Malaysia

4Department of Geology, Faculty of Science, University of Maiduguri, P.M.B 1069, Maiduguri, Borno State, Nigeria.

5Advanced Materials for Environmental Remediation (AMER), Faculty of Applied Sciences, Universiti Teknologi MARA, Cawangan Negeri Sembilan, Kampus Kuala Pilah, 72000 Kuala Pilah, Negeri Sembilan, Malaysia

6Electrochemical Material and Sensor (EMaS) Group, Universiti Teknologi MARA, Shah Alam, 40450, Selangor, Malaysia

 

*Corresponding author: kavirajaa@uitm.edu.my, muggundha@um.edu.my

 

 

Received: 17 February 2024; Accepted: 16 April 2024; Published:  29 June 2024

 

 

Abstract

A simple method to extract aromatic amines in environmental water samples was developed using β-cyclodextrin-toluene diisocyanate (β-CD-TDI) polymer enclosed with tea bag filter paper fashioned as a micro-solid phase extraction (µ-SPE) device combined with GC-FID. In this study, an efficient sorbent (β-CD-TDI polymer) was successfully synthesised and characterizaed for the microextraction of aromatic amines such as p-Toluidine, 4-chloroaniline, 2-naphthylamine, and 4-aminobiphenyl using FTIR, FESEM and TGA. Under optimized conditions (40 mg of β-CD-TDI polymer in 5 mL sample volume with 75 min extraction time and desorption with 300 µL of acetonitrile under 30s desorption time), β-CD-TDI polymer was proven to be an effective adsorbent for the extraction of aromatic amines in environmental water samples with a satisfactory percentage recovery achieved from 80 to 99%. All the studied analytes showed good linearity in the range of 5 to 500 µg L-1 and the correlation of determination (R2) was from 0.9980 to 0.9990. The LODs obtained were from 1.67 to 3.18 µg L-1, and LOQs were from 5.05 to 9.63 µg L-1. This method gives precision values for both intra- and inter-day within accepted variable limits (<15% of RSD). The self-made cellulose-based μ-SPE device revealed that it can be simply prepared, easy to operate, reusable, cost-effective, reduce chemical consumption during extraction, and additionally speed up the extraction process, making it more efficient.

 

Keywords: µ-SPE, β-cyclodextrin-toluene diisocyanate, aromatic amines, GC-FID, environmental water

 

 

Abstrak

Satu kaedah mudah untuk mengekstrak amin aromatik dalam sampel air alam sekitar telah dibangunkan menggunakan polimer β-siklodextrin-toluen diisosiyanat (β-CD-TDI) yang dilingkungi dengan kertas penapis beg teh yang dihasilkan sebagai peranti pengekstrakan fasa pepejal mikro (µ-SPE) yang digabungkan dengan GC-FID. Dalam kajian ini, penyerap yang berkesan (polimer β-CD-TDI) berjaya disintesis dan dicirikan untuk pengeluaran mikro amin aromatik seperti p-Toluidin, 4-kloroanilin, 2-naftilamina, dan 4-aminobifenil menggunakan FTIR, FESEM, dan TGA. Di bawah syarat yang dioptimumkan (40 mg polimer β-CD-TDI dalam 5 mL isipadu sampel dengan masa pengekstrakan 75 minit dan desorpsi dengan 300 µL asetonitril dalam masa desorpsi 30 saat), polimer β-CD-TDI terbukti menjadi penjerap yang berkesan untuk pengekstrakan amin aromatik dalam sampel air alam sekitar dengan perolehan peratusan yang memuaskan mencapai dari 80 hingga 99 %. Semua analit yang dikaji menunjukkan lineariti yang baik dalam julat 5 hingga 500 µg L-1 dan korelasi penentuan (R2) adalah dari 0.9980 hingga 0.9990. LOD yang diperolehi adalah dari 1.67 hingga 3.18 µg L-1, dan LOQ adalah dari 5.05 hingga 9.63 µg L-1. Kaedah ini memberikan nilai ketepatan untuk kedua-dua intraday dan inter-day dalam had batas variabel yang diterima (<15 % daripada RSD). Peranti µ-SPE berbahan selulosa buatan sendiri menunjukkan bahawa ia boleh disiapkan dengan mudah, mudah beroperasi, boleh digunakan semula, berkos rendah, mengurangkan penggunaan bahan kimia semasa pengekstrakan, dan tambahan pula mempercepatkan proses pengekstrakan, menjadikannya lebih cekap.

 

Kata Kunci: µ-SPE, β-siklodekstrin-toluena diisosiyanat, amin aromatik, GC-FID, air persekitaran

 

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