Malaysian Journal of Analytical Sciences Vol 19 No 3 (2015): 574 – 585

 

 

 

SELECTIVE SURFACE CHARACTERISTICS AND EXTRACTION PERFORMANCE OF A NITRO-GROUP EXPLOSIVE MOLECULARLY IMPRINTED POLYMER

 

(Karekter Permukaan yang Selektif dan Prestasi Pengekstrakan Kumpulan Nitro Peletup Polimer Molekul Tercetak)

 

Marinah Mohd Ariffin¹*, Norhafiza Ilyana Yatim¹, Norhayati Mohd Tahir^1,2

 

¹School of Marine and Environmental Sciences,

²Institute of Oceanography,

Universiti Malaysia Terengganu, 21300 Kuala Terengganu, Malaysia

 

*Corresponding author:  erin@umt.edu.my

 

 

Received: 21 January 2015; Accepted: 5 April 2015

 

 

Abstract

A novel molecularly imprinted polymer (MIP) was synthesized as a highly selective and specific sorbent for solid phase extraction (SPE) of 2,4,6-trinitrotoluene (TNT). TNT-MIP was prepared by bulk polymerisation process using 2,4,6-trinitrotoluene (TNT) as template, methacrylic acid (MAA) as the functional monomer and ethylene glycol dimethylacrylate (EGDMA) as the cross-linker. Non-imprinted polymer (NIP) was prepared under the similar procedure but without the addition of template as a control polymer. Prior to analysis, the polymer monoliths were ground and sieved in the range of 25-38 µm before incorporated as SPE sorbent. The TNT-MIP and NIP performance validation were analysed by high performance liquid chromatography (HPLC) at 254 nm of UV detector. The limit of detection (LOD) and limit of quantitation (LOQ) range were 0.03-0.07 µg/mL and 0.05-0.11 µg/mL, respectively. The MIP showed excellent selectivity towards the template, TNT with percentage recovery and RSD value, 94.1±13.7 compared to TNT’s metabolites, 4-amino-2,6-dinitrotoluene, 4-ADNT (31.7±27.2) and 2-amino-4,6-dinitrotoluene, 2-ADNT (41.2±6.1), respectively. The physical imprinting effect of MIP and NIP was characterized by using scanning electron microscopy (SEM) and Brunauer, Emmett and Teller (BET). Evaluation performance proved that the developed TNT-MIP was good in TNT selectivity and could be applied in real samples analysis.

 

Keywords: molecularly imprinted polymers, solid-phase extraction, 2,4,6-trinitrotoluene

 

Abstrak

Sebuah polimer molekul tercetak (MIP) baru telah disintesis sebagai pengerap yang sangat selektif dan khusus untuk pengekstrakan fasa pepejal (SPE) bagi 2,4,6- trinitrotoluena (TNT). TNT-MIP telah disediakan dengan proses pempolimeran pukal menggunakan 2,4,6- trinitrotoluena (TNT) sebagai templat, asid metakrilik (MAA ) sebagai monomer, etilena glikol dimetilakrilat (EGDMA) sebagai pemaut silang. Polimer molekul tidak-tercetak (NIP) telah disediakan bawah prosedur yang sama tetapi tanpa tambahan templat sebagai polimer kawalan. Sebelum analisis, polimer dihancurkan dan ditapis dalam lingkungan 25-38 μm sebelum dijadikan sebagai penjerap SPE. Pengesanan prestasi TNT-MIP dan NIP dianalisis oleh kromatografi cecair berprestasi tinggi (HPLC) pada 254 nm pengesan UV. Had pengesanan (LOD) dan had kuantitatif (LOQ) adalah, 0.03-0.07 μg/mL dan 0.05-0.11 μg/mL masing-masing . MIP menunjukkan pemilihan yang cemerlang ke arah templat, TNT dengan peratus pengembalian dan nilai RSD , 94.1 ± 13.7 berbanding metabolit TNT , 4-amina-2,6-dinitrotoluena , 4-ADNT ( 31.7 ± 27.2 ) dan 2-amina-4, 6-dinitrotoluena, 2-ADNT (41.2 ± 6.1). Kesan fizikal pencetakan MIP dan NIP dicirikan dengan menggunakan mikroskop imbasan elektron (SEM) dan Brunauer, Emmett dan Teller (BET). Penilaian prestasi membuktikan bahawa TNT-MIP yang dibangunkan bagus digunakan TNT pemilihan dan boleh digunakan dalam analisis sampel sebenar.

 

Kata kunci: polimer molekul tercetak, pengekstrakkan fasa pepejal, 2,4,6-trinitrotoluena

 

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