Malaysian Journal of Analytical Sciences Vol 24 No 1 (2020): 33 - 41

 

 

 

 

AGAROSE-CHITOSAN-INTERGRATED MULTIWALLED CARBON NANOTUBES FILM SOLID PHASE MICROEXTRACTION COMBINED WITH HIGH PERFORMANCE LIQUID CHROMATOGRAPHY FOR THE DETERMINATION OF TRICYCLIC ANTIDEPRESSANT DRUGS IN AQUEOUS SAMPLES

 

(Filem Agarosa-Kitosan Bersepadu Nanotiub Kabon Berbilang Dinding Pengestrakan Mikro Fasa Pepejal Digabungkan Dengan Kromatografi Cecair Prestasi Tinggi-Pengesanan Ultralembayung Untuk Penentuan Anti-Murung Trisiklik Di Dalam Sampel Akueus)

 

Wan Nazihah Wan Ibrahim¹*, Mohd Marsin Sanagi², Nor Suhaila Mohammad Hanapi¹, Nursyamsyila Mat Hadzir¹, Noorfatimah Yahaya³, Sazlinda Kamaruzaman⁴

 

¹Faculty of Applied Science,

Universiti Teknologi MARA, 40450 Shah Alam, Selangor, Malaysia

²Department of Chemistry, Faculty of Science,

Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor, Malaysia

³Integrative Medicine Cluster, Advanced Medical and Dental Institute,

Universiti Sains Malaysia, 13200 Kepala Batas, Penang, Malaysia

⁴Department of Chemistry, Faculty of Science,

Universiti Putra Malaysia, 43400 Serdang, Selangor, Malaysia

 

*Corresponding author: wannazihah@uitm.edu.my

 

 

Received: 20 November 2019; Accepted: 15 January 2020

 

 

Abstract

Agarose-chitosan-integrated multiwalled carbon nanotubes (Agr-Ch-MWCNTs) film solid phase microextraction (SPME) was developed and applied for the determination of tricyclic antidepressant drugs (TCAs) in aqueous samples using high performance liquid chromatography-ultraviolet detection (HPLC-UV). Integration of highly interconnected pores of MWCNTs in the agarose-chitosan matrix increases the hydrophobic sites, surface area and porosity of the materials and thus enhancing the extraction efficiency. The film of blended agarose and chitosan allows good dispersion of MWCNTs, prevents the leaching of MWCNTs during application and enhances the film mechanical stability. Optimized parameters for SPME parameters were obtained which no addition of salt included, sample pH = 11, 30 minutes extraction time, iso-propanol as desorption solvent and 0.4% w/v MWCNTs loading in agarose-chitosan matrix. The matrix match calibration curves demonstrated good linearity in the range of 10-500 ppb with excellent coefficients determination (r² = 0.9944-0.9961), good limits of detection (LODs) in the range of 3.13-3.60 ppb, high analyte recoveries (92.04-110.00%) and low relative standard deviations (RSD < 6.85).

 

Keywords:    blended agarose/chitosan/multiwalled carbon nanotubes, solid phase microextraction, tricyclic antidepressant drugs

 

Abstrak

Filem agarosa-kitosan bersepadu nanotiub kabon berbilang dinding  (Agr-Ch-MWCNTs) pengestrakan mikro fasa pepejal (SPME) telah dibangunkan dan diaplikasi untuk penentuan anti-murung trisiklik di dalam sampel akueus menggunakan kromatografi cecair prestasi tinggi-pengesanan ultralembayung  (HPLC-UV). Persepaduan MWCNTs yang mempunyai liang yang saling berhubung di dalam matriks agarosa/kitosan menambahbaik tapak hidrofobik, luas permukaan dan keliangan bahan dan meningkatkan kecekapan pengestrakan. Filem campuran agarosa dan kitosan membenarkan penyerakan MWCNTs yang baik, menghalang pelunturan MWCNTs semasa aplikasi dan meningkatkan kestabilan mekanikal filem.  Optimum parameter untuk SPME telah diperolehi termasuk tiada penambahan garam, pH sampel = 11, masa pengestrakan 30 minit, iso-propanol sebagai pelarut desorpsi dan 0.4% w/v  jumlah muatan MWCNTs di dalam matrik agarosa/kitosan. Lengkungan kalibrasi matrik menunjukkan kelinearan yang bagus di dalam skala 10-500 ppb dengan penentuan koefisien yang terbaik (r² = 0.9944-0.9961), had pengesanan yang bagus (LODs) di dalam skala 3.13-3.60 ppb, perolehan semula yang tinggi (92.04-110.00%) dan sisihan piawai relatif yang rendah (RSD < 6.85).

 

Kata kunci:  campuran agarosa/kitosan/nanotiub karbon berbilang dinding, pengestrakan mikro fasa pepejal, anti-murung trisiklik

 

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