Malaysian Journal of Analytical Sciences Vol 19 No 2 (2015): 325 – 337

 

 

 

MICROPOROUS CARBON SPHERES SOLID PHASE MEMBRANE TIP EXTRACTION FOR THE ANALYSIS OF NITROSAMINES IN WATER SAMPLES

 

(Pengekstrakan Muncung Membran Fasa Pepejal Sfera Karbon Berliang Mikro bagi Analisis Nitrosamin di dalam Sampel Air)

 

Mohammed Salisu Musa^1,3, Mohd Marsin Sanagi^{1,2 *}, Hadi Nur² , Wan Aini Wan Ibrahim¹

 

¹Department of Chemistry, Faculty of Science,

Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

²Ibnu Sina Institute for Fundamental Science Studies, Nanotechnology Research Alliance,

Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia

³Department of Pure and Industrial Chemistry, Faculty of Science,

Bayero University Kano, Nigeria.

 

*Corresponding author: marsin@kimia.fs.utm.my

 

 

Received: 20 November 2014; Accepted: 5 January 2015

 

 

Abstract

A simple solid phase membrane tip extraction (SPMTE) utilizing microporous carbon spheres (MCS) was developed for the analysis of nitrosamines in aqueous samples. The method termed MCS-SPMTE was optimized for various important extraction parameters namely conditioning organic solvent, extraction time, effects of salt addition and pH change, desorption time, desorption solvent and sample volume. Under the optimized conditions, the method indicated good linearity in the range of 10-100 µg/L with coefficients of determination, r² ≥ 0.9984. The method also demonstrated good reproducibility with %RSDs values ranging from 2.2 – 8.9 (n = 3). Limit of detection (LOD) and limit of quantification (LOQ) for the method ranged from 3.2 - 4.8 µg/L and      10.9 – 15.9 µg/L respectively. Recoveries for both tap-water and lake water samples spiked at 10 µg/L were in the range of 83.2 - 107.5%.

 

Keywords: hydrothermal reaction, microporous carbon spheres, nitrosamines, solid phase membrane tip extraction, gas chromatography mass spectrometry

 

Abstrak

Pengekstrakan muncung membrane fasa pepejal yang ringkas menggunakan sfera karbon berliang (MCS) telah dibangunkan bagi analisis nitrosamina di dalam sampel akues. Kaedah yang dikenali sebagai MCS-SPMTE telah dioptimumkan bagi pelbagai parameter penting iaitu pengkondisi pelarut organik, masa pengekstrakan, kesan penambahan garam dan perubahan pH, masa penyahjerapan, pelarut penyahjerap dan isipadu sampel. Di bawah keadaan optimum, kaedah ini menunjukkan kelinearan yang baik dalam julat 10-100 µg/L dengan koefisien penentuan, r² ≥ 0.9984. Kaedah itu juga menunjukkan kebolehulangan yang baik dengan nilai %RSDs dalam julat 2.2 – 8.9 (n = 3). Had pengesanan (LOD) dan had penentuan (LOQ) bagi kaedah itu adalah masing-masing di antara 3.2 - 4.8 µg/L dan 10.9 – 15.9 µg/L. Perolehan semulabagi sampel air paip dan air tasik yang dimasukkan kepekatan yang diketahui 10 µg/L adalah dalam julat 83.2 - 107.5%.

 

Kata kunci: tindak balas hidroterma, sfera karbon berliang mikro, nitrosamina, pengekstrakan muncung membran fasa pepejal, kromatografi gas-spektrometri jisim

 

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