Malaysian Journal of Analytical Sciences Vol 18 No 3 (2014): 534 - 543

 

 

 

SEPARATION OF N-NITROSAMINES BY MICELLAR ELECTROKINETIC CHROMATOGRAPHY

 

(Pemisahan N-Nitrosamina Menggunakan Kromatografi Elektrokinetik Misel)

 

Nur Amira Md Ali¹, Mohd Marsin Sanagi^1,2*, Wan Aini Wan Ibrahim¹

 

¹Department of Chemistry, Faculty of Science,

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

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

 

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

 

 

Abstract

A simple and rapid micellar electrokinetic chromatography (MEKC) method was developed for separation of three selected N-Nitrosamines namely N-nitrosodipropylamine (NDPA), N-nitrosodibutylamine (NDBA) and  N-nitrosodiphenylamine (NDPhA). The effects of composition of the buffer and its pH, concentration of surfactants on the separation and migration times of nitrosamines were investigated. The instrumental variables affecting sensitivity and resolution such as power supply and injection mode were carefully optimized. The best separation was achieved using 40 mM sodium dodecyl sulfate (SDS) as a surfactant in 10 mM phosphate buffer (pH 8.0) at a temperature of 25 ºC, applied voltage of 29 kV, wavelength of 230 nm and electrokinetic injection of 9 s at 5 kV within 10 min analysis time. Excellent linearity was obtained in the concentration range of 2 to 100 µg/mL with coefficients of determination, r² ≥ 0.979. This method showed good reproducibility with relative standard deviation (RSDs) value ranging from 2.46% to 6.61%. The limits of detection (LOD) and limits of quantification (LOQ) ranged from 0.16 to 0.43 µg/mL and 0.54 to 1.44 µg/mL respectively.

 

Keywords:  Nitrosamines, surfactants, capillary electrophoresis, micellar electrokinetic chromatography

 

Abstrak

Satu kaedah kromatografi elektrokinetik misel yang mudah dan cepat telah dibangunkan bagi pemisahan tiga sebatian N-Nitrosamina yang dipilih iaitu N-nitrosodipropilamina (NDPA), N-nitrosodibutilamina (NDBA) dan N-nitrosodifenilamina (NDPhA). Kesan komposisi penimbal dan pH, kepekatan surfaktan terhadap pemisahan dan masa peralihan nirosamina telah dikaji. Pembolehubah alat yang mempengaruhi kepekaan dan resolusi seperti bekalan kuasa dan mod suntikan telah dioptimumkan dengan berhati-hati. Pemisahan yang terbaik dicapai menggunakan 40 mM SDS sebagai  surfaktan di dalam 10 mM penimbal fosfat (pH 8.0) pada suhu 25 ºC, voltan gunakan 29 kV, panjang gelombang 230 nm dan suntikan elektrokinetik 9 saat pada 5 kV dengan masa analisis selama 10 minit. Kelinearan yang baik telah diperolehi dalam julat kepekatan 2 - 100 µg/mL dengan koefisien penentuan, r² ≥ 0.979. Kaedah ini menunjukkan kebolehulangan yang baik dengan nilai sisihan piawai relatif dalam julat 2.46% - 6.61%. Had pengesanan dan had penentuan adalah 0.16 - 0.43 µg/mL dan 0.54 - 1.44 µg/mL, masing-masingnya.

 

Kata kunci: Nitrosamina, surfaktan, elektroforesis kapilari, kromatografi elektrokinetik misel

 

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