Sains Malaysiana 49(5)(2020): 979-988

http://dx.doi.org/10.17576/jsm-2020-4905-02

 

Simple and Sensitive Electrokinetic Supercharging in Capillary Electrophoresis for Online Preconcentration and Separation of Secbumeton in Water Samples

 

(Superpengesan Elektrokinetik Ringkas dan Sensitif dalam Elektroforesis Rerambut Prapemerkatan secara Terus dan Permisahan Sekbumeton dalam Sampel Air)

 

RASMEY SOEUNG1,2, NADHIRATUL-FARIHIN SEMAIL1, WAN ADNAN WAN OMAR1, NUR NADHIRAH MOHAMAD ZAIN1, MAZIDATULAKMAM MISKAM3, YONG FOO WONG3, AEMI SYAZWANI ABDUL KEYON4, MUGGUNDHA RAOOV RAMACHANDRAN5, SAZLINDA KAMARUZAMAN6,7 & NOORFATIMAH YAHAYA1*

  1Integrative Medicine Cluster, Advanced Medical and Dental Institute (AMDI), Universiti Sains Malaysia, 13200 Bertam Kepala Batas, Penang, Malaysia

  2Royal University of Agriculture, 12400 Dangkor District, Phnom Penh, Cambodia

  3School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden Penang, Malaysia

4Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor Darul Takzim, Malaysia  

5Department of Chemistry, Faculty of Science, Universiti Malaya, 50603 Kuala Lumpur, Federal Territory, Malaysia  

6Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor Darul Ehsan, Malaysia  

7Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 Johor Bahru, Johor Darul Takzim, Malaysia  

Diserahkan: 26 Januari 2019/ Diterima: 19 Januari 2020  

ABSTRACT

This study describes an electrokinetic supercharging for online preconcentration capillary electrophoresis (CE) technique of secbumeton in water samples. Important CE separation and preconcentration conditions, such as concentration and pH of the background electrolyte, applied voltage and ultraviolet wavelength, type and injection time of the terminating electrolyte, and injection time of the leading electrolyte and sample were investigated and optimized. The optimum conditions involved hydrodynamic injection of leading electrolyte (100 mM sodium chloride, 30 s, 50 mbar), electrokinetic injection of the sample as high as 250 s (at +7 kV voltage), and hydrodynamic injection of terminating electrolyte (100 mM Tris buffer, 40 s, 50 mbar). This strategy enhanced secbumeton detection sensitivity up to 3847-fold and 2267-fold when compared with hydrodynamic and electrokinetic injection, respectively, providing a limit of detection as low as 0.03 µg L–1 with good repeatability (relative standard deviation < 4%, n = 5). Wide linear range (0.1–500 µg L–1) with good linearity (R2 = 0.9997) was obtained. The limit of detection was adequate for the analysis of secbumeton in water samples with concentrations lower than its maximum residual limit (0.1 µg L–1). The developed method was applied to environmental water samples, and recoveries were between 85.7 and 105.6%.

Keywords: Capillary electrophoresis; electrokinetic supercharging; environmental water samples; online preconcentration; secbumeton  

ABSTRAK

Kajian ini menerangkan suatu superpengecasan elektrokinetik bagi prapemekatan secara terus teknik elektroforesis rerambut (CE) bagi sekbumeton di dalam sampel air. Pemisahan CE dan keadaan prapemekatan yang penting seperti kepekatan dan pH bagi latar belakang elektrolit, voltan gunaan dan panjang gelombang ultraviolet, jenis dan masa suntikan bagi elektrolit penamat dan masa suntikan bagi elektrolit pemula dan sampel telah dikaji dan dioptimumkan. Keadaan optimum termasuklah suntikan hidrodinamik bagi elektrolit pemula (100 mM natrium klorida, 30 s, 50 mbar), suntikan elektrokinetik bagi sampel setinggi 250 s (pada +7 kV voltan) dan suntikan hidrodinamik bagi elektrolit penamat (100 mM larutan penimbal TRIS, 40 s, 50 mbar). Strategi ini meningkatkan kepekaan penentuan sekbumeton sehingga 3847-gandaan dan 2267-gandaan apabila dibandingkan dengan masing-masing, suntikan hidrodinamik dan elektrokinetik, dengan memberi had pengesanan serendah 0.03 µg L–1 dengan kebolehulangan yang baik (sisihan piawai relatif < 4 %, n = 5). Julat linear yang besar (0.1–500 µg L–1) dengan kelinearan yang baik (R2 = 0.9997) telah diperoleh. Had pengesanan ini adalah mencukupi bagi menganalisa sekbumeton di dalam sampel air dengan kepekatan yang lebih rendah daripada had surih maksimum (0.1 µg L–1). Kaedah yang telah dibangunkan telah digunakan bagi sampel air sekitaran dan pengembalian adalah antara 85.7 dan 105.6%.

Kata kunci: Elektroforesis rerambut; prapemekatan secara terus; sampel air sekitaran; sekbumeton; superpengecasan elektrokinetik  

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  *Pengarang untuk surat-menyurat; email: noorfatimah@usm.my

 

 

 

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