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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*
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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