Sains Malaysiana 50(5)(2021): 1297-1307

http://doi.org/10.17576/jsm-2021-5005-10

Vortex Assisted Liquid-Liquid Microextraction with Back Extraction of Repaglinide, Glibenclamide and Glimepiride in Water Samples

(Mikro Pengekstrakan Berbalik Cecair-Cecair Berbantu Vorteks bagi Repaglinida, Glibenclamida dan Glimepirida dalam Sampel Air)

SOHAIB JUMAAH OWAID LUHAIBI¹, NOORFATIMAH YAHAYA², ANAS ALSHISHANI³, MAIZATUL NAJWA JAJULI⁴ & MAZIDATULAKMAM MISKAM¹*

¹School of Chemical Sciences, Universiti Sains Malaysia, 11800 USM, Pulau Pinang, Malaysia

²Integrative Medicine Cluster, Advanced Medical and Dental Institute (AMDI), Universiti Sains Malaysia, 13200 Bertam, Pulau Pinang, Malaysia

³Faculty of Pharmacy, Zarqa University, 13132 Zarqa, Jordan

⁴Department of Chemistry, Faculty of Science and Mathematics, Sultan Idris Education University, 35900 Tanjung Malim, Perak Darul Ridzuan, Malaysia

Received: 15 April 2020/Accepted: 1 October 2020

ABSTRACT

A new analytical method based on vortex-assisted liquid-liquid microextraction with back extraction (VALLME-BE) coupled with high performance liquid chromatography was developed for the simultaneous determination of antidiabetic drugs; repaglinide, glibenclamide, and glimepiride in water samples. Chromatographic separation was achieved using C18 column (250 × 4.6 mm × 5 µm) and methanol-phosphate buffer (pH3.7) in the ratio of 70:30 v/v as a mobile phase at a flow rate of 1 mLmin^-1. VALLME-BE was performed using 200 μL of n-octane dispersed into the aqueous sample (10 mL) with the aid of vortexing agitation. Then, the analytes were back-extracted from the organic solvent to 0.05 M NaOH (40 µL). Under these conditions, enrichment factor of 155-fold was achieved. The developed VALLME-BE method showed excellent linearity in the range of 30 to 1000 µgL^-1 with limit of detection (LOD) of 0.41-1.66 µgL^-1 and limit of quantification (LOQ) of 1.38-5.54. 41-1.66 µgL^-1. VALLME-BE was applied for the determination of repaglinide, glibenclamide and glimepiride in water samples with the recoveries ranged from 83-109%. The relative standard deviation for inter-day and intra-day precision was less than 9.9%.

Keywords: Glibenclamide; glimepiride; HPLC-UV; repaglinide and vortex assisted liquid-liquid microextraction with back extraction

ABSTRAK

Suatu kaedah analitikal yang baharu berdasarkan pengekstrakan berbalik - mikro pengekstrakan cecair-cecair berbantu vorteks (VALLME-BE) digandingkan dengan kromatografi cecair berprestasi tinggi telah dibangunkan untuk penentuan serentak ubat anti-diabetik; repaglinida, glibenklamida dan glimepirida di dalam sampel air. Pemisahan kromatografi telah dicapai menggunakan turus C18 (250 × 4.6 mm × 5 µm) dan penimbal methanol-fosfat (pH3.7) dengan nisbah 70:30 v/v sebagai fasa bergerak pada kadar aliran 1 mLmin^-1. VALLME-BE telah dilakukan dengan menggunakan 200 μL n-oktana yang disebarkan ke dalam sampel akues (10 mL) dengan bantuan pengadukan. Kemudian, pengekstrakan berbalik dilakukan terhadap analit daripada pelarut organik kepada 0.05 M NaOH (40 µL). Di bawah keadaan optimum, faktor pengayaan sebanyak 155-lipat telah dicapai. Kaedah VALLME-BE yang dibangunkan telah menunjukkan kelinearan yang baik dalam julat 30 hingga 1000 µgL^-1 dengan had pengesanan (LOD) sebanyak 0.41-1.66 µgL^-1 dan had pengkuantitian (LOQ) sebanyak 1.38-5.54 µgL^-1. VALLME-BE digunakan untuk pengekstrakan repaglinida, glibenklamida dan glimepirida dengan julat pengembalian semula adalah 83-109%. Sisihan piawai relatif untuk inter-hari and intra-hari mempunyai kepersisan kurang daripada 9.9%.

Kata kunci: Glibenklamida; glimepirida; HPLC-UV; repaglinida dan pengekstrakan berbalik - mikro pengekstrakan cecair-cecair berbantu vortex

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*Corresponding author; email: mazidatul@usm.my