Analysis of Aceclofenac, Ketorolac, and Sulindac in Human Urine Using the Microemulsion Electrokinetic Chromatography Method

Author:

Hermawan Dadan1,Mohd Yatim Izdiani2,Wan Ibrahim Wan Aini2,Abdul Keyon Aemi Syazwani23,Cacu 1ORCID,Riswoko Asep4ORCID,Laksmono Joddy Arya4

Affiliation:

1. Department of Chemistry, Faculty of Mathematics and Natural Science, Jenderal Soedirman University, UNSOED, Purwokerto 53123, Central Java, Indonesia

2. Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia, UTM, Johor Bahru 81310, Johor, Malaysia

3. Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, UTM, Johor Bahru 81310, Johor, Malaysia

4. Research Center for Polymer Technology, National Research and Innovation Agency (BRIN), KST BJ. Habibie, Puspiptek Building 460, Tangerang Selatan 15314, Banten, Indonesia

Abstract

A method to determine aceclofenac, ketorolac, and sulindac in human urine samples using microemulsion electrokinetic chromatography (MEEKC) has been developed in this study. The optimization of MEEKC conditions was carried out by changing the microemulsion compositions including the buffer pH, borate salt concentration, surfactant concentration, co-surfactant concentration, organic modifier concentration, and oil droplet concentration. The optimum separation of selected drugs was obtained with a composition of microemulsion containing 10 mM borate buffer pH 9, 0.5% sodium dodecyl sulphate (SDS), 6.6% n-butanol, 6.0% acetonitrile, and 0.8% ethyl acetate. Excellent linearity was obtained in the range concentration of 25 to 200 ppm with r2 > 0.999. Limits of detection (LOD, S/N = 3) and limits of quantification (LOQ, S/N = 10) were 2.72 to 4.75 and 9.08 to 15.85 ppm, respectively. The solid-phase extraction (SPE) method using C-18 as an adsorbent and the solid phase micro-tip extraction (SPMTE) method using multiwalled carbon nanotubes (MWCNTs) as an adsorbent were used to clean-up and pre-concentrate the urine samples prior to the MEEKC analysis. The best recoveries of the selected drugs in the spiked urine sample were 91 to 103% with RSD of 1.26 to 4.03% (n = 3) using the SPE-MEEKC method.

Funder

Ministry of Education, Culture, Research, and Technology

Universitas Jenderal Soedirman, Indonesia

Publisher

MDPI AG

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