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Liquid Chromatographic Determination of NSAIDs in Urine After Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplets

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Abstract

An environmentally benign method of sample preparation based on dispersive liquid–liquid microextraction and solidification of floating organic droplets (DLLME-SFO) coupled with high-performance liquid chromatography with ultraviolet detection has been developed for analysis of non-steroidal anti-inflammatory drugs (NSAIDs) in biological fluids. A low-toxicity solvent was used to replace the chlorinated solvents commonly used in conventional DLLME. Seven conditions were investigated and optimized: type and volume of extraction solvent and dispersive solvent, extraction time, effect of addition of salt, and sample pH. Under the optimum conditions, good linearity was obtained in the range 0.01–10 µg mL−1, with coefficients of determination (r 2) >0.9949. Detection limits were in the range 0.0034–0.0052 µg mL−1 with good reproducibility (RSD) and satisfactory inter-day and intra-day recovery (95.7–115.6 %). The method was successfully used for analysis of diclofenac, mefenamic acid, and ketoprofen in human urine. Analysis of urine samples from a patient 2 and 4 h after administration of diclofenac revealed concentrations of 1.20 and 0.34 µg mL−1, respectively.

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Acknowledgments

The authors would like to thank Universiti Teknologi Malaysia, for use of facilities, the Ministry of Education Malaysia, for financial support through research grants R.J130000.7809.4F177 and Q.J130000.2509.09H84, and Universiti Teknologi MARA, for a fellowship for Dyia Syaleyana Md Shukri.

Conflict of Interest

The authors declare no conflict of interest.

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Authors and Affiliations

  1. Department of Chemistry, Faculty of Science, Universiti Teknologi Malaysia (UTM), 81310, Johor Bahru, Johor, Malaysia

    Dyia Syaleyana Md Shukri, Mohd Marsin Sanagi, Wan Aini Wan Ibrahim & Nurul Nabilah Zainal Abidin

  2. Centre for Functional Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia (UTM), 81310, Johor Bahru, Johor, Malaysia

    Mohd Marsin Sanagi

  3. Department of Chemistry, Faculty of Applied Science, Universiti Teknologi MARA Perlis (UiTM), 02600, Arau, Perlis, Malaysia

    Dyia Syaleyana Md Shukri

  4. Department of Pharmaceutical and Medicinal Chemistry, Pharmaceutical and Drug Industries Research Division, National Research Centre, Dokki, Giza, 12622, Egypt

    Hassan Y. Aboul-Enein

Authors
  1. Dyia Syaleyana Md Shukri
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  2. Mohd Marsin Sanagi
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  3. Wan Aini Wan Ibrahim
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  4. Nurul Nabilah Zainal Abidin
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  5. Hassan Y. Aboul-Enein
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Correspondence to Mohd Marsin Sanagi or Hassan Y. Aboul-Enein.

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Shukri, D.S.M., Sanagi, M.M., Ibrahim, W.A.W. et al. Liquid Chromatographic Determination of NSAIDs in Urine After Dispersive Liquid–Liquid Microextraction Based on Solidification of Floating Organic Droplets. Chromatographia 78, 987–994 (2015). https://doi.org/10.1007/s10337-015-2920-0

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  • DOI: https://doi.org/10.1007/s10337-015-2920-0

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