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Development of An HPLC Method for the Determination of Mesalazine in Human Plasma by Fluorimetric Derivatization and Application to A Prototype Pharmacokinetic Study

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Abstract

In this study, a new, fast and sensitive HPLC method with fluorometric detection was developed for the determination of mesalazine in human plasma and applied to a pharmacokinetic study. Mesalazine was precolumn derivatized with NBD-Cl and the fluorescent derivative was separated on a C18 (150 × 4.6 mm × 2.6 μm) analytical column at 30 ºC using a mobile phase composed of acetonitrile—0.1% o-phosphoric acid in water (70:30, v/v) by isocratic elution with flow rate of 1.0 mL min−1. The method was based on the measurement of the derivative using fluorescence detection (λex = 280 nm, λem = 325 nm). The retention time of mesalazine is 3.08 ± 0.06 min. Nortriptiline was used as internal standard. This currently developed method was validated according to ICH criteria by evaluating the specificity, linearity, precision, accuracy and robustness. The method was determined to be linear in a concentration range of 0.25–1.5 μg mL−1 with the correlation coefficient of 0.9997. LOD and LOQ were found to be 0.075 and 0.25 μg mL−1, respectively. Intraday and interday RSD values were less than 5.92%. The plasma concentration–time profile and pharmacokinetic parameters such as AUC0–t, AUC0–∞, Cmax, tmax, t1/2, were calculated according to the assays. The presented method can certainly be used for bioequivalence and bioavailability investigations and routine analysis of the drug in plasma.

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Funding

The study was carried out with the facilities of Bezmialem Vakif University Faculty of Pharmacy, no special financial support was required.

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Authors and Affiliations

  1. Institute of Health Sciences, Department of Pharmacognosy and Natural Products Chemistry, Bezmialem Vakif University, Fatih, Istanbul, Turkey

    Burhan Ceylan

  2. Faculty of Pharmacy, Department of Analytical Chemistry, Bezmialem Vakif University, Fatih, Istanbul, Turkey

    Evrim Kepekci Tekkeli

  3. Faculty of Pharmacy, Department of Analytical Chemistry, Istanbul Health and Technology University, Istanbul, Turkey

    Cem Önal

Authors
  1. Burhan Ceylan
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  2. Evrim Kepekci Tekkeli
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  3. Cem Önal
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Contributions

BC carried out calibration and validation process of the method, EKT carried out ethical commitee submission process and clinical part of the study, CO studied on all the data and all the authors contributed equally to prepare the manuscript. All authors read and approved the final manuscript.

Corresponding author

Correspondence to Evrim Kepekci Tekkeli.

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The study is approved by the Clinical Trials Ethic Commitee of Bezmialem Vakıf University (No: E.21699).

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There is no conflict of interest between authors and any kind of organisation.

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Ceylan, B., Tekkeli, E.K. & Önal, C. Development of An HPLC Method for the Determination of Mesalazine in Human Plasma by Fluorimetric Derivatization and Application to A Prototype Pharmacokinetic Study. J Fluoresc 32, 319–325 (2022). https://doi.org/10.1007/s10895-021-02848-4

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  • DOI: https://doi.org/10.1007/s10895-021-02848-4

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