One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD

The present study describes an “one-step” derivatization and microextraction using a pH-switchable hydrophilicity solvent for the determination of amantadine and memantine in human urine by liquid chromatography and fluorescence detection. The procedure is based on the derivatization of the analytes...

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Main Authors: Marianna Ntorkou, Paraskevas D. Tzanavaras, Constantinos K. Zacharis
Format: Article
Language:English
Published: Elsevier 2024-10-01
Series:Advances in Sample Preparation
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Online Access:http://www.sciencedirect.com/science/article/pii/S2772582024000330
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author Marianna Ntorkou
Paraskevas D. Tzanavaras
Constantinos K. Zacharis
author_facet Marianna Ntorkou
Paraskevas D. Tzanavaras
Constantinos K. Zacharis
author_sort Marianna Ntorkou
collection DOAJ
description The present study describes an “one-step” derivatization and microextraction using a pH-switchable hydrophilicity solvent for the determination of amantadine and memantine in human urine by liquid chromatography and fluorescence detection. The procedure is based on the derivatization of the analytes with o-phthalaldehyde/N-acetyl cysteine at alkaline conditions in the presence of sodium salicylate as extractant in a homogeneous solution. The liquid-solid transition of salicylic acid was achieved by adding an aliquot of concentrated phosphoric acid that enables efficient dispersion and phase separation in a single step. Due to the moderate melting point of salicylic acid, its solidification is carried out at room temperature without the need for sample cooling. Critical parameters affecting the efficiency of the derivatization reaction and the microextraction performance were investigated and optimized. The fluorescent analyte derivatives were monitored at λex/λem = 340/450 nm. The proposed method was validated in terms of specificity, linearity, precision and trueness. The method was linear in the range of 50–2000 ng mL−1 while the intraday and between days precision was less than 13.7% in all cases. The trueness of the method ranged between 87.9 and 113%. The green character and the applicability of the method were assessed using ComplexMoGAPI and BAGI tools. The developed analytical scheme presented satisfactory performance, and it could be applied in the analysis of selected drugs in human urine samples.
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spelling doaj-art-62031b275a2e40bdb7f270abaf2af2c32024-12-08T06:13:30ZengElsevierAdvances in Sample Preparation2772-58202024-10-0112100135One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLDMarianna Ntorkou0Paraskevas D. Tzanavaras1Constantinos K. Zacharis2Laboratory of Pharmaceutical Analysis, Department of Pharmacy, Aristotle University of Thessaloniki (AUTh), Thessaloniki 54124, GreeceLaboratory of Analytical Chemistry, School of Chemistry, Faculty of Sciences, Aristotle University of Thessaloniki, GR-54124, GreeceLaboratory of Pharmaceutical Analysis, Department of Pharmacy, Aristotle University of Thessaloniki (AUTh), Thessaloniki 54124, Greece; Corresponding author.The present study describes an “one-step” derivatization and microextraction using a pH-switchable hydrophilicity solvent for the determination of amantadine and memantine in human urine by liquid chromatography and fluorescence detection. The procedure is based on the derivatization of the analytes with o-phthalaldehyde/N-acetyl cysteine at alkaline conditions in the presence of sodium salicylate as extractant in a homogeneous solution. The liquid-solid transition of salicylic acid was achieved by adding an aliquot of concentrated phosphoric acid that enables efficient dispersion and phase separation in a single step. Due to the moderate melting point of salicylic acid, its solidification is carried out at room temperature without the need for sample cooling. Critical parameters affecting the efficiency of the derivatization reaction and the microextraction performance were investigated and optimized. The fluorescent analyte derivatives were monitored at λex/λem = 340/450 nm. The proposed method was validated in terms of specificity, linearity, precision and trueness. The method was linear in the range of 50–2000 ng mL−1 while the intraday and between days precision was less than 13.7% in all cases. The trueness of the method ranged between 87.9 and 113%. The green character and the applicability of the method were assessed using ComplexMoGAPI and BAGI tools. The developed analytical scheme presented satisfactory performance, and it could be applied in the analysis of selected drugs in human urine samples.http://www.sciencedirect.com/science/article/pii/S2772582024000330Switchable hydrophilicity solventDerivatizationMicroextractionAmantadineMemantineLiquid chromatography
spellingShingle Marianna Ntorkou
Paraskevas D. Tzanavaras
Constantinos K. Zacharis
One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD
Advances in Sample Preparation
Switchable hydrophilicity solvent
Derivatization
Microextraction
Amantadine
Memantine
Liquid chromatography
title One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD
title_full One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD
title_fullStr One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD
title_full_unstemmed One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD
title_short One step derivatization and switchable hydrophilicity solvent-based microextraction for the determination of adamantane analogues in human urine by HPLC-FLD
title_sort one step derivatization and switchable hydrophilicity solvent based microextraction for the determination of adamantane analogues in human urine by hplc fld
topic Switchable hydrophilicity solvent
Derivatization
Microextraction
Amantadine
Memantine
Liquid chromatography
url http://www.sciencedirect.com/science/article/pii/S2772582024000330
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