Research output: Contribution to journal › Article › peer-review
Solidified floating organic drop microextraction procedure based on deep eutectic solvent for the determination of melatonin in pharmaceuticals and dietary supplements. / Якупова, Зиля Рафаэлевна; Якубенко, Артем Алексеевич; Богданова, Полина Дмитриевна; Годунов, Павел Анатольевич; Вах, Кристина Степановна; Гармонов, Сергей; Булатов, Андрей Васильевич.
In: Microchemical Journal, Vol. 187, 108373, 01.04.2023.Research output: Contribution to journal › Article › peer-review
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TY - JOUR
T1 - Solidified floating organic drop microextraction procedure based on deep eutectic solvent for the determination of melatonin in pharmaceuticals and dietary supplements
AU - Якупова, Зиля Рафаэлевна
AU - Якубенко, Артем Алексеевич
AU - Богданова, Полина Дмитриевна
AU - Годунов, Павел Анатольевич
AU - Вах, Кристина Степановна
AU - Гармонов, Сергей
AU - Булатов, Андрей Васильевич
PY - 2023/4/1
Y1 - 2023/4/1
N2 - A miniaturized clean-up and preconcentration procedure involving deep eutectic solvent-based solidified floating organic drop microextraction was developed for the determination of melatonin in pharmaceuticals and dietary supplements by high-performance liquid chromatography with UV detection. Melatonin is widely used for the treatment of a large spectrum of diseases, and many studies have focused on its efficacy in reducing COVID-19 severity. For the first time, various hydrophobic deep eutectic solvents based on menthol, medium-chain fatty acids, and long-chain alcohols were studied for the microextraction of melatonin. Among the studied solvents, the deep eutectic solvent based on menthol and heptanoic acid provided the highest extraction recovery (90 %). In the developed procedure, a flat magnetic stirrer bar was covered by a microliter amount of the deep eutectic solvent and the sample solution was added under magnetic stirring. In this case, the deep eutectic solvent phase was easily dispersed into the aqueous phase without the use of any organic disperser solvents, resulting in fast analyte extraction (1 min). In the absence of stirring, the aggregation of extract as a floating drop on the surface of the aqueous phase was observed immediately. The low melting/freezing point and low density of the extraction solvent compared with water allowed one to quickly and easily retrieve a low volume of extract (25 μL) in a microextraction procedure by solidification. Validation of the procedure showed that limits of detection and quantification, calculated from the blank tests based on 3σ and 10 σ, were 0.003 mg g−1 and 0.01 mg g−1, respectively.
AB - A miniaturized clean-up and preconcentration procedure involving deep eutectic solvent-based solidified floating organic drop microextraction was developed for the determination of melatonin in pharmaceuticals and dietary supplements by high-performance liquid chromatography with UV detection. Melatonin is widely used for the treatment of a large spectrum of diseases, and many studies have focused on its efficacy in reducing COVID-19 severity. For the first time, various hydrophobic deep eutectic solvents based on menthol, medium-chain fatty acids, and long-chain alcohols were studied for the microextraction of melatonin. Among the studied solvents, the deep eutectic solvent based on menthol and heptanoic acid provided the highest extraction recovery (90 %). In the developed procedure, a flat magnetic stirrer bar was covered by a microliter amount of the deep eutectic solvent and the sample solution was added under magnetic stirring. In this case, the deep eutectic solvent phase was easily dispersed into the aqueous phase without the use of any organic disperser solvents, resulting in fast analyte extraction (1 min). In the absence of stirring, the aggregation of extract as a floating drop on the surface of the aqueous phase was observed immediately. The low melting/freezing point and low density of the extraction solvent compared with water allowed one to quickly and easily retrieve a low volume of extract (25 μL) in a microextraction procedure by solidification. Validation of the procedure showed that limits of detection and quantification, calculated from the blank tests based on 3σ and 10 σ, were 0.003 mg g−1 and 0.01 mg g−1, respectively.
KW - Deep eutectic solvent
KW - Dietary supplements
KW - HPLC-UV
KW - Melatonin
KW - Pharmaceuticals
KW - Solidified floating organic drop microextraction
UR - https://www.mendeley.com/catalogue/f4d2a8ed-feb0-39d7-a44f-f9c8b9ce52a0/
U2 - 10.1016/j.microc.2022.108373
DO - 10.1016/j.microc.2022.108373
M3 - Article
VL - 187
JO - Microchemical Journal
JF - Microchemical Journal
SN - 0026-265X
M1 - 108373
ER -
ID: 102384509