The Effectiveness of Liquid-Phase Microextraction of Beta-Blockers from Aqueous Matrices for Their Analysis by Chromatographic Techniques

Overview

Journal Molecules

Publisher MDPI

Specialty Biology

Date 2025 Mar 13

PMID 40076241

Authors

Mihail Simion Beldean-Galea

Mihaela-Catalina Herghelegiu

Vlad-Alexandru Panescu

Jerome Vial

Maria Concetta Bruzzoniti

Maria-Virginia Coman

Affiliations

Soon will be listed here.

Abstract

Beta-blockers are pharmaceuticals used to treat cardiovascular diseases such as hypertension, angina pectoris, and arrhythmia. Due to high consumption, they are continuously released into the environment, being detected in many aqueous matrices. The aim of this research is to test the effectiveness of two green liquid-phase microextraction procedures, such as dispersive liquid-liquid microextraction (DLLME) and solidification of floating organic droplet microextraction (SFOME) for the selective extraction of eight beta-blockers (atenolol, nadolol, pindolol, acebutolol, metoprolol, bisoprolol, propranolol, and betaxolol) from aqueous matrices for their analysis by gas chromatography (GC) or liquid chromatography (LC). The influence of extraction parameters, such as the type and volume of extraction and disperser solvents, and ionic strength were studied. The developed extraction procedures provide a good enrichment factor for six compounds (61.22-243.97), good extraction recovery (53.04-92.1%), and good sample cleaning for both extraction procedures. Good limits of detection (0.13 to 0.69 µg/mL for GC and 0.07 to 0.15 µg/mL for HPLC) and limits of quantification (0.39 to 2.10 µg/mL for GC and 0.20 to 0.45 µg/mL for LC) were obtained. The developed procedures were successfully applied to the analysis of selected beta-blockers in wastewater samples, proving their applicability to the real samples.

References

Godoy A, Kummrow F, Pamplin P . Occurrence, ecotoxicological effects and risk assessment of antihypertensive pharmaceutical residues in the aquatic environment--A review. Chemosphere. 2015; 138:281-91. DOI: 10.1016/j.chemosphere.2015.06.024. View

Xu J, Sun H, Zhang Y, Alder A . Occurrence and enantiomer profiles of β-blockers in wastewater and a receiving water body and adjacent soil in Tianjin, China. Sci Total Environ. 2018; 650(Pt 1):1122-1130. DOI: 10.1016/j.scitotenv.2018.09.086. View

Garcia M, Canada Canada F, Culzoni M, Vera-Candioti L, Siano G, Goicoechea H . Chemometric tools improving the determination of anti-inflammatory and antiepileptic drugs in river and wastewater by solid-phase microextraction and liquid chromatography diode array detection. J Chromatogr A. 2009; 1216(29):5489-96. DOI: 10.1016/j.chroma.2009.05.073. View

Yi M, Sheng Q, Sui Q, Lu H . β-blockers in the environment: Distribution, transformation, and ecotoxicity. Environ Pollut. 2020; 266(Pt 2):115269. DOI: 10.1016/j.envpol.2020.115269. View

Hemmati M, Asghari A, Bazregar M, Rajabi M . Rapid determination of some beta-blockers in complicated matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography. Anal Bioanal Chem. 2016; 408(28):8163-8176. DOI: 10.1007/s00216-016-9922-0. View

Jouyban A, Sorouraddin M, Farajzadeh M, Somi M, Fazeli-Bakhtiyari R . Determination of five antiarrhythmic drugs in human plasma by dispersive liquid-liquid microextraction and high-performance liquid chromatography. Talanta. 2015; 134:681-689. DOI: 10.1016/j.talanta.2014.12.008. View

Mousavi L, Tamiji Z, Khoshayand M . Applications and opportunities of experimental design for the dispersive liquid-liquid microextraction method - A review. Talanta. 2018; 190:335-356. DOI: 10.1016/j.talanta.2018.08.002. View

Leong M, Huang S . Dispersive liquid-liquid microextraction method based on solidification of floating organic drop combined with gas chromatography with electron-capture or mass spectrometry detection. J Chromatogr A. 2008; 1211(1-2):8-12. DOI: 10.1016/j.chroma.2008.09.111. View

Alder A, Schaffner C, Majewsky M, Klasmeier J, Fenner K . Fate of beta-blocker human pharmaceuticals in surface water: comparison of measured and simulated concentrations in the Glatt Valley Watershed, Switzerland. Water Res. 2009; 44(3):936-48. DOI: 10.1016/j.watres.2009.10.002. View

10.

Farhadi K, Hatami M, Forough M, Molaei R . Dispersive liquid-liquid microextraction of propranolol enantiomers from human plasma based on the solidification of a floating organic droplet. Bioanalysis. 2013; 5(6):701-10. DOI: 10.4155/bio.13.23. View

11.

Zamani-Kalajahi M, Fazeli-Bakhtiyari R, Amiri M, Golmohammadi A, Afrasiabi A, Khoubnasabjafari M . Dispersive liquid-liquid microextraction based on solidification of floating organic droplet followed by spectrofluorimetry for determination of carvedilol in human plasma. Bioanalysis. 2013; 5(4):437-48. DOI: 10.4155/bio.12.326. View

12.

Maszkowska J, Stolte S, Kumirska J, Lukaszewicz P, Mioduszewska K, Puckowski A . Beta-blockers in the environment: part II. Ecotoxicity study. Sci Total Environ. 2014; 493:1122-6. DOI: 10.1016/j.scitotenv.2014.06.039. View

13.

Beldean-Galea M, Coman V, Thiebaut D, Vial J . Determination of four acidic nonsteroidal anti-inflammatory drugs in wastewater samples by dispersive liquid-liquid microextraction based on solidification of floating organic droplet and high-performance liquid chromatography. J Sep Sci. 2014; 38(4):641-8. DOI: 10.1002/jssc.201400933. View

14.

Arismendi D, Becerra-Herrera M, Cerrato I, Richter P . Simultaneous determination of multiresidue and multiclass emerging contaminants in waters by rotating-disk sorptive extraction-derivatization-gas chromatography/mass spectrometry. Talanta. 2019; 201:480-489. DOI: 10.1016/j.talanta.2019.03.120. View

15.

Mlunguza N, Ncube S, Mahlambi P, Chimuka L, Madikizela L . Determination of selected antiretroviral drugs in wastewater, surface water and aquatic plants using hollow fibre liquid phase microextraction and liquid chromatography - tandem mass spectrometry. J Hazard Mater. 2019; 382:121067. DOI: 10.1016/j.jhazmat.2019.121067. View

16.

Farahmand F, Ghasemzadeh B, Naseri A . Air-assisted liquid-liquid microextraction using floating organic droplet solidification for simultaneous extraction and spectrophotometric determination of some drugs in biological samples through chemometrics methods. Spectrochim Acta A Mol Biomol Spectrosc. 2017; 188:72-79. DOI: 10.1016/j.saa.2017.06.069. View

17.

Beldean-Galea M, Klein R, Coman M . Simultaneous Determination of Four Nonsteroidal Anti-Inflammatory Drugs and Three Estrogen Steroid Hormones in Wastewater Samples by Dispersive Liquid-Liquid Microextraction Based on Solidification of Floating Organic Droplet and HPLC. J AOAC Int. 2019; 103(2):392-398. DOI: 10.5740/jaoacint.19-0258. View

18.

Wicht A, Heye K, Schmidt A, Oehlmann J, Huhn C . The wastewater micropollutant carbamazepine in insectivorous birds-an exposure estimate. Anal Bioanal Chem. 2022; 414(17):4909-4917. PMC: 9234033. DOI: 10.1007/s00216-022-04117-0. View

19.

Berlioz-Barbier A, Baudot R, Wiest L, Gust M, Garric J, Cren-Olive C . MicroQuEChERS-nanoliquid chromatography-nanospray-tandem mass spectrometry for the detection and quantification of trace pharmaceuticals in benthic invertebrates. Talanta. 2014; 132:796-802. DOI: 10.1016/j.talanta.2014.10.030. View

20.

Yildirim S, Sellitepe H . Vortex assisted liquid-liquid microextraction based on in situ formation of a natural deep eutectic solvent by microwave irradiation for the determination of beta-blockers in water samples. J Chromatogr A. 2021; 1642:462007. DOI: 10.1016/j.chroma.2021.462007. View