title: Rapid determination of some beta-blockers in complicated matrices by tandem dispersive liquid-liquid microextraction followed by high performance liquid chromatography.
abstract: In this research work, an efficient tandem dispersive liquid-liquid microextraction (TDLLME) procedure coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV) was successfully applied for the determination of beta-blockers in human plasma and pharmaceutical wastewater samples. High clean-up and preconcentration factor are easily and rapidly feasible via this novel, cheap, and safe microextraction method, leading to high quality experimental data. It consists of two sequential dispersive liquid-liquid microextraction methods, accomplished via air/ultrasonic agitation and air agitation, respectively. In order to enrich the optimal values for the mentioned procedures, the Box-Behnken design (BBD) combined with the desirability function (DF) was used. The optimum values were found to be 11.0 % (w/v) of the salt amount, an initial pH value of 12.0, 103 μL of organic extractant phase, and 45 μL of aqueous extractant phase with pH value of 2.0, resulted in reasonable recovery percentages with a logical desirability. Under optimal experimental conditions, good linear ranges (3-2000 ng mL-1for metoprolol and 2.5-2500 ng mL-1for propranolol with the correlation of determinations (R2s) higher than 0.99) and low limits of detection (0.8 and 1.0 ng mL-1for propranolol and metoprolol, respectively) were obtainable. Also, TDLLME-HPLC-UV provided good proper repeatabilities (relative standard deviations (RSDs) below 5.7 %, n = 3) and high enrichment factors (EFs) of 75-100. Graphical abstract TDLLME of beta-blockers from complicated matrices.
authors.affiliation: Department of Chemistry, Semnan University, Semnan, 2333383-193, Iran.
authors.forename: Maryam
authors.initials: M
authors.lastname: Hemmati
authors.affiliation: Department of Chemistry, Semnan University, Semnan, 2333383-193, Iran. aasghari@semnan.ac.ir.
authors.forename: Alireza
authors.initials: A
authors.lastname: Asghari
authors.affiliation: Department of Chemistry, Semnan University, Semnan, 2333383-193, Iran.
authors.forename: Mohammad
authors.initials: M
authors.lastname: Bazregar
authors.affiliation: Department of Chemistry, Semnan University, Semnan, 2333383-193, Iran.
authors.forename: Maryam
authors.initials: M
authors.lastname: Rajabi
mesh_terms: D000319:Adrenergic beta-Antagonists / Q000032:analysis / Q000097:blood*; D000704:Analysis of Variance; D002851:Chromatography, High Pressure Liquid; D006801:Humans; D057230:Limit of Detection; D059627:Liquid Phase Microextraction; D013997:Time Factors; D062065:Wastewater / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000032:analysis / Q000097:blood*
chemical_list: D000319:Adrenergic beta-Antagonists; D062065:Wastewater; D014874:Water Pollutants, Chemical
keywords: Beta-blockers; Box-Behnken design; Complicated matrices; Developed liquid-phase microextraction; High clean-up and preconcentration