Ultrasound-promoted dispersive micro solid-phase extraction of trace anti-hypertensive drugs from biological matrices using a sonochemically synthesized conductive polymer nanocomposite

Abstract

In this work, a rapid and efficient procedure named ultrasound meliorated dispersive micro solid-phase extraction followed by high performance liquid chromatography-ultra violet detection (US-D-μSPE-HPLC-UV) was developed for the pre-concentration of the main trace anti-hypertensive drugs in complex matrices. The basis of this procedure was a polypyrrole-sodium dodecylbenzenesulfonate/zinc oxide (PPy-DBSNa/ZnO) nanocomposite. It was readily synthesized by the impressive way of in situ sonochemical oxidative polymerization in the presence of some additives such as FeCl₃ and DBSNa, ultimately leading to the effective coating of PPy on the ZnO nanoparticle cores. Characterization of the proposed nanosorbent was performed by different techniques such as FESEM, XRD,EDX, and TGA, confirming the high quality and proper physico-chemical properties of the proposed sorbent. In order to better investigate the input variables, the central composite design (CCD) combined with the desirability function (DF) was utilized. The enriched optimum conditions consisted of the initial pH value of 11.8, 15mg of the PPy-DBSNa/ZnO nanocomposite, a sonication time of 4.6min, and 100μL of methanol, resulting in maximum responses at a relatively low extraction time with a logical DF. Under the optimum conditions, good linearity (5-5000, 2.5-3500, and 2.5-3000ngmL^-1 for metoprolol, propranolol, and carvedilol, respectively, with the correlation of determinations (R²s) higher than 0.99), low limits of detection (LODs) (0.8-1.5ngmL^-1), proper repeatabilities (relative standard deviation values (RSDs) below 6.3%, n=3), reasonable enrichment factors (EFs) (60-72), and good extraction recoveries (ERs) (higher than %75) were obtainable. These appropriate validations corroborated a good effectiveness of ultrasonic waves in the achievement of a supreme solid phase as well as a facile and efficient microextraction of the low therapeutic concentrations in human plasma and urine samples.

Keywords: Anti-hypertensive drugs; Biological samples; In situ sonochemical oxidative polymerization; PPy-DBSNa/ZnO nanocomposite; Ultrasound-promoted dispersive micro solid-phase extraction.