Comparison between Exhaustive and Equilibrium Extraction Using Different SPE Sorbents and Sol-Gel Carbowax 20M Coated FPSE Media.

Angela Tartaglia,Victoria F Samanidou,Kenneth G Furton,Daniela Macerola,Silvia Piccolantonio,Pantaleone Bruni,Marcello Locatelli,Fausto Croce,Elena Sperandio,Halil I Ulusoy,Abuzar Kabir,Fabio Maroni

doi:10.3390/molecules24030382

Abstract

This paper reports the performance comparison between the exhaustive and equilibrium extraction using classical Avantor C18 solid phase extraction (SPE) sorbent, hydrophilic-lipophilic balance (HLB) SPE sorbent, Sep-Pak C18 SPE sorbent, novel sol-gel Carbowax 20M (sol-gel CW 20M) SPE sorbent, and sol-gel CW 20M coated fabric phase sorptive extraction (FPSE) media for the simultaneous extraction and analysis of three inflammatory bowel disease (IBD) drugs that possess logP values (polarity) ranging from 1.66 for cortisone, 2.30 for ciprofloxacin, and 2.92 for sulfasalazine. Both the commercial SPE phases and in-house synthesized sol-gel CW 20M SPE phases were loaded in SPE cartridges and the extractions were carried out under an exhaustive extraction mode. FPSE was carried out under an equilibrium extraction mode. The drug compounds were resolved using a Luna C18 column (250 mm × 4.6 mm; 5 μm particle size) in gradient elution mode within 20 min and the method was validated in compliance with international guidelines for the bioanalytical method validation. Novel in-house synthesized and loaded sol-gel CW 20M SPE sorbent cartridges were characterized in terms of their extraction capability, breakthrough volume, retention volume, hold-up volume, number of the theoretical plate, and the retention factor.

Highlights

Sample preparation and ‘clean-up’ have the aim of improving the analytical parameters to enhance detectability and to protect the performance of analytical equipment
Solid-phase extraction (SPE) is the most popular sample preparation technique used for extraction, clean up, and pre-concentration of both environmental and biological samples
The primary advantage is that solid phase extraction (SPE) is a non-equilibrium, exhaustive extraction procedure; the problem with using an equilibrium process is that the analyst may never know when equilibrium has been reached, and the equilibrium distribution may necessitate multiple extractions [2]

Summary

Introduction

Sample preparation and ‘clean-up’ have the aim of improving the analytical parameters to enhance detectability and to protect the performance of analytical equipment. These steps are time consuming, utilize large volumes of toxic and hazardous organic solvents, and are prone to error. For these reasons, novel extraction technologies are continuously being developed to overcome these drawbacks [1] in order to improve the extraction efficiency, reduce the sample handling, and enhance the reproducibility. Solid-phase extraction (SPE) is the most popular sample preparation technique used for extraction, clean up, and pre-concentration of both environmental and biological samples. The primary advantage is that SPE is a non-equilibrium, exhaustive extraction procedure; the problem with using an equilibrium process is that the analyst may never know when equilibrium has been reached, and the equilibrium distribution may necessitate multiple extractions [2]

Methods

Results

Conclusion