Abstract

In this study, a novel sort of sample preparation sorbent was developed, by preparing thin layer graphene oxide tablets (GO-Tabs) utilizing a mixture of graphene oxide and polyethylene glycol on a polyethylene substrate. The GO-Tabs were used for extraction and concentration of omeprazole (OME) in human saliva samples. The determination of OME was carried out using liquid chromatography-tandem mass spectrometry (LC–MS/MS) under gradient LC conditions and in the positive ion mode (ESI+) with mass transitions of m/z 346.3→198.0 for OME and m/z 369.98→252.0 for the internal standard. Standard calibration for the saliva samples was in the range of 2.0–2000 nmol L−1. Limits of detection and quantification were 0.05 and 2.0 nmol L−1, respectively. Method validation showed good method accuracy and precision; the inter-day precision values ranged from 5.7 to 8.3 (%RSD), and the accuracy of determinations varied from −11.8% to 13.3% (% deviation from nominal values). The extraction recovery was 60%, and GO-Tabs could be re-used for more than ten extractions without deterioration in recovery. In this study, the determination of OME in real human saliva samples using GO-Tab extraction was validated.

Highlights

  • Omeprazole (OME) is a well-known drug that is used as a proton pump inhibitor to reduce the amount of acid produced in the stomach

  • Gas chromatography (GC) and liquid chromatography (LC) with mass spectrometric (MS) detection have been used for the determination of OME, and solid phase extraction (SPE) has often been utilized as a sample preparation technique for extracting OME from plasma samples [3,4]

  • During the last two decades, several sample preparation techniques have been developed and directed towards automation and on-line coupling. Two of these techniques are microextraction by packed sorbent (MEPS) and molecularly imprinted polymer tablets (MIP-Tabs), both of which were developed and introduced by researchers in the Abdel-Rehim group

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Summary

Introduction

Omeprazole (OME) is a well-known drug that is used as a proton pump inhibitor to reduce the amount of acid produced in the stomach. Developing a simple and novel sample preparation technique for measuring the OME in saliva samples is a demanding issue. During the last two decades, several sample preparation techniques have been developed and directed towards automation and on-line coupling Two of these techniques are microextraction by packed sorbent (MEPS) and molecularly imprinted polymer tablets (MIP-Tabs), both of which were developed and introduced by researchers in the Abdel-Rehim group. In our recent work, reduced graphene oxide (GO) materials as a solid phase in the MEPS method, was successfully applied for extraction and measurement of local anesthesia in plasma and saliva samples [18]. GO-Tabs is a novel, straightforward and effective sample preparation trend which will be presented here for extraction of OME from saliva samples and measurement by LC–MS/MS

Chemicals and Reagents
Instrumentation
Preparation of GO-Tabs
Preparation
Sample Preparation
Results and Discussion
GO-Tab
Extraction Time
Type of Desorption Solvent
Effect of pH
Adsorption
Selectivity of theselectivity
Method Validation
Accuracy and Precision
Method Selectivity and Matrix Effects
Carry-Over
Analysis of Patient Samples
Chromatogram
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