Dispersive liquid–liquid microextraction of Cd, Hg and Pb from medicines prior to ICP OES determination according to the United States Pharmacopeia
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Title: | Dispersive liquid–liquid microextraction of Cd, Hg and Pb from medicines prior to ICP OES determination according to the United States Pharmacopeia |
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Authors: | Pinheiro, Fernanda C. | Aguirre Pastor, Miguel Ángel | Nóbrega, Joaquim A. | Canals, Antonio |
Research Group/s: | Espectroscopía Atómica-Masas y Química Analítica en Condiciones Extremas |
Center, Department or Service: | Universidad de Alicante. Departamento de Química Analítica, Nutrición y Bromatología | Universidad de Alicante. Instituto Universitario de Materiales |
Keywords: | Dispersive liquid-liquid microextraction | United States Pharmacopeia | Cd | Hg | Pb | Drug samples | ICP-OES |
Knowledge Area: | Química Analítica |
Issue Date: | 10-Nov-2021 |
Publisher: | Royal Society of Chemistry |
Citation: | Analytical Methods. 2021, 13: 5670-5678. https://doi.org/10.1039/D1AY01566D |
Abstract: | A simple, sensitive and matrix-effect free analytical method for simultaneous determination of Cd, Hg and Pb in drug samples (i.e., commercial dosage tablets) by inductively coupled plasma optical emission spectrometry (ICP OES) has been developed. According to the United States Pharmacopeia (USP) Chapter 232, those metals are considered elemental impurities from class 1 and they must be assessed in pharmaceutical production as well as in quality control evaluation. In order to increase the sensitivity of the analysis, dispersive liquid–liquid microextraction (DLLME) was performed and seven factors affecting analyte extraction were optimized by multivariate analysis. A microvolume of analyte enriched phase was directly introduced into the plasma using a multi-nebulizer, providing a high enrichment factor. When compared to conventional ICP OES analysis, DLLME improves the limit of quantitation (LOQ) values on average 40-fold for all analytes. Consequently, LOQ values were significantly lower than their permissible daily exposure limits for oral drugs. Accuracy was evaluated by addition and recovery experiments following USP recommendations in eight commercial drug samples. Recovery and RSD values were within the range of 90–108% and 1–9%, respectively. |
Sponsor: | The authors are grateful to the Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq, process no. 141634/2017-0, 202722/2019-8, 305201/2018-2 and 428558/2018-6), the Regional Government of Valencia (Spain) (PROMETEO/2018/087) for the financial support, Agilent Technologies Inc. for the loan of the ICP OES spectrometer, and Ingeniatrics for the MultiNeb® provided. This study was financed in part by the Coordenaçao de Aperfeiçoamento de Pessoal de Nível Superior – Brasil (CAPES) – Finance Code 001. The authors extend their appreciation to Ministry of Science, Innovation and Universities for granting the Spanish Network of Excellence in Sample Preparation (RED2018-102522-T). This article is based upon work from the Sample Preparation Study Group and Network, supported by the Division of Analytical Chemistry of the European Chemical Society. |
URI: | http://hdl.handle.net/10045/119854 |
ISSN: | 1759-9660 (Print) | 1759-9679 (Online) |
DOI: | 10.1039/D1AY01566D |
Language: | eng |
Type: | info:eu-repo/semantics/article |
Rights: | © The Royal Society of Chemistry 2021 |
Peer Review: | si |
Publisher version: | https://doi.org/10.1039/D1AY01566D |
Appears in Collections: | INV - SP-BG - Artículos de Revistas |
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File | Description | Size | Format | |
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Pinheiro_etal_2021_AnalMethods_final.pdf | Versión final (acceso restringido) | 722,33 kB | Adobe PDF | Open Request a copy |
Pinheiro_etal_2021_AnalMethods_preprint.pdf | Preprint (acceso abierto) | 800,35 kB | Adobe PDF | Open Preview |
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