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Updated: Oct 15, 2025

Cellular Lipid Extraction for Targeted Stable Isotope Dilution Liquid Chromatography-Mass Spectrometry Analysis
Published on: November 17, 2011
Dispersive liquid-liquid microextraction based on deep eutectic solvent for elemental impurities determination in
Fernanda C Pinheiro1, Miguel Ángel Aguirre2, Joaquim A Nóbrega3
1Group for Applied Instrumental Analysis, Department of Chemistry, Federal University of São Carlos, P.O. Box 676, São Carlos, SP, 13560-270, Brazil; Department of Analytical Chemistry and Food Sciences, University Institute of Materials, Faculty of Science, University of Alicante, P.O. Box 99, 03080, Alicante, Spain.
Abstract:
A simple, fast, sensitive and green pretreatment method for determination of Cd, Co, Hg, Ni, Pb and V in oral and parenteral drug samples using inductively coupled plasma optical emission spectrometry (ICP OES) has been developed. According to United States Pharmacopoeia (USP), those metals must be reported in all pharmaceutical products for quality control evaluation (i.e., elemental impurities from classes 1 and 2A of USP Chapter 232). To improve the analytical capabilities of ICP OES, a dispersive liquid-liquid microextraction (DLLME) has performed using a safe, cheap and biodegradable deep eutectic solvent (DES) as extractant solvent (a mixture of 2:1 M ratio of DL-menthol and decanoic acid). Seven parameters affecting the microextraction efficiency have carefully optimized by multivariate analysis. Under optimized conditions, the DES-based DLLME-ICP OES procedure improved limit of quantitation (LOQ) values on range from 12 to 85-fold and afforded an enrichment factor on average 60-times higher than those obtained to direct ICP OES analysis. Consequently, LOQ values for Cd, Co, Hg, Ni, Pb and V have been on average 10-times lower than target limits recommended for drugs from parenteral route of administration. Trueness has evaluated by addition and recovery experiments following USP recommendations for three oral drug samples in liquid dosage form and three parenteral drugs. Recovery and RSD values have been within the range of 90-109% and 1-6%, respectively. All analytes were below the respectives LOQ values, hence, lower than the limits proposed by USP Chapter 232.
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