In this work, a new method was developed for multi-element determination of Cd and Mn in samples of sugarcane spirit (cachaça) by FAAS using the air-assisted dispersive liquid-liquid microextraction (AA-DLLME). After univariate and multivariate optimizations (mixture design), the experimental conditions were as follows: 5.2 mL of sample at pH 8.5, 0.7 mL 10% (w/v) NaCl solution, 120 μL of trichlorethylene (extraction solvent) containing 1-(2-pyridylazo)-2-naphthol (PAN) at 0.05% (w/v) as chelating agent, six cycles of stirring the mixture with a glass syringe, and 3 min of centrifugation. In these conditions, the calibration curve obtained for Cd was Abs = 0.0158CCd + 0.0333, with R2 0.9951 and for Mn was Abs = 0.0011CMn + 0.0142 and R2 0.9911. The limits of detection, enrichment factor, and consumption index were, respectively, 0.51 μg L−1, 79 and 0.07 mL for Cd, and 1.64 μg L−1, 18, and 0.28 mL for Mn. Precision was evaluated at concentrations of 5 and 10 μg L−1, and RSD% (N = 10) was 0.97% and 6.6% for Cd and 2.8% and 4.5% for Mn, respectively. Addition and recovery tests in samples of Brazilian cachaça were performed to evaluate the accuracy, and recoveries were 87% to 120%, with concentrations found between 1.20 and 3.05 μg L−1 for Cd and between 6.98 and 14.4 μg L−1 for Mn. The developed method proved to be sensitive, efficient, simple, fast, and having low reagent consumption, and of applicability not previously reported in the literature.
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This research was supported by the Fundação de Amparo à Pesquisa do Estado da Bahia (FAPESB), Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq), Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES), Financiadora de Estudos e Projetos (FINEP), and Santa Cruz State University (UESC).
Conflict of Interest
Adrielle S. Fontes has received research grants from Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES). Leonardo B. Guimarães has received research grants from Fundação de Amparo à Pesquisa do Estado da Bahia (FAPESB). Erik G. P. da Silva has received research grants from Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq).
Adrielle S. Fontes declares that she has no conflict of interest. Julia A. Romero declares that she has no conflict of interest. Leonardo B. Guimarães declares that he has no conflict of interest. Erik G. P. da Silva declares that he has no conflict of interest. Daniel de C. Lima declares that he has no conflict of interest.
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Fontes, A.S., Romero, J.C., Guimarães, L.B. et al. Development of Method Based on Dispersive Liquid-Liquid Microextraction Air-Assisted for Multi-Element Determination of Cadmium and Manganese in Sugarcane Spirit (Brazilian cachaça) by FAAS. Food Anal. Methods 13, 222–229 (2020). https://doi.org/10.1007/s12161-019-01600-w
- Mixture design