Desenvolvimento de métodos para a determinação de Pb, Cd, Cr, Ni e Sb em cosméticos faciais por espectrometria de absorção atômica em forno de grafite de alta resolução com fonte contínua empregando amostragem direta de sólidos
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Data
2016-08-23
Autores
Barros, Ariane Isis [UNESP]
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Universidade Estadual Paulista (Unesp)
Resumo
Este trabalho relata o desenvolvimento de métodos para a determinação de Pb, Cd, Cr, Ni e Sb em cosméticos faciais por espectrometria de absorção atômica em forno de grafite de alta resolução com fonte contínua (HR-CS GF AAS) empregando análise direta de amostras sólidas. Essa técnica foi utilizada devido a sua alta capacidade para a correção de fundo baseada em algoritmos dos mínimos quadrados. Para a determinação de Pb e Sb, interferências causadas por moléculas de SiO(g) nas linhas 283,306 nm (Pb), 217,582 nm (Sb) e 231,147 nm (Sb) foram eliminadas pela aplicação do método de correção de fundo pelos mínimos quadrados (LSBC). Para a correção de fundo na determinação de Pb, o espectro de referência foi gerado a partir de SiO2. Diferentes precursores foram avaliados para geração do espectro de referência para a correção de fundo na determinação de Sb, sendo a zeólita e a mica os precursores mais eficazes. Efeitos de matriz foram avaliados pela comparação das massas características e inclinações das curvas obtidas em padrões aquosos e amostras (ou material de referência certificado). Calibrações com padrões aquosos foram possíveis e curvas com bom coeficiente de correlação (r>0,99) foram obtidas para todos os analitos. Os limites de detecção foram de 0,06 mg kg -1 Pb, 3,67 µg kg-1 Cd, 0,5 mg kg-1 Cr, 0,292 mg kg-1 Ni e 0,32 mg kg-1 Sb. As concentrações dos analitos encontradas em amostras comerciais de blush, sombra de olho e pó compacto variaram de 1,0 – 27,08 mg kg-1 Pb, 5,06 – 198,20 µg kg-1 Cd, 2,87 – 23,65 mg kg-1 Cr, 1,36 – 12,09 mg kg-1 Ni e 9,14 – 14,52 mg kg-1 Sb. A exatidão foi checada pela análise de material de referência certificado (CRM) de solo, testes de adição e recuperação e/ou método comparativo. As concentrações encontradas no CRM foram concordantes com os valores certificados ao nível de 95% de confiança (teste t). Recuperações variaram de 99 – 108 % (Pb), 86 – 115 % (Cd), 105 – 115 % (Cr), 83 – 106 % (Ni) e 82 – 108 % (Sb). Os resultados para Cd e Pb determinados com os métodos propostos foram concordantes com os obtidos com os métodos comparativos, ao nível de 95% de confiança (teste t-pareado).
This work reports on the development of methods for determination of Pb, Cd, Cr, Ni and Sb in facial cosmetics by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) employing direct solid sample analysis. This technique was used due to the high capability for background correction based on least-squares algorithm. For Pb and Sb determinations, interferences caused by SiO(g) molecule at the lines 283.306 nm (Pb), 217.582 nm (Sb) and 231.147 nm (Sb) were eliminated by applying the least-squares background correction (LSBC). For background correction in the determination of Pb, a reference spectrum was generated from SiO2. Different precursors were evaluated to generate reference spectra for correction of the background in the determination of Sb, been zeolite and mica the most effective precursors. Matrix effects were evaluated by comparing the characteristics masses and slopes of curves in aqueous standards and sample (or certified reference material). Calibration with aqueous standards were possible, and curves with good correlation coefficients (r>0.99) were attained for all analytes. The limits of detection were 0.06 mg kg-1 Pb, 3.67 µg kg-1 Cd, 0.5 mg kg-1 Cr, 0.292 mg kg-1 Ni and 0.32 mg kg-1 Sb. The found concentrations of analytes in commercial blush, eye shadow and compact powder samples were within 1.0 – 27.08 mg kg-1 Pb, 5.06 – 198.20 µg kg-1 Cd, 2.87 – 23.65 mg kg-1 Cr, 1.36 – 12.09 mg kg-1 Ni, and 9.14 – 14.52 mg kg-1 Sb. Accuracy was checked by analyzing soil certified reference materials (CRM), addition and recovery tests and/or comparative method. The concentrations found in CRM were in agreement with certified values at a 95% confidence level (t-test). Recoveries were in the 99 – 108 % (Pb), 86 – 115 % (Cd), 105 – 115 % (Cr), 83 – 106 % (Ni) and 82 – 108 % (Sb) intervals. Results for Cd and Pb determined with the proposed method were in agreement with those obtained by the comparative method at a 95% confidence level (paired t-test).
This work reports on the development of methods for determination of Pb, Cd, Cr, Ni and Sb in facial cosmetics by high-resolution continuum source graphite furnace atomic absorption spectrometry (HR-CS GF AAS) employing direct solid sample analysis. This technique was used due to the high capability for background correction based on least-squares algorithm. For Pb and Sb determinations, interferences caused by SiO(g) molecule at the lines 283.306 nm (Pb), 217.582 nm (Sb) and 231.147 nm (Sb) were eliminated by applying the least-squares background correction (LSBC). For background correction in the determination of Pb, a reference spectrum was generated from SiO2. Different precursors were evaluated to generate reference spectra for correction of the background in the determination of Sb, been zeolite and mica the most effective precursors. Matrix effects were evaluated by comparing the characteristics masses and slopes of curves in aqueous standards and sample (or certified reference material). Calibration with aqueous standards were possible, and curves with good correlation coefficients (r>0.99) were attained for all analytes. The limits of detection were 0.06 mg kg-1 Pb, 3.67 µg kg-1 Cd, 0.5 mg kg-1 Cr, 0.292 mg kg-1 Ni and 0.32 mg kg-1 Sb. The found concentrations of analytes in commercial blush, eye shadow and compact powder samples were within 1.0 – 27.08 mg kg-1 Pb, 5.06 – 198.20 µg kg-1 Cd, 2.87 – 23.65 mg kg-1 Cr, 1.36 – 12.09 mg kg-1 Ni, and 9.14 – 14.52 mg kg-1 Sb. Accuracy was checked by analyzing soil certified reference materials (CRM), addition and recovery tests and/or comparative method. The concentrations found in CRM were in agreement with certified values at a 95% confidence level (t-test). Recoveries were in the 99 – 108 % (Pb), 86 – 115 % (Cd), 105 – 115 % (Cr), 83 – 106 % (Ni) and 82 – 108 % (Sb) intervals. Results for Cd and Pb determined with the proposed method were in agreement with those obtained by the comparative method at a 95% confidence level (paired t-test).
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Palavras-chave
Cosméticos Faciais, HR-CS GF AAS, Análise direta de sólidos, LSBC, Facial Cosmetics, Direct solid sampling