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<p>This research addresses the development of a methodology, based on a sample suspension in tetramethylammonium hydroxide (TMAH) with the aid of ultrasonic energy, for the determination of Ca, Fe, Mg, Mn, and Zn in spirulina samples sold as powdered food supplement by flame atomic absorption spectrometry. The variables were optimized using Doehlert design and desirability function. The developed method presented quantification limits of 29, 12, 3.8, 0.039, and 1.8&#xa0;mg Kg<sup>−1</sup>, respectively, for Ca, Fe, Mg, Mn, and Zn. Accuracy was assessed by addition/recovery tests, comparison with another method adopted as a standard (acid digestion in a digestion block) and analysis of certified reference material (Apple leaves—NIST 1515, Bovine liver—NIST 1577c) and Lobster hepatopancreas (NRC Tort-3). The concentrations of Ca, Fe, Mg, Mn, and Zn found in spirulina samples were in the ranges of 680 to 1827, 712 to 1508, 307 to 321, 41.1 to 61.1, and 20.5 to 33.0&#xa0;mg Kg<sup>−1</sup>, respectively.</p>

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Doehlert Design in the Optimization of a Method for Determining Metals in Spirulina (Arthrospira sp.) Samples Based on a Tetramethylammonium Hydroxide Suspension

  • 期刊论文

  • 发表日期：

    2025年3月31日

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  • Uillian Mozart Ferreira Mata Cerqueira,
  • Lais Silva Gomes,
  • Marcos Almeida Bezerra,
  • Cleber Galvão Novaes,
  • Sulene Alves Araújo,
  • Anderson Santos Souza,
  • Walter Nei Lopes dos Santos

摘要

This research addresses the development of a methodology, based on a sample suspension in tetramethylammonium hydroxide (TMAH) with the aid of ultrasonic energy, for the determination of Ca, Fe, Mg, Mn, and Zn in spirulina samples sold as powdered food supplement by flame atomic absorption spectrometry. The variables were optimized using Doehlert design and desirability function. The developed method presented quantification limits of 29, 12, 3.8, 0.039, and 1.8 mg Kg−1, respectively, for Ca, Fe, Mg, Mn, and Zn. Accuracy was assessed by addition/recovery tests, comparison with another method adopted as a standard (acid digestion in a digestion block) and analysis of certified reference material (Apple leaves—NIST 1515, Bovine liver—NIST 1577c) and Lobster hepatopancreas (NRC Tort-3). The concentrations of Ca, Fe, Mg, Mn, and Zn found in spirulina samples were in the ranges of 680 to 1827, 712 to 1508, 307 to 321, 41.1 to 61.1, and 20.5 to 33.0 mg Kg−1, respectively.