<p>Ultrasound-assisted extraction (UAE) offers a faster and eco-friendly alternative for samples prepared for essential mineral determination in foods. This study aims to validate a UAE method for sample preparation to determine Ca, Mg, Zn, Na, and K in organic dairy products using flame atomic absorption spectroscopy (FAAS) and confocal microscopy was used as one parameter to evaluate the efficiency of process. Commercial organic milk, yogurt, and cheese were analyzed. For experiments, a face-centered experimental design to optimize acid volume (5 and 10&#xa0;mL) and ultrasonic bath temperature (45 and 70&#xa0;°C) are used. Optimal conditions were identified for each sample type, and a <i>t</i>-test showed no significant differences in mineral content between the UAE (30&#xa0;min) and traditional wet mineralization in digestion block (4&#xa0;h) procedures for the majority of samples. The validated method carried out by UAE demonstrated satisfactory linearity (R<sup>2</sup> &gt; 0.98), repeatability (RSD &lt; 10%), and inter-day precision (RSD &lt; 8%). Fortified samples showed mineral recovery within the validation range for Ca (82–95%), Mg (85–96%), Zn (92–102%), K (97–109%), and Na (84–102%). Similar recovery rates were achieved in a certified reference material (CRM NIST 1549) evaluated. Confocal microscopy confirmed that UAE effectively degraded organic matter for essential mineral determination. Overall, the UAE proved effective for sample preparation for mineral determination in organic dairy samples, offering time efficiency, reduced solvent use, and reliable results.</p>

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Ultrasound-Assisted Extraction for Essential Minerals in Organic Dairy Matrices and Confocal Microscopy Application

  • Augusto César Costa-Santos,
  • Eduardo Adilson Orlando,
  • Ana Paula Rebellato,
  • Maria Cristina Ferreira Zambom,
  • Gisele Marcondes Luz,
  • Venancio Ferreira Moraes-Neto,
  • Elem Tamirys dos Santos Caramês,
  • Nathan Hargreaves Noguera,
  • Amanda Silva do Carmo,
  • Mirna Lúcia Gigante,
  • Márcia Miguel Castro Ferreira,
  • Juliana Azevedo Lima Pallone

摘要

Ultrasound-assisted extraction (UAE) offers a faster and eco-friendly alternative for samples prepared for essential mineral determination in foods. This study aims to validate a UAE method for sample preparation to determine Ca, Mg, Zn, Na, and K in organic dairy products using flame atomic absorption spectroscopy (FAAS) and confocal microscopy was used as one parameter to evaluate the efficiency of process. Commercial organic milk, yogurt, and cheese were analyzed. For experiments, a face-centered experimental design to optimize acid volume (5 and 10 mL) and ultrasonic bath temperature (45 and 70 °C) are used. Optimal conditions were identified for each sample type, and a t-test showed no significant differences in mineral content between the UAE (30 min) and traditional wet mineralization in digestion block (4 h) procedures for the majority of samples. The validated method carried out by UAE demonstrated satisfactory linearity (R2 > 0.98), repeatability (RSD < 10%), and inter-day precision (RSD < 8%). Fortified samples showed mineral recovery within the validation range for Ca (82–95%), Mg (85–96%), Zn (92–102%), K (97–109%), and Na (84–102%). Similar recovery rates were achieved in a certified reference material (CRM NIST 1549) evaluated. Confocal microscopy confirmed that UAE effectively degraded organic matter for essential mineral determination. Overall, the UAE proved effective for sample preparation for mineral determination in organic dairy samples, offering time efficiency, reduced solvent use, and reliable results.