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<p>This study examined how particle size, extraction time, and ultrasonication influence fennel essential oil quality using a D-optimal design (19 experiments). Volatile compounds were analyzed via GC/MS, with data evaluated through RSM for single-response optimization and ASCA for multivariate assessment. Single-response optimization considered (1) essence volume and (2) anethole peak area. Essence volume was significantly affected by all three factors and their interactions (particle size × time, size × ultrasound), while anethole yield depended primarily on ultrasonication and its interaction with time. Finer particles (Mesh 50) and shorter extraction times maximized thermally sensitive anethole. Multivariate ASCA of a 19 × 10 metabolite matrix revealed dominant interaction effects (&gt; 130% cumulative variance), overshadowing individual factor contributions. Particle size (12.82%) and extraction time (12.64%) had comparable impacts (<i>p</i> &gt; 0.05), whereas ultrasonication (1.76%) was markedly weaker (<i>p</i> &lt; 0.01). Notably, the size-time interaction explained 63.97% variance (<i>p</i> &lt; 0.001), highlighting non-additive effects: (1) particle size governed time-dependent extraction kinetics, and (2) ultrasonication efficacy depended on parameter combinations (e.g., size × ultrasound: 37.14%; time × ultrasound: 33.13%). Ultrasonication’s effectiveness was system-dependent, improving with smaller particles and optimized extraction times. These findings underscore the need for holistic parameter optimization over isolated adjustments to enhance essential oil quality.</p> Graphical abstract <p></p>

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Multivariate optimization of fennel essential oil extraction: integrating ASCA metabolite profiling with response surface methodology

  • 期刊论文

  • 发表日期：

    2025年10月18日

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  • Mahdi Tavakolizadeh,
  • Leila Moradi,
  • Maryam Khoshkam,
  • Maryam Afshar

摘要

This study examined how particle size, extraction time, and ultrasonication influence fennel essential oil quality using a D-optimal design (19 experiments). Volatile compounds were analyzed via GC/MS, with data evaluated through RSM for single-response optimization and ASCA for multivariate assessment. Single-response optimization considered (1) essence volume and (2) anethole peak area. Essence volume was significantly affected by all three factors and their interactions (particle size × time, size × ultrasound), while anethole yield depended primarily on ultrasonication and its interaction with time. Finer particles (Mesh 50) and shorter extraction times maximized thermally sensitive anethole. Multivariate ASCA of a 19 × 10 metabolite matrix revealed dominant interaction effects (> 130% cumulative variance), overshadowing individual factor contributions. Particle size (12.82%) and extraction time (12.64%) had comparable impacts (p > 0.05), whereas ultrasonication (1.76%) was markedly weaker (p < 0.01). Notably, the size-time interaction explained 63.97% variance (p < 0.001), highlighting non-additive effects: (1) particle size governed time-dependent extraction kinetics, and (2) ultrasonication efficacy depended on parameter combinations (e.g., size × ultrasound: 37.14%; time × ultrasound: 33.13%). Ultrasonication’s effectiveness was system-dependent, improving with smaller particles and optimized extraction times. These findings underscore the need for holistic parameter optimization over isolated adjustments to enhance essential oil quality.

Graphical abstract