Fractional Factorial Design-Guided Optimization of Flavonoid Content and Antioxidant Capacity in Justicia gendarussa Leaf Extracts and UHPLC-HRMS-Based Metabolite Characterization

Background/Objectives: Extraction conditions can influence the chemical profile and antioxidant properties of medicinal plant extracts. This study aimed to optimize ethanol-based extraction of Justicia gendarussa leaves and characterize the optimized extract through UHPLC-HRMS metabolite profiling, with application to cultivated plant materials. Methods: A two-level half-fractional factorial design was used to assess the effects of five extraction factors—liquid-to-solid ratio, temperature, ethanol concentration, extraction time, and pH—on three response variables: total flavonoid content (TFC), DPPH radical-scavenging activity, and ferric reducing antioxidant power (FRAP). The optimized condition was validated experimentally, characterized by UHPLC-Q Exactive Plus Orbitrap HRMS with data-dependent MS/MS, and applied to cultivated leaf and stem materials under six fertilization treatments, analyzed using two-way ANOVA (organ × treatment). Results: The liquid-to-solid ratio × temperature interaction was the dominant determinant of TFC, and the liquid-to-solid ratio alone dominated both DPPH and FRAP. Desirability-based optimization identified a condition of 100 mL g−1 liquid-to-solid ratio, 30 °C, 20% ethanol, 30 min, and pH 2. Confirmatory extraction resulted in 16.43 ± 0.30 mg QE g−1 DW TFC, 12.30 ± 0.02 µmol TE g−1 DW DPPH, and 190.56 ± 2.58 µmol TE g−1 DW FRAP, in close agreement with model predictions (0.10–1.54% error). UHPLC-HRMS/MS detected 52 putatively annotated metabolites, including a candidate gendarusin A/B (apigenin di-C-arabinoside)-type C-glycosylflavone. Leaves showed significantly higher TFC, CUPRAC, and FRAP than stems regardless of fertilization treatment (organ effect p < 0.0001), whereas the leaf–stem difference in DPPH capacity varied significantly with treatment (interaction p = 0.0010). Conclusions: These findings provide a validated extraction condition for the measured responses and support further targeted metabolite evaluation of J. gendarussa.

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Journal
Pharmaceuticals
Published
2026-09-16
DOI
https://doi.org/10.3390/ph19091466
Primary Topic
Plant-derived Lignans Synthesis and Bioactivity
Type
article
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article

Fractional Factorial Design-Guided Optimization of Flavonoid Content and Antioxidant Capacity in Justicia gendarussa Leaf Extracts and UHPLC-HRMS-Based Metabolite Characterization

Viktória Poór, I Made Artika, Ulfa Elfiah, Endre Kristóf et al.
Pharmaceuticals
Plant-derived Lignans Synthesis and Bioactivity
article

Fractional Factorial Design-Guided Optimization of Flavonoid Content and Antioxidant Capacity in Justicia gendarussa Leaf Extracts and UHPLC-HRMS-Based Metabolite Characterization

Viktória Poór, I Made Artika, Ulfa Elfiah, Endre Kristóf, Tamás Marosvölgyi, Waras Nurcholis, Syarifah Iis Aisyah, Rini Arianti, Gyath Karadsheh, Aditya Kurniawan, Gendhis Mahestri Handiani
article en

Abstract

Background/Objectives: Extraction conditions can influence the chemical profile and antioxidant properties of medicinal plant extracts. This study aimed to optimize ethanol-based extraction of Justicia gendarussa leaves and characterize the optimized extract through UHPLC-HRMS metabolite profiling, with application to cultivated plant materials. Methods: A two-level half-fractional factorial design was used to assess the effects of five extraction factors—liquid-to-solid ratio, temperature, ethanol concentration, extraction time, and pH—on three response variables: total flavonoid content (TFC), DPPH radical-scavenging activity, and ferric reducing antioxidant power (FRAP). The optimized condition was validated experimentally, characterized by UHPLC-Q Exactive Plus Orbitrap HRMS with data-dependent MS/MS, and applied to cultivated leaf and stem materials under six fertilization treatments, analyzed using two-way ANOVA (organ × treatment). Results: The liquid-to-solid ratio × temperature interaction was the dominant determinant of TFC, and the liquid-to-solid ratio alone dominated both DPPH and FRAP. Desirability-based optimization identified a condition of 100 mL g−1 liquid-to-solid ratio, 30 °C, 20% ethanol, 30 min, and pH 2. Confirmatory extraction resulted in 16.43 ± 0.30 mg QE g−1 DW TFC, 12.30 ± 0.02 µmol TE g−1 DW DPPH, and 190.56 ± 2.58 µmol TE g−1 DW FRAP, in close agreement with model predictions (0.10–1.54% error). UHPLC-HRMS/MS detected 52 putatively annotated metabolites, including a candidate gendarusin A/B (apigenin di-C-arabinoside)-type C-glycosylflavone. Leaves showed significantly higher TFC, CUPRAC, and FRAP than stems regardless of fertilization treatment (organ effect p < 0.0001), whereas the leaf–stem difference in DPPH capacity varied significantly with treatment (interaction p = 0.0010). Conclusions: These findings provide a validated extraction condition for the measured responses and support further targeted metabolite evaluation of J. gendarussa.

PharmaceuticalsVol. 19(9)
University of Debrecen (HU), IPB University (ID), Universitas Jember (ID), University of Pecs (HU)
Openalex Percentile: Top 18%
Plant-derived Lignans Synthesis and Bioactivity
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