Utilizing Plackett–Burman and Box–Behnken Designs for Plant Extract–Based AgNP Synthesis Optimization: Unveiling Antifungal Potential Against Phytophthora Species

Muharrem Türkkan

doi:10.18016/ksutarimdoga.vi.1523681

EN TR

Utilizing Plackett–Burman and Box–Behnken Designs for Plant Extract–Based AgNP Synthesis Optimization: Unveiling Antifungal Potential Against Phytophthora Species

Abstract

This study optimized a green synthesis method for silver nanoparticles (AgNPs) using aqueous extracts of black tea, linden, cherry laurel, kale, and melocan, employing a statistical design of experiments. The plant extracts acted as bio-reducing agents. Total and individual phenolic compounds in the extracts were quantified using ultraviolet-visible (UV–Vis) spectroscopy and ultra-high-performance liquid chromatography (UHPLC). AgNP yields were maximized through a combination of Plackett–Burman and Box–Behnken designs. The synthesized AgNPs were characterized by UV–Vis spectroscopy, Fourier transform infrared (FT–IR) spectroscopy, scanning electron microscopy (SEM) coupled with energy-dispersive X-ray spectroscopy (EDS), and transmission electron microscopy (TEM). Optimal AgNP production was achieved under the following conditions (determined by response surface methodology, RSM): 9.6 g of plant material, extraction heating at 80°C for 20 minutes, 10 mM AgNO3, 2.5 mL of extract, 800 W microwave irradiation, and a 90-second reaction time. FT–IR analysis confirmed the role of phenolic compounds in reducing and stabilizing AgNPs. The resulting AgNPs exhibited uniform spherical morphology, with average particle sizes of 5.30 nm (black tea), 8.74 nm (linden), 7.20 nm (cherry laurel), 6.32 nm (kale), and 9.44 nm (melocan). Antifungal assays against five Phytophthora species revealed that kale-derived AgNPs were most potent, with EC50, MIC, and MFC values ranging from 9.28–30.84 µg mL−1, 200–300 µg mL−1, and 200–400 µg mL−1, respectively. These results suggest that plant-extract-synthesized AgNPs offer a sustainable approach to managing Phytophthora diseases, warranting further research.

Keywords

Bitki Ekstraktı Bazlı AgNP Sentez Optimizasyonu için Plackett–Burman ve Box–Behnken Tasarımlarının Kullanımı: Phytophthora Türlerine Karşı Antifungal Potansiyelinin Ortaya Çıkarılması

Öz

Bu çalışma, siyah çay, ıhlamur, karayemiş, yaprak lahana ve melocan sulu ekstraktları kullanılarak gümüş nanoparçacıklar (AgNP’ler) için deneysel bir istatistiksel tasarım ile yeşil bir sentez yöntemini optimize etmiştir. Bu bitki ekstraktları biyo-indirgeyici ajanlar olarak işlev görmüştür. Ekstraktlardaki toplam ve bireysel fenolik bileşikler ultraviyole-görünür (UV–Vis) spektroskopi ve ultra yüksek performansli sivi kromatografisi (UHPLC) kullanılarak ölçülmüştür. AgNP verimleri, Plackett‒Burman ve Box‒Behnken tasarımlarının bir kombinasyonu ile maksimize edilmiştir. Sentezlenen AgNP’ler UV‒Vis spektroskopisi, Fourier dönüşümlü kizilötesi (FT–IR) spektroskopisi, taramali elektron mikroskobu (SEM)-enerji dağilimli X-ışını spektroskopisi (EDS) ve geçirimli elektron mikroskopisi (TEM) ile karakterize edilmiştir. Optimum AgNP üretimi aşağıdaki koşullar altında elde edilmiştir (yanıt yüzey metodolojisi, RSM ile belirlenmiştir): 9.6 g bitki materyali, 80°C’de 20 dakika ekstraksiyon ısıtma, 10 mM AgNO3, 2.5 mL ekstrakt, 800 W mikrodalga irritasyonu ve 90 saniyelik reaksiyon süresi. FT–IR analizi, fenolik bileşiklerin AgNP indirgenmesi ve stabilize edilmesindeki rolünü göstermiştir. Elde edilen AgNP’ler 5.30 nm (siyah çay), 8.74 nm (ıhlamur), 7.20 nm (karayemiş), 6.32 nm (yaprak lahana) ve 9.44 nm (melocan) ortalama partikül boyutları ile tek tip küresel morfoloji sergilemiştir. Beş Phytophthora türüne karşı yapılan antifungal deneyler, yaprak lahana türevi AgNP’lerin sırasıyla 9.28-30.84 µg mL−1, 200-300 µg mL−1 ve 200-400 µg mL−1 arasında değişen EC50, MIC ve MFC değerleri ile en güçlü olduğunu ortaya koymuştur. Bu sonuçlar, bitki ekstraktı ile sentezlenen AgNP’lerin Phytophthora hastalıkların yönetiminde sürdürülebilir bir yaklaşım sunduğunu ve daha fazla araştırılması gerektiğini göstermektedir.

Anahtar Kelimeler

Supporting Institution

Ordu Üniversitesi BAP

Project Number

B2209

Thanks

The author is grateful to Dr. İlker Kurbetli for supplying the Phytophthora isolates, Dr. Umut Ateş for performing high-performance liquid chromatography (HPLC) analysis of the total phenolic content and individual phenolic compounds in the plant extracts, and Dr. Hamdi Güray Kutbay for confirming the identification of melocan (Smilax excelsa L.).

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Details

Primary Language

English

Subjects

Phytopathology

Journal Section

Research Article

Authors

Muharrem Türkkan ^*
0000-0001-7779-9365
Türkiye

Early Pub Date

March 20, 2025

Publication Date

March 27, 2025

Submission Date

July 28, 2024

Acceptance Date

February 17, 2025

Published in Issue

Year 2025 Volume: 28 Number: 2

DOI

https://doi.org/10.18016/ksutarimdoga.vi.1523681

IZ

https://izlik.org/JA83KT66KB

Cite

RIS / Bibtex

APA

Türkkan, M. (2025). Utilizing Plackett–Burman and Box–Behnken Designs for Plant Extract–Based AgNP Synthesis Optimization: Unveiling Antifungal Potential Against Phytophthora Species. Kahramanmaraş Sütçü İmam Üniversitesi Tarım Ve Doğa Dergisi, 28(2), 516-534. https://doi.org/10.18016/ksutarimdoga.vi.1523681

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Application of response surface methodology for green synthesis of silver nanoparticles using Prunus mahaleb L.

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