Graphic abstract
In this study, the extraction of oil from pinecone of
Pinus brutia
was evaluated by supercritical CO
2
(Sc-CO
2
) and Soxhlet extraction methods. The quercetin, rutin and kaempferol (QRK) contents of oil were analyzed one by one via HPLC. The rutin compound investigated in this study has the potential to be a drug against the COVID 19 virus. SEM and BET analysis were performed to observe the structural change and increase in surface area after Sc-CO
2
extraction. The operating conditions were investigated in the range of 35–65 °C temperatures, 140–220 bar of pressures, 0.30–1.00 mm of mean particle sizes, 3–7 l/min of CO
2
flow rates, 0–8% w/w co-solvent and 30–150 min extraction periods. When the results obtained by the Sc-CO
2
method were compared with the results of Soxhlet extraction method, the maximum recovery of total QRK was found 4.18% in co-solvent-free studies and 30.94% in co-solvent-added Sc-CO
2
studies. Sc-CO
2
extraction results of Q, R, and K were found as 14.75 ± 1.08 µg/g, 14.23 ± 1.27 µg/g, and 15.70 ± 1.13 µg/g pinecone, respectively. Soxhlet extraction results of Q, R, and K were found as 36.43 ± 2.26 μg/g, 57.19 ± 3.81 μg/g, and 50.80 ± 2.79 μg/g pinecone, respectively. The maximum amount of QRK was found as 44.68 ± 2.89 μg/g pinecone by Sc-CO
2
method via adding 8% ethanol by mass and as 144.42 ± 5.39 μg/g pinecone by Soxhlet method. According to the reference Soxhlet method efficiency, the Sc-CO
2
extraction recovery was found as 30.94%.
Supplementary Information
The online version contains supplementary material available at 10.1007/s11696-021-01644-5.
In this study, extract of elaeagnus angistofolia seed was obtained by supercritical carbon dioxide solvent method and measured the amount of quercetin by using HPLC equipped with UV detector. Experimental results were analyzed by using "Design Expert 7.0 (demo)" program. Increasing temperature and pressure at about extraction conditions caused a significant increase of quercetin amount. Particle size and extraction period parameters was studied parametrically at the start of this study and identified these parameters according to maximize amount of quercetin. After parametric experiments, the small particle size 0.5 mm and experiment period 120 min were found suitable for this study. After identification of these parameters, experimental design conditions identified by response surface design method were used to optimize pressure and temperature, we optimized temperature and pressure parameters as 65°C and 311 bar to maximize quercetin amount. Maximum oil amount was measured 48.68 mg/g sample. After checking experiments of optimum conditions provided by design method, quercetin amount was found experimentally 9.44 µg quercetin /100 g sample, it was considerably approximate value and favourably to model for estimated 9.49 µg quercetin /100 g sample by Design Expert 7.0 (demo) program.
Bu çalışmada Ardıç bitkisi meyvelerinden deneysel tasarım yöntemiyle tasarlanan ekstraksiyon deneyleri gerçekleştirilmiş ve ekstraktlar içerisindeki Silibinin ve Rutin bileşiklerinin miktarları araştırılmıştır. Ardıç bitkisi geleneksel tıpta yüz yıllardır tedavi amaçlı olarak kullanıldığı için bilimsel çalışmalarda üzerinde araştırmaların yoğunlukla yapılan bir bitkidir. Geleneksel tıpta idrar söktürücü, iltihap önleyici, ağrı kesici, karaciğer koruyucu, anti mikrobiyal ve anti bakteriyel etkileri bilinmektedir. Bağımsız parametreler olan Etanol/su oranı ve özütleme süresinin aktif madde verimlerine etkisi, Design Expert 11 (Demo) programı kullanılarak tasarlanmış ve araştırılmıştır. Soxhlet yöntemi için özütte bulunan silibinin ve rutin etken maddelerinin maksimum miktarını veren matematiksel modeller elde edilmiştir. Çalışmada elde edilen modellerin önerdiği optimum çalışma koşulları ile deneysel sonuçların uyumlu olduğu görülmüştür. Deneysel çalışmaların sonucu olarak ardıç meyvelerinde en yüksek silibinin ve rutin miktarları sırasıyla 17,9 μg/g ve 261,8 μg/g bulunmuştur.
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