Yüzey aktif madde destekli propolis ekstraksiyonu ve elde edilen ekstrelerin bazı biyolojik aktivitelerinin belirlenmesi
Küçük Resim Yok
Tarih
2025
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
İnönü Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu çalışmada, propolisten fenolik bileşiklerin ekstraksiyonu için su içinde yağ (O/W) ve yağ içinde su (W/O) emülsiyonlarının çevreci ve etkili çözücüler olarak kullanılmasının olanakları araştırılmıştır. Deneysel tasarım ve istatistiksel optimizasyon için yanıt yüzeyi yöntemi (Box-Behnken tasarımı) kullanılmıştır ve bağımsız değişkenler olan emülsifiyer oranı, ekstraksiyon süresi ve yağ/su oranı parametreleri, yanıt olarak toplam fenolik madde (TFM) miktarına karşı optimize edilmiştir. Karşılaştırma amacıyla; su (S+P), ayçiçek yağı (A+P) ve %70 etanol (E+P) ile elde edilen ekstreler kullanılmıştır. Ekstrelerde TFM ve ABTS/DPPH radikal süpürme aktiviteleri spektrofotometrik olarak, fenolik bileşim ise sıvı kromatografisi-yüksek çözünürlüklü kütle spektrometrisi (LC-HRMS) ile belirlenmiştir. Emülsiyon kullanılarak elde edilen ekstrelerin fiziksel karakterizasyonu gerçekleştirilmiş ve oksidatif kararlılıkları standart antioksidanlarla oluşturulan emülsiyonlarla karşılaştırmalı olarak belirlenmiştir. Çalışmanın son bölümünde, optimum koşullarda elde edilen ekstreler, salata sosu ve kakaolu fındık kreması formülasyonlarına ilave edilerek bu ürünlerin fonksiyonel özellikleri, duyusal beğeni düzeyleri ve fenoliklerin in vitro biyogeçişliliği incelenmiştir. Elde edilen sonuçlarda örneklerin TFM, ABTS ve DPPH değerleri arasında istatistiksel olarak önemli farklılıklar olduğu tespit edilmiştir (P<0.05). En yüksek TFM değeri O/W+P örneğinde gözlenmiş ve E+P'ye göre %18, A+P'ye göre %58 ve S+P'ye göre %830 daha fazla fenolik maddenin ekstrakte edildiği tespit edilmiştir. Radikal süpürme aktivitesi bakımından O/W+P, W/O+P ve E+P örneklerinin en yüksek değerleri gösterdiği ve bunları A+P ve S+P örneklerinin takip ettiği görülmüştür. Ekstrelerin fenolik bileşimleri incelendiğinde ise Naringenin, kafeik asit, diosmetin, kumarik asit ve galangin bakımından zengin olduğu ve en yüksek değerlerin O/W+P, W/O+P örneklerinde ölçüldüğü görülmüştür. Oksidatif stabilite çalışmalarında, peroksitlerin miktarının 30 günlük inkübasyon sonunda O/W+P örneğinde 1000 ppm askorbik asit içeren emülsiyona göre %86, 200 ppm ?-tokoferol içeren emülsiyona göre de %83 daha az olduğu görülmüştür. Benzer şekilde W/O+P örneğinde ölçülen hidroperoksit miktarı tokoferol örneğinden %55, askorbik asit örneğinden %48 daha düşük olarak ölçülmüştür. İkincil oksidasyon ürünlerinin göstergesi olan TBARS testinde de bu sonuçlara paralel sonuçlar alınmıştır. Emülsifiye propolis ekstresi ile zenginleştirilen salata sosu ve kakaolu fındık kreması örneklerinde artan propolis ekstresi ile örneklerin TFM, ABTS ve DPPH değerlerinde istatistiksel olarak önemli artış olduğu tespit edilmiştir (P<0.05). Yapılan duyusal değerlendirmede, 150 ppm O/W+P ilavesinin salata sosunda belirgin bir koku/aroma değişimi meydana getirmediği ve kontrol örneğine göre daha yüksek "genel kabul edilebilirlik" değerleri gösterdiği tespit edilmiştir. Kakaolu fındık kremasında ise W/O +P formunda ilave edilen 35 ppm propolisin, lezzette belirgin bir değişime sebep olmadığı gibi görünüş ve renk bakımından da kontrole göre daha iyi skorlar aldığı görülmüştür. Sonuç olarak, bu çalışma, O/W ve W/O emülsiyonlarının propolisten fenolik bileşiklerin ekstraksiyonunu ve gerçek gıda uygulamalarını önemli ölçüde iyileştirebileceğini göstermektedir. Geleneksel çözücülerle karşılaştırıldığında, bu çalışmada kullanılan emülsiyonlar daha yüksek geri kazanım, daha yüksek antioksidan aktivite ve tatmin edici duyusal özellikler sunmakta ve temiz etiketli gıda formülasyonları için umut vermektedir.
In this study, the feasibility of utilizing oil-in-water (O/W) and water-in-oil (W/O ) emulsions as green, effective solvents for extracting phenolic compounds from propolis was evaluated. Response surface methodology (Box-Behnken design) was employed for experimental design and statistical optimization of emulsifier ratio, extraction time and oil/water ratio as independent variables against total phenolic content (TFM) as the response. For comparison, extracts obtained with water (S+P), sunflower oil (A+P) and 70% ethanol (E+P) were used. TFM and ABTS/DPPH radical scavenging activities in the extracts were determined spectrophotometrically, whereas phenolic composition was revealed by liquid chromatography-high resolution mass spectrometry (LC-HRMS). The physical properties of the extracts obtained using the emulsions were characterized and their oxidative stability was determined comparatively with emulsions prepared with standard antioxidants. In the last stage of the study, the extracts obtained under optimum conditions were added to salad dressing and cocoa hazelnut spread formulations and the functional properties, sensory acceptability and in vitro bioaccessibility of phenolics in these products were studied. According to the results, it was determined that there were statistically significant differences between the TFM, ABTS and DPPH values of the samples (P<0.05). The O/W+P sample yielded the highest TPC, which was 18%, 58%, and 830% higher compared to E+P, A+P, and S+P, respectively (P<0.05). In terms of radical scavenging activity, it was observed that O/W+P, W/O +P and E+P samples showed the highest values and followed by A+P and S+P samples. Upon analyzing the phenolic compositions of the extracts, it was observed that they exhibited a high concentration of naringenin, caffeic acid, diosmetin, coumaric acid, and galangin. Notably, the highest values were recorded in the O/W+P and W/O +P samples. In oxidative stability studies, it was observed that the amount of peroxides was 86% lower in the O/W+P sample compared to the emulsion containing 1000 ppm ascorbic acid and 83% lower than the emulsion containing 200 ppm ?-tocopherol after 30 days of incubation. Likewise, the amount of hydroperoxide measured in the W/O +P sample was 55% lower than the tocopherol sample and 48% lower than the ascorbic acid sample. Parallel results were obtained in the TBARS test, which is an indicator of secondary oxidation products. It was determined that there was a statistically significant increase in the TFM, ABTS and DPPH values of the samples with increasing propolis extract in the salad dressing and cocoa hazelnut cream samples fortified with emulsified propolis extract (P<0.05). In the sensory evaluation, it was determined that the addition of 150 ppm O/W+P did not cause a substantial alteration in the odor/aroma profile of the salad dressing. Furthermore, the resulting sample exhibited higher "general acceptability" values in comparison to the control sample. In the cocoa hazelnut cream formulation, the addition of 35 ppm propolis in the form of W/O +P did not significantly alter the flavor profile. On the other hand, the propolis-infused cream exhibited superior visual and color characteristics compared to the control group. Overall, this study demonstrates that O/W and W/O emulsions can significantly improve the extraction and real world application of phenolic compounds from propolis. Compared to traditional solvents, these emulsions offer higher recovery, enhanced antioxidant activity, and satisfactory sensory properties, making them promising candidates for clean-label food formulations.
In this study, the feasibility of utilizing oil-in-water (O/W) and water-in-oil (W/O ) emulsions as green, effective solvents for extracting phenolic compounds from propolis was evaluated. Response surface methodology (Box-Behnken design) was employed for experimental design and statistical optimization of emulsifier ratio, extraction time and oil/water ratio as independent variables against total phenolic content (TFM) as the response. For comparison, extracts obtained with water (S+P), sunflower oil (A+P) and 70% ethanol (E+P) were used. TFM and ABTS/DPPH radical scavenging activities in the extracts were determined spectrophotometrically, whereas phenolic composition was revealed by liquid chromatography-high resolution mass spectrometry (LC-HRMS). The physical properties of the extracts obtained using the emulsions were characterized and their oxidative stability was determined comparatively with emulsions prepared with standard antioxidants. In the last stage of the study, the extracts obtained under optimum conditions were added to salad dressing and cocoa hazelnut spread formulations and the functional properties, sensory acceptability and in vitro bioaccessibility of phenolics in these products were studied. According to the results, it was determined that there were statistically significant differences between the TFM, ABTS and DPPH values of the samples (P<0.05). The O/W+P sample yielded the highest TPC, which was 18%, 58%, and 830% higher compared to E+P, A+P, and S+P, respectively (P<0.05). In terms of radical scavenging activity, it was observed that O/W+P, W/O +P and E+P samples showed the highest values and followed by A+P and S+P samples. Upon analyzing the phenolic compositions of the extracts, it was observed that they exhibited a high concentration of naringenin, caffeic acid, diosmetin, coumaric acid, and galangin. Notably, the highest values were recorded in the O/W+P and W/O +P samples. In oxidative stability studies, it was observed that the amount of peroxides was 86% lower in the O/W+P sample compared to the emulsion containing 1000 ppm ascorbic acid and 83% lower than the emulsion containing 200 ppm ?-tocopherol after 30 days of incubation. Likewise, the amount of hydroperoxide measured in the W/O +P sample was 55% lower than the tocopherol sample and 48% lower than the ascorbic acid sample. Parallel results were obtained in the TBARS test, which is an indicator of secondary oxidation products. It was determined that there was a statistically significant increase in the TFM, ABTS and DPPH values of the samples with increasing propolis extract in the salad dressing and cocoa hazelnut cream samples fortified with emulsified propolis extract (P<0.05). In the sensory evaluation, it was determined that the addition of 150 ppm O/W+P did not cause a substantial alteration in the odor/aroma profile of the salad dressing. Furthermore, the resulting sample exhibited higher "general acceptability" values in comparison to the control sample. In the cocoa hazelnut cream formulation, the addition of 35 ppm propolis in the form of W/O +P did not significantly alter the flavor profile. On the other hand, the propolis-infused cream exhibited superior visual and color characteristics compared to the control group. Overall, this study demonstrates that O/W and W/O emulsions can significantly improve the extraction and real world application of phenolic compounds from propolis. Compared to traditional solvents, these emulsions offer higher recovery, enhanced antioxidant activity, and satisfactory sensory properties, making them promising candidates for clean-label food formulations.
Açıklama
Anahtar Kelimeler
Gıda Mühendisliği, Food Engineering











