Emülsiyon elektroeğirme yöntemiyle bazı tıbbi aromatik bitkilerin yağlarının akıllı polimerlerle nanolif yapısında enkapsülasyonu, enkapsülasyonun karakterizasyonu ve enkapsüle etken maddelerin kontrollü salım kinetiklerinin modellenmesi
Yükleniyor...
Dosyalar
Tarih
2022
Yazarlar
Dergi Başlığı
Dergi ISSN
Cilt Başlığı
Yayıncı
Hatay Mustafa Kemal Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu çalışmada tıbbi aromatik bitkilerden (TAB) fesleğen, biberiye, kekik, kimyon ve zencefil yağlarının emülsiyon elektroeğirme yöntemi ile akıllı polimerler kullanılarak nanolif yapısında enkapsüle edilmesi, elde edilen enkapsülasyonun karakterize edilmesi ve elektroeğirmenin yağların antimikrobiyal özelliklerine, uçucu bileşenlerine etkilerinin ve in vitro biyoyararlılıklarının belirlenmesi üzerine çalışılmıştır. Araştırmanın ilk aşamasında tıbbi aromatik bitki yağları (TABY) ve bu yağların enkapsüle edilmesi amacıyla hazırlanan besleme emülsiyonlarında (BE) elektriksel iletkenlikleri, dielektrik özellikleri, viskozite değerleri, gram negatif olan E. coli, S. Enteridis ve gram pozitif olan L. monocytogenes ve L. rhamnosus bakterilerine karşı antimikrobiyal aktiviteleri ve TABY'nın gaz kromatografisi kütle spektrometresi (GK-KS) ile uçucu bileşenleri belirlenmiştir. İkinci aşamada ise TABY'nın emülsiyon elektroeğirme tekniği kullanılarak enkapsüle edilen nanolif yapısındaki materyallerin karakterize edilmesi, in vitro biyoyararlanımının belirlenmesi ve salım kinetiğinin matematiksel olarak modellenmesi amacıyla, materyallerin morfolojik karakterizasyonu taramalı elektron mikroskobu (SEM), materyaldeki moleküler etkileşimler ve yapay mide ortamındaki in vitro salım şekilleri Fourier dönüşümlü infrared spektrometresi (FTIR) ile belirlenmiştir. Çalışmanın ilk aşamasında elde edilen sonuçlara göre; TABY'nın iletkenlikleri 1.58±0.01-14±0.01 mS/cm arasında değişirken, BE'nın iletkenliği 1.64±0.01–4.88±0.01 mS/cm arasında olduğu; TABY'nın dielektrik değerleri 3.65±0.21-12.56±0.01 arasında değişirken, BE'nın dielektrik değerleri 10.78±0.27-23.91±0.07 arasında olduğu; TABY'nın viskozite değerleri 58.63±5.56-99.52±7.52 mPa.s arasında değişirken, BE'nın viskozite değerleri 74.44±3.28-93.72±12.42 mPa.s arasında olduğu ve TABY'nda yapılan antimikrobiyal test sonuçlarına göre; yalnızca biberiye ve kekik yağlarının gram negatif olan E. coli ve S. Enteridis'te de gram pozitif olan L. monocytogenes ve L. rhamnosus'a kıyasla daha düşük inhibisyon zon çapı oluşturduğu görülmüştür. GK-KS analizlerine göre, fesleğen, kimyon, biberiye, kekik ve zencefil yağlarında sırasıyla 14, 19, 35, 24 ve 31 adet bileşen tespit edilmiştir. TABY'larda belirlenen majör bileşenler ise sırasıyla estragol (%33.06), küminaldehit (%19.97), α-pinen (%10.72), timol (%50.68) ve fenipentol (%20.37) olarak bulunmuştur. Çalışmanın ikinci aşamasında elde edilen sonuçlara göre; yapılan SEM analizlerinde lif çapları 253±46 - 464±107 nm arasında iken en düşük ve en yüksek lif çapları kekik ve zencefil yağı içeren örneklerde belirlenmiştir. Yağsız-kontrol örneğinde ise lif çapı 801±157 nm olarak belirlenmiş olup beslemede yağ bulunmasıyla lif çaplarının istatistiki açıdan önemli derecede düştüğü tespit edilmiştir. Ayrıca TABY'nda bulunan antimikrobiyal karakterleri bileşenlerin varlığı ve üretilen liflerin çaplarının da 253-322 nm seviyelerine düşürülmüş olmasına rağmen üretilen liflerin zon çapı oluşturmadığı görülmüştür. Normal şartlarda pH-hassas polimerler olarak seçilen zein, jelatin ve hyaluronik asitin gastrik pH seviyesinde sıkılaşarak intestinal pH seviyesinde şişme ve enkapsüle ettiği bileşenlerin salımına uygun hale geldiği bilinse de bu polimerlerin üçlü kombinasyonu ile üretilen liflerin pH hassas özellikleri olması beklenenin tersi yönünde özellik göstermeye başlayarak gastrik/asidik pH seviyelerinde şişme ve çekirdek materyalin salımını teşvik eden, intestinal/bazik pH seviyelerinde ise büzülüp kapanarak salımın önüne geçen bir hale gelmiştir. FTIR spektrumlarından elde edilen verilere göre, yapay mide ortamında gerçekleştirilen sindirimin üretilen liflerin çapları ile ters orantılı olarak ilerlediği, lif çapı düştükçe moleküler kırılımların daha kolay sağlandığı ve sindirimin daha kolay gerçekleşmesine katkı sağladığı gözlenmiştir. Dahası, pH-hassas özelliği ters yönde etki eden polimerlerin asidik pH seviyelerinde şişerek esansiyel bileşen salımının daha elverişli hale geldiği; bazik pH seviyesinde ise büzüşerek salımı engellemesi ile de liflerde yapılan antimikrobiyal testlerde sonuç alınamadığı düşünülmektedir. Salım davranışları da incelendiğinde; yalnızca kekik ve zencefil yağlı liflerin sindirimi sonucu ortama salımında Fickian difüzyonun baskın olduğu (n<0.43); fesleğen yağı ve biberiye yağı içeren liflerin sindirimi sonrası ortama salınmasında tüm modellerde yüksek oranda R2 değerleri bulunsa da bu iki örneğin de akış davranış katsayısı n>0.85 değerinden yüksek olduğundan her iki örnekte de salımın sıfırıncı dereceden gerçekleştiği belirlenmiştir. Hixson-Crowell modeline göre salım kinetikleri incelendiğinde de Peppas denklemi ile yakın R2 değerleri belirlense de bu sefer n değerlerine göre zencefil ve kekik yağlı örneklerle beraber fesleğen yağlı örnekte gerçekleşen salımın da Fickian difüzyonun baskın olduğu (n<0.43) görülmekte iken; kimyon ve biberiye yağlı örneklerde ise Fickian olmayan difüzyon (0.43
In this study, basil, rosemary, thyme, cumin and ginger oils from medicinal aromatic plants (MAP) were encapsulated in nanofiber structure using smart polymers by emulsion electrospinning method, the encapsulation was characterized and the effects of electrospinning on the antimicrobial properties, volatile components of the oils, and their in vitro bioavailability were determined. In the first stage of the research, electrical conductivity, dielectric properties, viscosity values of MAP oils and the prepared feed emulsions (FE); antimicrobial activities against gram-negative E. coli, S. Enteridis and gram-positive L. monocytogenes and L. rhamnosus bacteria; and volatile components of MAP oils by gas chromatography mass spectrometry (GC-MS) were determined. In the second stage of the research, the morphological characterization of the materials was carried out by scanning electron microscopy (SEM) in order to characterize the nanofiber materials encapsulated by the emulsion electrospinning technique. Moreover, the in vitro bioavailability and the release kinetics mathematically modelling were also investigated. In vitro release patterns were determined by Fourier transform infrared spectrometry (FTIR). According to the results obtained in the first stage of the study; the conductivity of MAP oils varied between 1.58±0.01-14±0.01 mS/cm, while the conductivity of FE was between 1.64±0.01-4.88±0.01 mS/cm. While the dielectric values of MAP oils varied between 3.65±0.21-12.56±0.01, the dielectric values of FE were between 10.78±0.27-23.91±0.07. While the viscosity values of MAP oils vary between 58.63±5.56-99.52±7.52 mPa.s, the viscosity values of FE vary between 74.44±3.28-93.72±12.42 mPa.s. According to the antimicrobial test results in MAP oils; only rosemary and thyme oils were found to produce a lower inhibition zone diameter in gram-negative E. coli and S. Enteridis compared to gram-positive L. monocytogenes and L. rhamnosus. According to GC-MS analysis, 14, 19, 35, 24 and 31 components were determined in basil, cumin, rosemary, thyme and ginger oils, respectively. Besides, the major components in the oils were determined as estragole (33.06%), cuminaldehyde (19.97%), α-pinene (10.72%), thymol (50.68%) and phenipentol (20.37%), respectively. According to the results obtained in the second stage of the study; In the SEM analyzes performed, the fiber diameters were between 253±46 - 464±107 nm, while the lowest and highest fiber diameters were determined in the samples containing thyme and ginger oil. In the lean-control sample, the fiber diameter was determined as 801±157 nm, and it was determined that the effect of added oils on reducing the diameters was statistically significant. In addition, it was observed that the produced fibers did not form a zone diameter, although the presence of components with antimicrobial characters in MAP oils and the diameters of the produced fibers were reduced to 253-322 nm. Although it is known that zein, gelatin and hyaluronic acid, which are selected as pH-sensitive polymers under normal conditions, tighten at the gastric pH level and become suitable for swelling at the intestinal pH level and the release of the encapsulated components, the pH-sensitive properties of the fibers produced by the triple combination of these polymers begin to show the opposite of what is expected to be as pH sensitive properties. According to the data obtained from the FTIR spectra, it was observed that the digestion carried out in the artificial stomach environment progressed inversely with the diameters of the fibers produced, and as the fiber diameter decreased, molecular breakdowns were provided more easily and contributed to the easier digestion. Moreover, the pH-sensitive properties of the adversely affecting polymers swell at acidic pH levels, making essential component release more favorable: at basic pH level, it is thought that antimicrobial tests on the fibers could not yield results because it prevents the release by shrinkage. When the release behaviors are examined; only thyme and ginger oily fibers were digested and released to the environment by Fickian diffusion (n<0.43); Although there were high R2 values in all models in the release of fibers containing basil oil and rosemary oil into the environment after digestion, since the flow behavior coefficient of these two samples was higher than n>0.85, it was determined that the release occurred in both samples with the zero order kinetics. When the release kinetics were examined according to the Hixson-Crowell model, although close R2 values were determined with the Peppas equation, this time it was observed that Fickian diffusion was dominant (n<0.43) in the release that took place in the basil oil samples together with the ginger and thyme oil samples according to the n values. On the other hand, in the cumin and rosemary oil samples, non-Fickian diffusion (0.43
In this study, basil, rosemary, thyme, cumin and ginger oils from medicinal aromatic plants (MAP) were encapsulated in nanofiber structure using smart polymers by emulsion electrospinning method, the encapsulation was characterized and the effects of electrospinning on the antimicrobial properties, volatile components of the oils, and their in vitro bioavailability were determined. In the first stage of the research, electrical conductivity, dielectric properties, viscosity values of MAP oils and the prepared feed emulsions (FE); antimicrobial activities against gram-negative E. coli, S. Enteridis and gram-positive L. monocytogenes and L. rhamnosus bacteria; and volatile components of MAP oils by gas chromatography mass spectrometry (GC-MS) were determined. In the second stage of the research, the morphological characterization of the materials was carried out by scanning electron microscopy (SEM) in order to characterize the nanofiber materials encapsulated by the emulsion electrospinning technique. Moreover, the in vitro bioavailability and the release kinetics mathematically modelling were also investigated. In vitro release patterns were determined by Fourier transform infrared spectrometry (FTIR). According to the results obtained in the first stage of the study; the conductivity of MAP oils varied between 1.58±0.01-14±0.01 mS/cm, while the conductivity of FE was between 1.64±0.01-4.88±0.01 mS/cm. While the dielectric values of MAP oils varied between 3.65±0.21-12.56±0.01, the dielectric values of FE were between 10.78±0.27-23.91±0.07. While the viscosity values of MAP oils vary between 58.63±5.56-99.52±7.52 mPa.s, the viscosity values of FE vary between 74.44±3.28-93.72±12.42 mPa.s. According to the antimicrobial test results in MAP oils; only rosemary and thyme oils were found to produce a lower inhibition zone diameter in gram-negative E. coli and S. Enteridis compared to gram-positive L. monocytogenes and L. rhamnosus. According to GC-MS analysis, 14, 19, 35, 24 and 31 components were determined in basil, cumin, rosemary, thyme and ginger oils, respectively. Besides, the major components in the oils were determined as estragole (33.06%), cuminaldehyde (19.97%), α-pinene (10.72%), thymol (50.68%) and phenipentol (20.37%), respectively. According to the results obtained in the second stage of the study; In the SEM analyzes performed, the fiber diameters were between 253±46 - 464±107 nm, while the lowest and highest fiber diameters were determined in the samples containing thyme and ginger oil. In the lean-control sample, the fiber diameter was determined as 801±157 nm, and it was determined that the effect of added oils on reducing the diameters was statistically significant. In addition, it was observed that the produced fibers did not form a zone diameter, although the presence of components with antimicrobial characters in MAP oils and the diameters of the produced fibers were reduced to 253-322 nm. Although it is known that zein, gelatin and hyaluronic acid, which are selected as pH-sensitive polymers under normal conditions, tighten at the gastric pH level and become suitable for swelling at the intestinal pH level and the release of the encapsulated components, the pH-sensitive properties of the fibers produced by the triple combination of these polymers begin to show the opposite of what is expected to be as pH sensitive properties. According to the data obtained from the FTIR spectra, it was observed that the digestion carried out in the artificial stomach environment progressed inversely with the diameters of the fibers produced, and as the fiber diameter decreased, molecular breakdowns were provided more easily and contributed to the easier digestion. Moreover, the pH-sensitive properties of the adversely affecting polymers swell at acidic pH levels, making essential component release more favorable: at basic pH level, it is thought that antimicrobial tests on the fibers could not yield results because it prevents the release by shrinkage. When the release behaviors are examined; only thyme and ginger oily fibers were digested and released to the environment by Fickian diffusion (n<0.43); Although there were high R2 values in all models in the release of fibers containing basil oil and rosemary oil into the environment after digestion, since the flow behavior coefficient of these two samples was higher than n>0.85, it was determined that the release occurred in both samples with the zero order kinetics. When the release kinetics were examined according to the Hixson-Crowell model, although close R2 values were determined with the Peppas equation, this time it was observed that Fickian diffusion was dominant (n<0.43) in the release that took place in the basil oil samples together with the ginger and thyme oil samples according to the n values. On the other hand, in the cumin and rosemary oil samples, non-Fickian diffusion (0.43
Açıklama
Anahtar Kelimeler
Gıda Mühendisliği, Food Engineering
