Çapraz bağlı kitosan benzofuran schiff bazlarının ve metal komplekslerinin sentezi, karakterizasyonu ve antioksidan etkilerinin incelenmesi
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Dosyalar
Tarih
2023
Yazarlar
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Yayıncı
Hatay Mustafa Kemal Üniversitesi
Erişim Hakkı
info:eu-repo/semantics/openAccess
Özet
Bu çalışmada, düşük ve yüksek molekül ağırlıklı kitosan kullanılarak, Ammi Visnaga bitkisinden izole edilen khellinin alkali ortamda hidroliziyle elde edilen khellinone ile Schiff bazları sentezlenmiştir (HCS-KH, LCS-KH). Sentezlenen Schiff bazları tereftalaldehit (HCS-KH-TA, LCS-KH-TA) ve glutaraldehit (HCS-KH-GA, LCS-KH-GA) kullanılarak çapraz bağlı yapılar elde edilmiştir. Elde edilen çapraz bağlı bileşiklerin Cu (II) ([HCS-KH-TA-CuCl(H2O)], [LCS-KH-TA-CuCl(H2O)], [HCS-KH-GA-CuCl(H2O)], [LCS-KH-GA-CuCl(H2O)]) ve Fe(II) koordinasyon bileşikleri sentezlenmiştir ([HCS-KH-TA-FeCl(H2O)3], [LCS-KH-TA-FeCl(H2O)3], [HCS-KH-GA-FeCl(H2O)3], [LCS-KH-GA-FeCl(H2O)3]). Sentezlenen bileşiklerin yapıları elementel analiz, FT-IR, 13C NMR, SEM ve termal analizle karakterize edilmiştir. Yapılan karakterizasyon çalışmaları sonucunda elde edilen bulgular çapraz bağlı yapıların ve metal komplekslerinin önerilen yapılarını desteklemektedir. Metal komplekslerindeki metal oranları incelendiğinde kitosanın deasetilasyon derecesine bağlı olarak değişen molekül ağırlığının ve kullanılan çapraz bağlayıcının koordine olan metal oranına etkili olduğu görülmüştür. Sentezlenen tüm bileşiklerin DPPH radikal süpürme aktivitesi UV-vis spektrofotometresi ile 517 nm'de ölçülmüştür. Kitosanın değişen molekül ağırlığının, kullanılan çapraz bağlayıcının ve koordine olan metal iyonunun antioksidan aktivite üzerine etkili olduğu görülmüştür. Serbest radikal süpürme aktiviteleri ile ilgili yapılan ölçümler sonucunda düşük molekül ağırlıklarına sahip kitosandan elde edilen türevlerin ve metal komplekslerinin yüksek molekül ağırlıklı kitosan türevlerine ve metal komplekslerine kıyasla daha yüksek süpürme aktivitesi göstermiştir. Çapraz bağlayıcı olarak tereftalaldehit kullanılmasının glutaraldehit kullanılmasına kıyasla antioksidan aktivite açısından avantajlı olduğu ve Cu(II) komplekslerinin Fe(II) komplekslerine kıyasla daha yüksek radikal süpürme yeteneği gösterdiği belirlenmiştir.
In this study, Schiff bases were synthesized with khellinone obtained by hydrolysis of khellin isolated from Ammi Visnaga plant in alkaline medium using low and high molecular weight chitosan (L1, L2). Schiff bases cross-linked structures were obtained by using the synthesized with terephthalaldehyde (HCS-KH-TA, LCS-KH-TA) and glutaraldehyde (HCS-KH-GA, LCS-KH-GA). Cu(II) complexes ([HCS-KH-TA-CuCl(H2O)], [LCS-KH-TA-CuCl(H2O)], [HCS-KH-GA-CuCl(H2O)], [LCS-KH-GA-CuCl(H2O)]) and Fe(II) complexes ([HCS-KH-TA-FeCl(H2O)3], [LCS-KH-TA-FeCl(H2O)3], [HCS-KH-GA-FeCl(H2O)3], [LCS-KH-GA-FeCl(H2O)3]) of cross-linked structures were synthesized. The structures of the synthesized compounds were characterized by elemental analysis, FT-IR, 13C NMR, SEM and thermal analysis. The findings obtained from the characterization studies supporting the proposed structures of the cross-linked structures and metal complexes. When the metal ratios in the metal complexes were examined, it was found that the molecular weight of chitosan, which varies depending on the degree of deacetylation, and the cross-linker affecting the coordinated metal ratio. DPPH radical scavenging activity of all synthesized compounds was measured at 517 nm in UV-vis spectrophotometer. It was observed that varying molecular weight of chitosan, cross-linker used and coordinating metal ion were effective on antioxidant activity. As a result of the free radical scavenging activity measurements, the derivatives and metal complexes obtained from low molecular weight chitosan showed higher scavenging activity compared to high molecular weight chitosan derivatives and metal complexes. It was determined that the use of terephthalaldehyde as a crosslinker was advantageous in terms of antioxidant activity compared to the use of glutaraldehyde and Cu(II) complexes showed higher radical scavenging ability compared to Fe(II) complexes.
In this study, Schiff bases were synthesized with khellinone obtained by hydrolysis of khellin isolated from Ammi Visnaga plant in alkaline medium using low and high molecular weight chitosan (L1, L2). Schiff bases cross-linked structures were obtained by using the synthesized with terephthalaldehyde (HCS-KH-TA, LCS-KH-TA) and glutaraldehyde (HCS-KH-GA, LCS-KH-GA). Cu(II) complexes ([HCS-KH-TA-CuCl(H2O)], [LCS-KH-TA-CuCl(H2O)], [HCS-KH-GA-CuCl(H2O)], [LCS-KH-GA-CuCl(H2O)]) and Fe(II) complexes ([HCS-KH-TA-FeCl(H2O)3], [LCS-KH-TA-FeCl(H2O)3], [HCS-KH-GA-FeCl(H2O)3], [LCS-KH-GA-FeCl(H2O)3]) of cross-linked structures were synthesized. The structures of the synthesized compounds were characterized by elemental analysis, FT-IR, 13C NMR, SEM and thermal analysis. The findings obtained from the characterization studies supporting the proposed structures of the cross-linked structures and metal complexes. When the metal ratios in the metal complexes were examined, it was found that the molecular weight of chitosan, which varies depending on the degree of deacetylation, and the cross-linker affecting the coordinated metal ratio. DPPH radical scavenging activity of all synthesized compounds was measured at 517 nm in UV-vis spectrophotometer. It was observed that varying molecular weight of chitosan, cross-linker used and coordinating metal ion were effective on antioxidant activity. As a result of the free radical scavenging activity measurements, the derivatives and metal complexes obtained from low molecular weight chitosan showed higher scavenging activity compared to high molecular weight chitosan derivatives and metal complexes. It was determined that the use of terephthalaldehyde as a crosslinker was advantageous in terms of antioxidant activity compared to the use of glutaraldehyde and Cu(II) complexes showed higher radical scavenging ability compared to Fe(II) complexes.
Açıklama
Anahtar Kelimeler
Kimya, Chemistry
