Rizzi Vito, Matera Sergio, Semeraro Paola, Fini Paola, Cosma Pinalysa
Università degli Studi "Aldo Moro" di Bari, Dipartimento di Chimica Chimica, Via Orabona, 4, 70126 Bari, Italy.
Consiglio Nazionale delle Ricerche CNR-IPCF, UOS Bari, Via Orabona, 4, 70126 Bari, Italy.
Beilstein J Org Chem. 2016 Mar 21;12:549-63. doi: 10.3762/bjoc.12.54. eCollection 2016.
Since several years the inclusion of organic compounds (guests) within the hydrophobic cavity (host) of cyclodextrins (CDs) has been the subject of many investigations. Interestingly, the formation of inclusion complexes could affect the properties of the guest molecules and, for example, the influence of the delivery system can be a method to improve/change the photochemical behavior of the guest. In particular, very recent studies have shown the protective role of CDs preventing the degradation of the encapsulated guest. Starting from this consideration, in this work, only the structure and complexation mode of the inclusion complexes involving 4-thiothymidine (S(4)TdR, a known photosensitizer) and five CDs, namely 2-hydroxypropyl-α-cyclodextrin (2-HP-α-CD), 2-hydroxypropyl-β-cyclodextrin (2-HP-β-CD), 2-hydroxypropyl-γ-cyclodextrin (2-HP-γ-CD), heptakis-(2,6-di-O-methyl)-β-cyclodextrin (DIMEB CD) and heptakis-(2,3,6-tri-O-methyl)-β-cyclodextrin (TRIMEB CD) were investigated by different spectroscopic techniques (UV-vis, FTIR-ATR, (1)H NMR) and cyclic voltammetry analysis (CV). This work is necessary for a prospective research on the photoreactivity of S(4)TdR in aqueous environment and in the presence of CDs to prevent its degradation under irradiation. UV-vis, FTIR-ATR and CV measurements suggested the formation of supramolecular structures involving the employed CDs and mainly the pyrimidine ring of S(4)TdR. (1)H NMR analyses confirmed such indication, unveiling the presence of inclusion complexes. The strongest and deepest interactions were suggested when TRIMEB and DIMEB CDs were studied. The S(4)TdR affinity towards CDs was also evaluated by using the Benesi-Hildebrand (B-H) equation at 25 °C employing CV and (1)H NMR methods. The stoichiometry of the interaction was also inferred and it appears to be 1:1 for all examined CDs.
多年来,将有机化合物(客体)包合在环糊精(CDs)的疏水腔内(主体)一直是众多研究的主题。有趣的是,包合物的形成会影响客体分子的性质,例如,递送系统的影响可能是改善/改变客体光化学行为的一种方法。特别是,最近的研究表明CDs具有防止被包封客体降解的保护作用。基于这一考虑,在本工作中,仅通过不同的光谱技术(紫外可见光谱、傅里叶变换红外衰减全反射光谱、¹H核磁共振)和循环伏安分析(CV)研究了涉及4-硫代胸苷(S(4)TdR,一种已知的光敏剂)与五种CDs,即2-羟丙基-α-环糊精(2-HP-α-CD)、2-羟丙基-β-环糊精(2-HP-β-CD)、2-羟丙基-γ-环糊精(2-HP-γ-CD)、七(2,6-二-O-甲基)-β-环糊精(DIMEB CD)和七(2,3,6-三-O-甲基)-β-环糊精(TRIMEB CD)的包合物的结构和络合模式。这项工作对于前瞻性研究S(4)TdR在水性环境中和存在CDs时的光反应性以防止其在光照下降解是必要的。紫外可见光谱、傅里叶变换红外衰减全反射光谱和循环伏安测量表明形成了涉及所用CDs且主要是S(4)TdR嘧啶环的超分子结构。¹H核磁共振分析证实了这一迹象,揭示了包合物的存在。研究TRIMEB和DIMEB CDs时表明存在最强和最深的相互作用。还通过在25℃下使用循环伏安法和¹H核磁共振方法的贝内西-希尔德布兰德(B-H)方程评估了S(4)TdR对CDs的亲和力。还推断了相互作用的化学计量比,对于所有检测的CDs,其化学计量比似乎均为1:1。