Socaciu Carmen, Fetea Florinela, Socaciu Mihai Adrian
Faculty of Food Science and Technology, University of Agricultural Sciences and Veterinary Medicine, 400372 Cluj-Napoca, Romania.
Department of Biotechnology, BIODIATECH-Proplanta Research Centre for Applied Biotechnology in Diagnosis and Molecular Therapy, 400478 Cluj-Napoca, Romania.
Pharmaceuticals (Basel). 2024 Dec 31;18(1):33. doi: 10.3390/ph18010033.
: Pentacyclic triterpenoids, as bioactive phytochemicals, have proven to exhibit significant bioactivity (antioxidant, anti-inflammatory, hypoglycemic, and anticancer) and low cytotoxicity. This study developed convenient methods for extracting and characterizing a birch bark extract enriched in pentacyclic triterpenoids (betulin, betulinic acid, and lupeol) and entrapped in two bioavailable nanoformulations. The performance of ATR-FTIR spectroscopy as a cost-effective and non-destructive method was evaluated comparatively with accurate HPLC-based methods. : The bark extract and pure betulin or betulinic acid were used to obtain PEGylated liposomes and nano lipid carriers (NLCs). Their size was characterized by light scattering diffraction. UV-Vis spectrometry was applied as a preliminary evaluation (1), as well as UHPLC-QTOF-ESI-MS for structure identification (2), ATR-FTIR spectroscopy (for semi-quantitative evaluation) (3), and HPLC-DAD for an accurate quantification of each component, either in the organic solvents or in the nanoformulations (4). : The PEGylated liposomes had smaller sizes, and higher entrapment efficiency, significantly correlated between the three analytical methods. The performance of ATR-FTIR spectroscopy was positively correlated with HPLC-DAD data and confirmed the potential of this cheaper and reliable semi-quantitative method to evaluate the entrapment efficiency of TTs in liposome and NLC nanoformulations. : The results recommend using liposomal nanoformulations for the entrapment of bioactive terpenoids and their characterization by ATR-FTIR after validation by HPLC-DAD. The ATR-FTIR spectroscopy also offers the possibility of screening in a short time different recipes of nanoformulations as well as their stability and bioavailability, which is useful for investigations in vitro and in vivo, which may confirm their efficacy as therapeutic agents.
五环三萜类化合物作为具有生物活性的植物化学物质，已被证明具有显著的生物活性（抗氧化、抗炎、降血糖和抗癌）且细胞毒性低。本研究开发了便捷的方法，用于提取和表征富含五环三萜类化合物（桦木醇、桦木酸和羽扇豆醇）并包封于两种具有生物利用度的纳米制剂中的桦树皮提取物。将衰减全反射傅里叶变换红外光谱（ATR-FTIR）作为一种经济高效且无损的方法与基于高效液相色谱（HPLC）的精确方法进行了比较评估。使用树皮提取物以及纯桦木醇或桦木酸来制备聚乙二醇化脂质体和纳米脂质载体（NLC）。通过光散射衍射对其尺寸进行了表征。紫外-可见光谱法用于初步评估（1），超高效液相色谱-四极杆飞行时间-电喷雾电离质谱（UHPLC-QTOF-ESI-MS）用于结构鉴定（2），ATR-FTIR光谱法用于半定量评估（3），HPLC-二极管阵列检测法（HPLC-DAD）用于精确量化有机溶剂或纳米制剂中的每种成分（4）。聚乙二醇化脂质体尺寸更小，包封效率更高，这三种分析方法之间存在显著相关性。ATR-FTIR光谱法的性能与HPLC-DAD数据呈正相关，并证实了这种更便宜且可靠的半定量方法在评估三萜类化合物在脂质体和NLC纳米制剂中的包封效率方面的潜力。研究结果建议使用脂质体纳米制剂来包封生物活性萜类化合物，并在通过HPLC-DAD验证后通过ATR-FTIR对其进行表征。ATR-FTIR光谱法还提供了在短时间内筛选不同纳米制剂配方及其稳定性和生物利用度的可能性，这对于体外和体内研究很有用，可能会证实它们作为治疗剂的功效。
