Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DAD
<b>Background/Objectives</b>: 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 characteriz...
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2024-12-01
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| author | Carmen Socaciu Florinela Fetea Mihai Adrian Socaciu |
| author_facet | Carmen Socaciu Florinela Fetea Mihai Adrian Socaciu |
| author_sort | Carmen Socaciu |
| collection | DOAJ |
| description | <b>Background/Objectives</b>: 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. <b>Methods</b>: 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<sup>+</sup>-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). <b>Results</b>: 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. <b>Conclusions</b>: 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. |
| format | Article |
| id | doaj-art-dd4a89c9c8914876b9c41a5cb3affc90 |
| institution | Kabale University |
| issn | 1424-8247 |
| language | English |
| publishDate | 2024-12-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Pharmaceuticals |
| spelling | doaj-art-dd4a89c9c8914876b9c41a5cb3affc902025-01-24T13:45:05ZengMDPI AGPharmaceuticals1424-82472024-12-011813310.3390/ph18010033Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DADCarmen Socaciu0Florinela Fetea1Mihai Adrian Socaciu2Faculty of Food Science and Technology, University of Agricultural Sciences and Veterinary Medicine, 400372 Cluj-Napoca, RomaniaFaculty of Food Science and Technology, University of Agricultural Sciences and Veterinary Medicine, 400372 Cluj-Napoca, RomaniaDepartment of Biotechnology, BIODIATECH—Proplanta Research Centre for Applied Biotechnology in Diagnosis and Molecular Therapy, 400478 Cluj-Napoca, Romania<b>Background/Objectives</b>: 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. <b>Methods</b>: 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<sup>+</sup>-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). <b>Results</b>: 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. <b>Conclusions</b>: 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.https://www.mdpi.com/1424-8247/18/1/33pentacyclic triterpenoidsPEGylated liposomesnano lipid carriersdiffraction light scatteringATR–Fourier-transform infrared spectroscopyhigh-performance liquid chromatography |
| spellingShingle | Carmen Socaciu Florinela Fetea Mihai Adrian Socaciu Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DAD Pharmaceuticals pentacyclic triterpenoids PEGylated liposomes nano lipid carriers diffraction light scattering ATR–Fourier-transform infrared spectroscopy high-performance liquid chromatography |
| title | Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DAD |
| title_full | Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DAD |
| title_fullStr | Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DAD |
| title_full_unstemmed | Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DAD |
| title_short | Synthesis and Characterization of PEGylated Liposomes and Nanostructured Lipid Carriers with Entrapped Bioactive Triterpenoids: Comparative Fingerprints and Quantification by UHPLC-QTOF-ESI<sup>+</sup>-MS, ATR-FTIR Spectroscopy, and HPLC-DAD |
| title_sort | synthesis and characterization of pegylated liposomes and nanostructured lipid carriers with entrapped bioactive triterpenoids comparative fingerprints and quantification by uhplc qtof esi sup sup ms atr ftir spectroscopy and hplc dad |
| topic | pentacyclic triterpenoids PEGylated liposomes nano lipid carriers diffraction light scattering ATR–Fourier-transform infrared spectroscopy high-performance liquid chromatography |
| url | https://www.mdpi.com/1424-8247/18/1/33 |
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