Journal
POLYMERS
Volume 11, Issue 12, Pages -Publisher
MDPI
DOI: 10.3390/polym11122045
Keywords
silk fibroin nanoparticles; cocoon degumming; Bombyx mori; ionic liquids; ultrasound; autoclave
Categories
Funding
- European Commission ERDF/FEDER Operational Programme `Murcia' CCI [Nffi 2007ES161PO001, 14-20/20]
- Spanish MINECO [CTQ2017-87708-R]
- Seneca Foundation of Science and Technology of Murcia, Spain [20977/PI/18]
- ERDF/FEDER Operational Programme 'Murcia' CCI [Nffi 2007ES161PO001, 14-20/20]
- Spanish MINECO (Juan de la Cierva-Formacion) [FJCI-2016-28081]
- program INIA-CCAA (DOC INIA)
- National Institute for Agricultural and Food Research and Technology (INIA)
- Spanish State Research Agency (AEI) under the Spanish Ministry of Economy, Industry and Competitiveness
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Several studies have stated that the process used for sericin removal, or degumming, from silk cocoons has a strong impact in the silk fibroin integrity and consequently in their mechanical or biochemical properties after processing it into several biomaterials (e.g. fibers, films or scaffolds) but still, there is a lack of information of the impact on the features of silk nanoparticles. In this work, silk cocoons were degummed following four standard methods: autoclaving, short alkaline (Na2CO3) boiling, long alkaline (Na2CO3) boiling and ultrasounds. The resultant silk fibroin fibers were dissolved in the ionic liquid 1-ethyl-3-methylimidazolium acetate and used for nanoparticle synthesis by rapid desolvation in polar organic solvents. The relative efficiencies of the degumming processes and the integrity of the resulting fibroin fibers obtained were analyzed by mass loss, optical microscopy, thermogravimetric analysis, infrared spectroscopy and SDS-PAGE. Particle sizes and morphology were analyzed by Dynamic Light Scattering and Field Emission Scanning Electronic Microscopy. The results showed that the different treatments had a remarkable impact on the integrity of the silk fibroin chains, as confirmed by gel electrophoresis, which can be correlated with particle mean size and size distribution changes. The smallest nanoparticles (156 +/- 3 nm) and the most negative Z potential (-30.2 +/- 1.8 mV) were obtained with the combination of long treatment (2 h) of boiling in alkaline solution (Na2CO3 0.02 eq/L). The study confirms that parameters of the process, such as composition of the solution and time of the degumming step, must be controlled in order to reach an optimum reproducibility of the nanoparticle production.
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