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Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme

View Article: PubMed Central - PubMed

ABSTRACT

Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, 29Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g−1 in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3.

No MeSH data available.


FTIR spectra of pure lysozyme (a) and lysozyme loaded on FDU-12-H200 (b).
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Figure 7: FTIR spectra of pure lysozyme (a) and lysozyme loaded on FDU-12-H200 (b).

Mentions: The structural stability of the lysozyme immobilized into the pores of FDU12-200H was confirmed through Fourier transform infrared (FTIR) absorption studies. Here, a comparison is drawn between pure lysozyme protein and the lysozyme immobilized into the silica matrix. As can be seen in figure 7(a), the FTIR spectra show distinct amide I and amide II bands, which are characteristic of the structure of the enzyme depicting the confirmation of the α-helical and β-sheets of the lysozyme. The amide I of the lysozyme, which is observed near 1650 cm−1, is attributed to the most sensitive part of the spectral region given by the C=O stretching of the peptide linkages. The amide II found near 1520 cm−1 is attributed to the NH bending vibrations of the lysozyme molecule. It is also evident from figure 7(b) that the two amide bands are observed near 1650 and 1550 cm−1. It is seen that the intensity ratio of the amide bands in both pure lysozyme and the lysozyme immobilized into the FDU-12 matrix is almost same, which reveals that the lysozyme molecules are quite stable as seen through the secondary structures such as the α-helical and β-sheets of the immobilized enzyme [32].


Quick high-temperature hydrothermal synthesis of mesoporous materials with 3D cubic structure for the adsorption of lysozyme
FTIR spectra of pure lysozyme (a) and lysozyme loaded on FDU-12-H200 (b).
© Copyright Policy - open-access
Related In: Results  -  Collection

License 1 - License 2
Show All Figures
getmorefigures.php?uid=PMC5036462&req=5

Figure 7: FTIR spectra of pure lysozyme (a) and lysozyme loaded on FDU-12-H200 (b).
Mentions: The structural stability of the lysozyme immobilized into the pores of FDU12-200H was confirmed through Fourier transform infrared (FTIR) absorption studies. Here, a comparison is drawn between pure lysozyme protein and the lysozyme immobilized into the silica matrix. As can be seen in figure 7(a), the FTIR spectra show distinct amide I and amide II bands, which are characteristic of the structure of the enzyme depicting the confirmation of the α-helical and β-sheets of the lysozyme. The amide I of the lysozyme, which is observed near 1650 cm−1, is attributed to the most sensitive part of the spectral region given by the C=O stretching of the peptide linkages. The amide II found near 1520 cm−1 is attributed to the NH bending vibrations of the lysozyme molecule. It is also evident from figure 7(b) that the two amide bands are observed near 1650 and 1550 cm−1. It is seen that the intensity ratio of the amide bands in both pure lysozyme and the lysozyme immobilized into the FDU-12 matrix is almost same, which reveals that the lysozyme molecules are quite stable as seen through the secondary structures such as the α-helical and β-sheets of the immobilized enzyme [32].

View Article: PubMed Central - PubMed

ABSTRACT

Three-dimensional cage-like mesoporous FDU-12 materials with large tuneable pore sizes ranging from 9.9 to 15.6 nm were prepared by varying the synthesis temperature from 100 to 200 °C for the aging time of just 2 h using a tri-block copolymer F-127(EO106PO70EO106) as the surfactant and 1,3,5-trimethyl benzene as the swelling agent in an acidic condition. The mesoporous structure and textural features of FDU-12-HX (where H denotes the hydrothermal method and X denotes the synthesis temperature) samples were elucidated and probed using x-ray diffraction, N2 adsorption, 29Si magic angle spinning nuclear magnetic resonance, scanning electron microscopy and transmission electron microscopy. It has been demonstrated that the aging time can be significantly reduced from 72 to 2 h without affecting the structural order of the FDU-12 materials with a simple adjustment of the synthesis temperature from 100 to 200 °C. Among the materials prepared, the samples prepared at 200 °C had the highest pore volume and the largest pore diameter. Lysozyme adsorption experiments were conducted over FDU-12 samples prepared at different temperatures in order to understand their biomolecule adsorption capacity, where the FDU-12-HX samples displayed high adsorption performance of 29 μmol g−1 in spite of shortening the actual synthesis time from 72 to 2 h. Further, the influence of surface area, pore volume and pore diameter on the adsorption capacity of FDU-12-HX samples has been investigated and results are discussed in correlation with the textural parameters of the FDU-12-HX and other mesoporous adsorbents including SBA-15, MCM-41, KIT-5, KIT-6 and CMK-3.

No MeSH data available.