Synthesis and Characterization of Mesoporous Silica Nanoparticles

Stӧber nanoparticles and mesoporous silica nanoparticles of different shapes and pore structures were generated as previously described in the literature^{17 (link),19 (link),27 (link),38 (link)–40 (link)}. MSNs were made via a hydrolytic sol gel method under base catalytic conditions and using cationic surfactant as structure directing agent and porogen, and TEOS (Sigma-Aldrich) as silica precursor. The specific procedures for synthesis of bare MSNs, as well as functionalization of stellate MSNs by polyethylene glycol (PEG) and nickel charged nitrilotriacetic acid (NiNTA), are described in the supporting information (SI). Upon washing and surfactant extraction, all resulting MSNs were resuspended in pure ethanol and passed through a 1 µm glass filter (Millipore-Sigma) to remove any residual aggregates. Size and zeta potential were assessed using a Zetasizer instrument (Malvern Instruments, Ltd.) and morphology was assessed by TEM (JEOL 2010).

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LaBauve A.E., Saada E.A., Jones I.K., Mosesso R., Noureddine A., Techel J., Gomez A., Collette N., Sherman M.B., Serda R.E., Butler K.S., Brinker C.J., Schoeniger J.S., Sasaki D, & Negrete O.A. (2023). Lipid-coated mesoporous silica nanoparticles for anti-viral applications via delivery of CRISPR-Cas9 ribonucleoproteins. Scientific Reports, 13, 6873.

Publication 2023

Zetasizer instrument

Catalytic Cationic Ethanol Hydrolytic Msns Nickel Nitrilotriacetic acid Polyethylene glycol Silica Surfactant Synthesis

Corresponding Organization :

Other organizations : Sandia National Laboratories California, University of New Mexico, Lawrence Livermore National Laboratory, The University of Texas Medical Branch at Galveston, Sandia National Laboratories

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Variable analysis

independent variables

Stӧber nanoparticles and mesoporous silica nanoparticles (MSNs) of different shapes and pore structures

dependent variables

Size and zeta potential of the resulting MSNs
Morphology of the resulting MSNs

control variables

Hydrolytic sol gel method under base catalytic conditions
Use of cationic surfactant as structure directing agent and porogen
Use of TEOS (Sigma-Aldrich) as silica precursor
Washing and surfactant extraction of the resulting MSNs
Resuspension of the resulting MSNs in pure ethanol and filtration through a 1 µm glass filter (Millipore-Sigma) to remove any residual aggregates

controls

No positive or negative controls were explicitly mentioned in the provided information.

Annotations

Based on most similar protocols

Optimized synthesis conditions: The synthesis of MSNs is carried out under base catalytic conditions using CTAB as a structure directing agent and porogen, and TEOS as a silica precursor (Input protocol). The specific procedures for the synthesis of bare MSNs, as well as their functionalization with PEG and NiNTA, are described in the supporting information (Input protocol).

Validation steps: The size and zeta potential of the resulting MSNs are assessed using a Zetasizer instrument, and the morphology is analyzed by TEM (Input protocol). Additionally, the pore diameter, surface area, and pore volume of the functionalized MSNs are characterized by BET and BJH methods (Protocol 4).

Comparison of protocols: The protocols vary in terms of the specific reagents used, reaction conditions (temperature, duration, stirring), and the methods employed for surfactant removal and particle functionalization. For example, Protocol 2 uses DMSO and APTES for amino-functionalization, while Protocol 5 utilizes 3,3-dithiodipropionic acid, EDC, and NHS for the preparation of MSN-S-S-COOH and MSN-S-S-CS.

Reproducibility enhancement: To ensure full reproducibility, the lab notes should record the exact amounts and concentrations of all reagents, the precise reaction temperatures and durations, the details of the centrifugation and washing steps, and the specific parameters used for characterization (e.g., Zetasizer settings, TEM operating conditions) (Input protocol, Protocols 1-5).

Critical control variables: The synthesis of MSNs is highly sensitive to the pH, temperature, and stirring conditions. Maintaining a stable pH (e.g., by using a buffer solution), precise temperature control, and homogeneous mixing are crucial for obtaining uniform particle size and morphology (Protocols 1, 3, 5).

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