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Design, Optimization and Characterization of γ-Methacryloxypropyltrimethoxysilane-doped Halloysite Clay Nanotubes Using Ultra-turrax Homogenizer

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Abstract

Objectives

Doping of halloysite nanotubes (HNTs) with γ-methacryloxypropyltrimethoxysilane (γ-MPS) as a silane coupling agent has sparked the interest of researchers. The objective of the study was to design, characterize and critically optimize γ-MPS–doped HNTs by homogenization technique to achieve uniform dispersion and homogenous mixture of clay minerals.

Methods

Optimization of doped HNTs was performed by applying custom design using JMP software 16.1, by considering 2 levels and 3 factors, to determine the impact of independent variables such as concentration of γ-MPS (X1), HNTs (X2) and ethanol (X3) on the response variables diffraction angle (Y1) and zeta potential (Y2).

Results

The results showed that γ-MPS was successfully doped on the surface of HNTs. Existence of characteristic peaks in Fourier-transform infrared analysis affirms the doping of pristine HNTs. From the x-ray diffraction patterns, it was observed that upon doping there was slight shift in the interlayer distance signifying the intercalation of γ-MPS onto the layers of HNTs. Scanning electron microscopic analysis revealed that the doped HNTs showed reduced aggregation as compared to pristine HNT. DHNT F3 and DHNT F7 exhibited higher zeta potential values indicating the excellent stability and dispersibility of the formulation. The predicted R2 values for diffraction angle (2θ) (0.94) and zeta potential (mv) (0.95) were close to 1. The optimal values of the independent variables were obtained to measure the desirability of independent variables (X1, X2 and X3) at the concentration of 9 ml, 37.5 g and 87.5 ml, respectively. The overall desirability D = 0.998, indicates the efficiency of custom design for the studied responses.

Conclusion

The present study concluded that HNTs were successfully doped with γ-MPS using ultra-turrax homogenizer and the results of statistical analysis indicate that the application of custom design proves to be an ideal tool for optimizing the doping of HNTs.

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Abbreviations

PHNTs:

Pristine Halloysite nanotubes

γ-MPS:

γ-methacryloxypropyltrimethoxysilane

DHNTs F1:

Doped HNT Formulation 1

DHNTs F2:

Doped HNT Formulation 2

DHNTs F3:

Doped HNT Formulation 3

DHNTs F4:

Doped HNT Formulation 4

DHNTs F5:

Doped HNT Formulation 5

DHNTs F6:

Doped HNT Formulation 6

DHNTs F7:

Doped HNT Formulation 7

DHNTs F8:

Doped HNT Formulation 8

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Acknowledgements

The authors are thankful to KLE College of Pharmacy, Belgaum for providing the facility to carry out zeta potential analysis. We also express special thanks to National Institute of Technology, Surathkal, Karnataka for XRD and SEM analysis, Jiwaji University, Gwalior for TGA, DSC and TEM analysis, Furthermore, we are also thankful to JMP support team to carry out optimization studies by using JMP software.

Funding

The research work was supported by funding agency AICTE - RPS Scheme, Government of India. Scheme sanctioned with file no: 8-89/FDC/RPS (POLICY-1) /2019-2020.

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Authors and Affiliations

  1. Department of Pharmaceutics, KLE College of Pharmacy, Vidyanagar, Hubballi, 580031 Karnataka, India

    Revati Dharampal Sagare & Fatima Sanjeri Dasankoppa

  2. Department of Pharmacognosy, KLE College of Pharmacy, Vidyanagar, Hubballi, 580031 Karnataka, India

    Hasanpasha N. Sholapur

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Contributions

All the authors have equal contribution and participation in this research work. RS and FD have structured the study design and carried out the optimization, experimentation, collection and interpretation of data. RS and FD contributed in drafting and revision of the manuscript. HS has contributed in interpretation of statistical data analysis. RS, FD and HS have read and approved the manuscript.

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Correspondence to Fatima Sanjeri Dasankoppa.

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Sagare, R.D., Dasankoppa, F.S. & Sholapur, H.N. Design, Optimization and Characterization of γ-Methacryloxypropyltrimethoxysilane-doped Halloysite Clay Nanotubes Using Ultra-turrax Homogenizer. J Pharm Innov 18, 719–734 (2023). https://doi.org/10.1007/s12247-022-09680-8

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