SiOx barrier for pharmaceutical package and coating process
Inventors
Weikart, Christopher • Felts, John T. • Fisk, Thomas E. • Abrams, Robert S. • Ferguson, John • Freedman, Jonathan R. • Pangborn, Robert J. • Sagona, Peter J.
Assignees
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Publication Number
US-12257371-B2
Publication Date
2025-03-25
Expiration Date
Abstract
A vessel including a thermoplastic wall enclosing a lumen is disclosed. The wall supports an SiOx composite barrier coating or layer, for which x is from 1.8 to 2.4, between the wall and the lumen. High Resolution X-ray Photoelectron Spectroscopy (XPS) shows the presence of an interface between the composite barrier coating or layer and the wall or substrate. In one aspect, the interface has at least 1 mol. % O3—Si—C covalent bonding, as a proportion of the O3—Si—C covalent bonding plus SiO4 bonding. In another aspect, the interface has an Si 2p chemical shift to lower binding energy (eV), compared to the binding energy of SiO4 bonding. The result is a tightly adherent composite barrier coating or layer having a high degree of adhesion to the substrate under practical use conditions. Methods of applying the composite barrier coating or layer are also disclosed.
Core Innovation
The invention relates to a vessel comprising a thermoplastic wall enclosing a lumen and an SiO_x composite barrier coating or layer supported by the wall between the wall and the lumen. A pH protective coating or layer of SiO_xC_y or SiN_xC_y is arranged between the lumen and the composite barrier coating or layer, with an interior surface facing the lumen and an outer surface facing the interior surface of the composite barrier coating or layer. The composite barrier has x from 1.8 to 2.4, and the pH protective layer has x from about 0.5 to about 2.4 and y from about 0.6 to about 3.
The pH protective layer is characterized by an FTIR absorbance spectrum ratio greater than 0.75 and at most 1 between the maximum amplitude of a Si–O–Si symmetrical stretch peak between about 1000 and 1040 cm−1 and the maximum amplitude of a Si–O–Si asymmetric stretch peak between about 1060 and about 1100 cm−1. The layered structure is effective to increase the calculated shelf life of the vessel using the total Si/Si dissolution rate. The stated performance goal is reduced silicon dissolution as measured by the calculated total Si/Si dissolution rate.
The disclosed approach is implemented as a composite coating system combining an SiO_x barrier layer and a separate SiO_xC_y or SiN_xC_y pH protective layer. The content describes performance targets emphasizing very low total silicon dissolution into pH 8 test compositions and extended calculated shelf life based on reduced total Si/Si dissolution rates.
The disclosed system is used in vessels for applications including coated pharmaceutical vessels, with emphasis on prefilled syringes and vials. The content describes additional biological-related observations, including reduced blood clotting, platelet activation, coagulation, and insulin precipitation, in the context of the layered coating system intended to protect against pH-related degradation and silicon dissolution.
Claims Coverage
The independent claim defines a thermoplastic-walled vessel with a two-layer coating system: an SiO_x composite barrier and a SiO_xC_y or SiN_xC_y pH protective layer with a specific FTIR-derived spectral ratio constraint. The claim also requires effectiveness to increase calculated shelf life based on total Si/Si dissolution rate.
Thermoplastic vessel with SiOx composite barrier layer supported on the wall
A vessel comprising a thermoplastic wall enclosing a lumen, with an SiO_x composite barrier coating or layer supported by the wall between the wall and the lumen, where x is from 1.8 to 2.4.
Separate SiOxCy or SiNxCy pH protective coating positioned between lumen and composite barrier
A pH protective coating or layer of SiO_xC_y or SiN_xC_y having an interior surface facing the lumen and an outer surface facing the interior surface of the composite barrier coating or layer, where x is from about 0.5 to about 2.4 and y is from about 0.6 to about 3.
FTIR spectral ratio constraint for pH protective layer Si–O–Si peaks
An FTIR absorbance spectrum of the pH protective coating or layer having a ratio greater than 0.75 and at most 1 between the maximum amplitude of a Si–O–Si symmetrical stretch peak between about 1000 and 1040 cm−1 and the maximum amplitude of a Si–O–Si asymmetric stretch peak between about 1060 and about 1100 cm−1.
Increase calculated shelf life via reduced total Si/Si dissolution rate
The pH protective coating or layer is effective to increase the calculated shelf life of the vessel based on the total Si/Si dissolution rate.
The main inventive coverage is the combination of an SiO_x composite barrier with a separate SiO_xC_y or SiN_xC_y pH protective layer that satisfies an FTIR-derived Si–O–Si peak amplitude ratio constraint and is effective to increase calculated shelf life by reducing total Si/Si dissolution rate.
Stated Advantages
Increased calculated shelf life of the vessel via effectiveness to increase shelf life based on the total Si/Si dissolution rate.
Reduced total silicon dissolution into pH 8 test compositions.
Improved lubricity/coating performance and reduced dissolution/extractables behavior.
Reduced blood clotting, platelet activation, coagulation, and reduced insulin precipitation.
Documented Applications
Pharmaceutical vessels coated with the layered barrier system, with emphasis on prefilled syringes and vials.
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