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    • 专利摘要:
    NANOBOARD PRODUCTION PROCESSES CONCENTRATED SILVER AND COMPOSITION. These are modalities of the presentinvention that relate to methods for preparing density solutionsnanoparticle high optics such as nanoplates, silver nanoplates orsilver platelet nanoparticles, and prepared solutions and substratesby the methods. The process may include the addition ofstabilization (e.g., biological or chemical agents trapped orotherwise bound to the nanoparticle surface) that stabilize thenanoparticle before, during and/or after concentration, allowingthereby producing a solution of high optical density andstability of silver nanoplates. The process may also include increasing the concentration of silver nanoplates in the solution, increasing throughhence the optical density of the solution.
    公开号:BR112015008063A2
    申请号:R112015008063-4
    申请日:2013-10-08
    公开日:2021-08-24
    发明作者:Steven J. Oldenburg；Martin G. Miranda；David S. Sebba；Todd J. Harris
    申请人:Nanocomposix, Inc.；Sienna Biopharmaceuticals, Inc.；
    IPC主号:
    专利说明:

    [0001] [0001] This application claims the priority benefit of Interim Application in U.S. 61/795,149, filed October 11, 2012, which is incorporated by reference in its entirety. PARTIES TO THE JOINT RESEARCH AGREEMENT
    [0002] [0002] The invention described in this document was created subject to a Joint Research Agreement between Sienna Labs, Inc. and nano-Composix, Inc. BACKGROUND FIELD OF THE INVENTION
    [0003] [0003] The invention relates to a method for preparing high optical density solutions of silver platelet nanoparticles (e.g. nanoplates) and for nanoparticles, solutions and substrates prepared by said methods. DESCRIPTION OF RELATED TECHNIQUE
    [0004] [0004] Nanoparticles, including nanospheres, nanorods, nanowires, nanocubes, nanoplates, as well as other shapes can be synthesized from a range of materials. In one embodiment, a platelet nanoparticle is a nanoplate. Nanoparticles produced from metals including gold and silver have unique optical properties that can be tuned to interact with light across the electromagnetic spectrum due to the localized surface plasmon resonance sustained by such nanomaterials. Technologies that take advantage of the unique optical properties of silver nanoparticles include, but are not limited to, diagnostic, photonic, medical, and obscurant technologies. A subset of such technologies that include photothermal tumor ablation, hair removal, acne treatment, wound healing and antimicrobial applications among others, can use nanoparticle solutions with high optical densities. Silver nanoplates, which are also known as silver platelet nanoparticles or nanoprisms, are of specific interest for technologies that utilize nanoparticle optical properties due to their adjustable spectral peaks and extremely high optical efficiencies. Although the methods to manufacture silver nanoplates through photoconversion (Jin et al. 2001; Jin et al. 2003), pH controlled photoconversion (Xue 2007), thermal growth (Hao et al. 2004; Hao 2002; He 2008 ; Metraux 2005), molded growth (Hao et al. 2004; Hao 2002) and seed-mediated growth (Aherne 2008; Chen; Carroll 2003; Chen; Carroll 2002, 2004; Chen et al. 2002; He 2008 ; Le Guevel 2009; Xiong et al. 2007) have been developed, such methods generate relatively dilute solutions with a correspondingly low visible and approximately infrared optical density. SUMMARY
    [0005] [0005] For various silver nanoplate applications, a more concentrated solution of silver nanoplates is useful and can be particularly advantageous. In some cases, when so-fabricated solutions of silver nanoplates are concentrated to yield a higher particle density using previously developed methods, the nanoparticle shape may undergo a change that results in a shift in optical properties, such as optical density. In many cases, such changes result in an undesirable degradation of the nanoparticle's optical properties. Accordingly, various embodiments of the present invention provide methods for preparing solutions of silver nanoplates at higher concentrations with increased optical density while reducing degradation of the optical properties of the nanoplates.
    [0006] [0006] The various embodiments of the invention provide methods for preparing high optical density solutions of silver nanoplates, as well as the nanoparticles and solutions prepared by such methods. In one embodiment, the process comprises replacing one or more parent components (e.g., biological or chemical agents) attached to or otherwise coupled to the nanoparticle surface with a stabilizing agent. In another embodiment, the stabilizing agent does not replace the original component, but rather supplements or alters the original component. The stabilizing agent can be a biological or chemical agent that stabilizes the nanoplates before, during and/or after concentration, thus allowing the production of a stable and high optical density solution of silver nanoplates. . In one embodiment, the process also comprises a method for increasing the concentration of silver nanoplates within the solution and, therefore, increasing the optical density of the solution. In several embodiments, the stability (eg, characteristics of the nanoparticles in the solution, such as shape, size, optical properties, peak response, plasmonic properties, etc.) of the high optical density solution is not affected or is substantially unaffected during the process. Various embodiments of the invention comprise a high optical density solution of silver nanoplates that have been stabilized with stabilizing agents (e.g. surface bound molecules, chemical agents and/or biological agents). In one embodiment, the invention comprises a solution of silver nanoplates that have been subjected to surface functionalization with biological or chemical agents that are physisorbed at the surface, molecularly bound to the surface through specific interactions, or encapsulate each nanoparticle.
    [0007] [0007] In one embodiment, a high optical density solution of silver nanoplates is associated with a substrate. In one embodiment, a portion of the nanoplates in solution binds to the substrate to create a nanoplate/substrate composite. The high optical density solutions of silver nanoplates can be exposed to substrates to generate nanoplate composites in which a substantial portion of a substrate's surface area is coated with nanoplates. In some embodiments the substrate comprises fibers, cloth, mesh, bandages, socks, wraps, other articles of clothing, sponges, high porosity substrates, particles with edge lengths greater than 1 micron, microspheres, hair, skin , paper, absorbent polymers, foam, wood, cork, sheets, rough surfaces, biocompatible substrates, filters and/or medical implants.
    [0008] [0008] In various embodiments, a process for increasing the optical density of a stable silver nanoplate solution comprises (i) providing a solution comprising a plurality of silver nanoplates that have a plate shape and that have a density peak optics between 0.1 to 10 cm -1 ; (ii) adding a stabilizing agent to the solution; (iii) adding a buffer to the solution; and (iv) concentrating the buffer-containing solution to form a concentrated solution, wherein the concentrated solution comprises a plurality of silver nanoplates that are plate-shaped and wherein the concentrated solution has a greater peak optical density than than cm-1.
    [0009] [0009] In various embodiments, a method for producing a stable and high optical density solution of silver nanoplates comprises the following: (i) adding a stabilizing agent to a solution of silver nanoplates, (ii) adding a buffer ( for example, such as a buffer containing a water-soluble salt) to the silver nanoplate solution, (iii) mixing the stabilizing agent with the buffer and silver nanoplates over a period of time sufficient for the agent to stabilizing agent interacts with the water-soluble salt in the buffer on the surface of the silver nanoplates and (iv) concentrates the solution to a peak optical density greater than cm-1 (eg, 50 to 1500 cm-1).
    [0010] [0010] Stabilizing agents may include one or more of sodium citrate, a water-soluble polymer, (such as a polystyrene sodium sulfonate and/or a sulfonate-derived hydrocarbon polymer), a polyvinyl based polymer (such as polyvinyl alcohol (PVA) and/or polyvinyl pyrrolidone (PVP)), polyethylene glycol, polyacrylic acid or dextran. The water-soluble salt may include one or more of the sulfates, carbonates, chromates, borates, phosphates and sulfides, acetates and nitrates. In various embodiments, the combination of the stabilizing agent and a buffer that contains one or more water-soluble salts provides stabilization to the nanoplate formulation, wherein one of the components of the salt can interact with the stabilizing agent to cross-link the nanoplate. stabilization agent and increase the stability of a coating on the silver nanoplate. In one embodiment, an initial solution of silver nanoplates can be produced from a solution comprising one or more stabilizing agents and a source of silver (e.g., such as a silver salt, silver seeds, etc.). ) and in which chemical agents, biological agents, mixing, electromagnetic radiation, and/or heating are used to reduce the source of silver (e.g., photoconversion, photoconversion,
    [0011] [0011] In various embodiments, a process for concentrating a solution of silver nanoplates includes the steps of providing a solution comprising a plurality of silver nanoplates that have a peak optical density below 10 cm -1 (e.g. , 0.1 to 9.9 cm-1, 1 to 9 cm-1, 3 to 7 cm-1, 1 to 5 cm-1 and/or 5 to 10 cm-1), add a stabilizing agent to the solution , add a buffer containing a water-soluble salt to the solution and concentrate the solution to a peak optical density greater than 10 cm-1 (e.g. 80 to 150 cm-1, 900 to 1100 cm-1, 100 cm-1, 1000 cm-1 or more). In various embodiments, peak optical density is increased by 10%, 50%, 100%, 200%, 500%, 1000%, 10,000% or more and/or increased in a ratio of 1:1.5, 1: 2, 1:5, 1:10 or more and/or increased by a factor of 1, 1.5, 2, 5, 10, 25, 50, 100, 1000 or more.
    [0012] [0012] In various embodiments, silver nanoplates have an aspect ratio between 1.5 and 50 (eg, 1.5 to 10, 25 to 50). In one embodiment, the silver nanoplates comprise an edge length between 10 nm and 300 nm (eg, 50 to 250, 65 to 100 nm). In various embodiments, the stabilizing agent comprises sodium citrate or at least one water-soluble polymer selected from the group consisting of sodium polystyrene sulfonate and a sulfonate-derived hydrocarbon polymer. In some embodiments, the water-soluble salt comprises one or more of sulfates, carbonates, chromates, borates, phosphates, and sulfides, acetates, and nitrates. In one embodiment, the stabilizing agent comprises at least one of the group consisting of polyvinyl pyrrolidone, polyvinyl alcohol, polyethylene glycol, polyacrylic acid, and dextran. In one embodiment, the stabilizing agent comprises a thiol-containing molecule. The thiol-containing molecule can
    [0013] [0013] In various embodiments, a process for generating metal oxide coated silver nanoplates is provided. The method may include the steps of providing a silver nanoplate solution that has a peak absorption spectrum between 500 and 1500 nm (e.g. 600 to 1400, 800 to 1200 nm) and an optical density greater than 10 cm-1 (e.g. 100 cm-1, 1000 cm-1 or more) and contacting such a solution with a solution of metal oxide or metal oxide precursor in an amount sufficient to form an oxide coating of metal on an outer surface of the silver nanoplates. In certain embodiments, the silver nanoplates are associated with a stabilizing polymer (e.g., polyvinyl pyrrolidone, polyvinyl alcohol, or a combination thereof) prior to contacting the metal oxide precursor, such as through arraying. of the stabilization polymer on an external surface of the silver nanoplates. In various embodiments, the metal oxide is silica or includes silica.
    [0014] [0014] In various embodiments, a process for generating a solution of silver nanoplates includes the steps of providing a solution comprising a reducing agent, a stabilizing agent,
    [0015] [0015] In various embodiments, a composition comprises or essentially consists of a solution of silver nanoplates wherein the silver nanoplates comprise a polyvinyl polymer. In some embodiments, the polyvinyl polymer comprises polyvinyl pyrrolidone or polyvinyl alcohol. In various embodiments, the composition (e.g., solution) comprises one or more salts, such as water-soluble salts (e.g., sulfates, carbonates, chromates, borates, phosphates and sulfides, acetates and nitrates). .
    [0016] [0016] In various embodiments, the polyvinyl polymer is associated with the salt, the polyvinyl polymer coats at least a portion of the silver nanoplates, and/or the polyvinyl polymer is disposed on an external surface of the silver nanoplates. In one embodiment, the solution comprises silver nanoplates in a concentration effective to adhere to a non-metal coating material present in the solution. The solution can be formulated to be concentrated. In some embodiments, the optical density of the silver solution or nanoplates is greater than 10 cm-1 (eg, 100 cm-1, 1000 cm-1 or more). The solution may contain a salt (sulfates, carbonates, chromates, borates, phosphates and sulfides, acetates and nitrates) at a concentration greater than 0.1 mM (eg, 0.1 mM to 10 mM). In one embodiment, the solution has a pH greater than 7 (e.g., 8 to
    [0017] [0017] In various embodiments, a composition comprises or essentially consists of a solution of silver nanoplates bonded to a shell material comprising a polyvinyl polymer. In one embodiment, the silver nanoplates are substantially coated with the polyvinyl polymer. In various embodiments, the composition includes a metal oxide, the metal oxide comprises silica, the polyvinyl polymer comprises polyvinyl alcohol or polyvinyl pyrrolidone, the silver nanoplates are bonded to polyvinyl alcohol and silica and/or silver nanoplates are bonded to polyvinyl pyrrolidone and silica or any combination thereof. In one embodiment, the composition includes a chemical moiety selected from an amine chemical moiety and a mercapto chemical moiety. In one embodiment, the chemical moiety is bonded to the silica. In one embodiment, the composition includes aluminum. In one embodiment, the optical density of the solution is greater than 10 cm-1 (e.g., 100 to
    [0018] [0018] In various embodiments, a composition includes silver nanoplates at least partially coated by a shell material that includes a polyvinyl polymer, wherein the average thickness of the shell material is between 1 nm and 50 nm (e.g. , 5, 15, 40 nm). In one embodiment, the silver nanoplates have at least an edge length between 10 nm and 500 nm (e.g., 25, 100, 250, 300 nm).
    [0019] [0019] In various embodiments, a kit essentially comprises or consists of one or more containers comprising nanoplates with an optical density greater than 10 cm-1 (e.g., 100 cm-1, 1,000 cm-1 or more), a suitable solution for coating nanoplates with a metal oxide shell and instructions for its use. In one embodiment, the nanoplates comprise a polyvinyl polymer. In one embodiment, the polyvinyl polymer interacts with (e.g., crosslinks or otherwise couples) a water-soluble salt (e.g., sulfates, carbonates, chromates, borates, phosphates and sulfides, acetates and nitrates). .
    [0020] [0020] In various embodiments, a solution includes silver nanoplates at least partially coated with a silica coating, wherein the silver nanoplates comprise a peak optical density of greater than 10 cm-1 (e.g. , 11 to 5000 cm-1, 90 to 1100 cm-1 or more). In one embodiment, the silica coating has a shell thickness between 2 and 100 nm (e.g., 10 to 70, 30 to 90, 40 to 60 nm). In one embodiment, the solution comprises a water-soluble salt (e.g., sulfates, carbonates, chromates, borates, phosphates and sulfides, acetates and nitrates) at a concentration greater than 0.1 mM (e.g., 0.1 mM at 10 mM). in a fashion-
    [0021] [0021] In some embodiments, a process to generate a solution of silver nanoplates with extremely high optical density includes the steps of (i) adding a chemical concentration stabilizing agent to a solution of silver nanoplates or reagents precursors and (ii) increase the concentration of silver nanoplates to increase the optical density of the solution.
    [0022] [0022] In various embodiments, silver nanoplates have an aspect ratio between 1.5 and 25 (eg, 1.5 to 10; 1.5 to 5; 10 to 30; 25 to 50); and/or the nanoplate has an edge length between about 10 nm and 250 nm (e.g., 25 to 180; 50 to 150 nm); and/or the nanoplate is triangular in cross-section; and/or the nanoplate is circular in cross-section. In one embodiment, the perimeter of the nanoplate cross-section has between 4 and 8 edges (eg, 5, 6, 7). In various embodiments, the silver nanoplate solution is formed using one or more of a photoconversion method, a pH-controlled photoconversion method, a thermal growth method, a seed-mediated growth method and/or or a solution comprising a formate stabilizing agent or agents and a source of silver. In various embodiments, biological or chemical agents and/or electromagnetic radiation and/or heating or a combination thereof are used to reduce the source of silver. In one embodiment, the silver nanoplate solution is formed from a combination of a reducing agent, a format stabilizing agent, a light source, a heat source, and a silver source.
    [0023] [0023] In one embodiment, an acid, base or buffer (also called a "buffering agent") is added to alter the pH of the solution. In various embodiments, the chemical concentration stabilizing agent is added before, during and/or after the formation of silver nanoplates. In one embodiment, the chemical concentration stabilizing agent acts as a format stabilizing agent. In one embodiment, the chemical concentration stabilizing agent acts as a reducing agent. In one embodiment, the chemical concentration stabilizing agent acts as an agent to alter the pH of the solution.
    [0024] [0024] In one embodiment, the chemical concentration stabilizing agent is a water-soluble polymer. In various embodiments, the polymer is any one or more of a polysulfonate derivative, sodium polystyrene sulfonate, a vinyl polymer derivative, and a polyvinyl alcohol (PVA). In various embodiments, the PVA has a molecular weight of less than about 80,000 Daltons, between about 80,000 Daltons and 120,000 Daltons, and/or more than about
    [0025] [0025] In one embodiment, the polymer is a polyethylene glycol (PEG). In various embodiments, the PEG has a molecular weight of less than about 5,000 Daltons, between about 5,000 Daltons and 10,000 Daltons, and/or greater than about 10,000 Daltons. In one embodiment, the PEG contains a single functional group. In one embodiment, the PEG contains two functional groups. In some embodiments, the functional group or groups consists of one or more of the following: an amine, thiol, acrylate, alkyne, maleimide, silane, azido, hydroxyl, lipid, disulfide, fluorescent molecule, and/or biotin, or combinations thereof . In one embodiment, the functional group or groups can be any one or more of an amine, thiol, acrylate, alkyne, maleimide, silane, azido, hydroxyl, lipid, disulfide, fluorescent molecule, and/or biotin. In one embodiment, the concentration stabilizing agent is a carbohydrate derivative. In various embodiments, the polymer is a monosaccharide, a disaccharide, an oligosaccharide, a polysaccharide, and/or dextran. In various embodiments, dextran has a molecular weight that is less than about 2000 Daltons (e.g. 500, 1000, 1500 Daltons), between about 2000 Daltons and 5000 Daltons (e.g. 3000, 4000 Daltons) and/ or more than about 5,000 Daltons (eg, 6,000, 8,000, 10,000 Daltons or more).
    [0026] [0026] In various embodiments, the chemical concentration stabilizing agent is any one or more of a phenol, a monomeric phenol, a dimeric phenol, a trimeric phenol, a polyphenol, a tannic acid, is gum arabic, a biological molecule, a protein, a bovine serum albumin, streptavidin, biotin, a peptide, an oligonucleotide, a naturally occurring oligonucleotide, an oligonucleotide
    [0027] [0027] In various embodiments, the solvent can be one or more of water, an alcohol, ethanol, isopropyl alcohol, t-butanol, a mixture of a water and an alcohol.
    [0028] [0028] In one embodiment, the concentration of silver nanoplates is increased with the use of tangential flow filtration. In one embodiment, tangential flow filtration is performed using a tangential flow filter membrane. In one embodiment, the tangential flow membrane is produced from a cellulose ester or mixture of cellulose esters.
    [0029] [0029] In various embodiments, the tangential flow membrane is produced from one or more of a polyethersulfone and/or polysulfone. In various embodiments, the tangential flow membrane has a molecular weight cutoff of less than about 10 kD (e.g., 1, 5, 8 kD), between about 10 kD and 500 kD (e.g., 50, 250, 400 kD), greater than about 500 kD (e.g. 750, 1000,
    [0030] [0030] In various embodiments, the silver nanoplate solution is concentrated to produce a solution with an optical density greater than about 10 cm-1, greater than about 50 cm-1, greater than about 75 cm-1, greater than about 100 cm-1, and/or greater than about 500 cm-1 (e.g., 100 to 1000, 100 to
    [0031] [0031] In one embodiment, the concentrated solution solvent is exchanged using tangential flow filtration. In one embodiment, the concentrated solution is processed to remove residual chemicals using tangential flow filtration.
    [0032] [0032] In various embodiments, a nanoparticle solution comprising silver nanoparticles is coated with a polymer having an optical density greater than 100 cm-1 (e.g., 200, 500, 700, 1,500 cm-1 or more) in in one embodiment, the silver nanoplate solution is incubated with a substrate. In one embodiment, the substrate is removed from the silver nanoplate solution and dried.
    [0033] [0033] One embodiment of the present invention provides processes for producing plasmonic nanoparticle solutions, such as, for example, silver nanoplates, which are suitable for thermomodulating a target tissue region. Thermomodulation of a target tissue can be achieved when a composition comprising a plurality of plasmonic nanoparticles is administered to an individual under conditions such that an effective amount of the plasmonic nanoparticles localizes a domain of the target tissue region and exposes the target tissue region to energy delivered from an excitation surface plasmon resonance source in an amount effective to induce thermomodulation of the target tissue region domain. In various embodiments, the materials described herein are useful for performing targeted ablative or non-ablative tissue heating. For example, in one embodiment, a method is provided for performing targeted ablative or non-ablative tissue heating to treat a mammalian subject in need thereof, comprising the steps of (i) topically administering the an individual's skin surface, the composition of plasmonic nanoparticles that includes silver nanoplates; (ii) providing penetration means to redistribute plasmon particles from the skin surface to a dermal tissue component; and (iii) causing the skin surface to be irradiated by light.
    [0034] [0034] In various embodiments, the invention comprises compositions which, when used with suitable methods of delivery and excitation with a light-based energy source, can achieve non-invasive or minimally invasive treatment of the skin and underlying tissues. or other tissue spaces accessible using nanoparticles. The use of optical density solutions of plasmonic nanoparticles, such as, for example, silver nanoplates, with short-pulse-width laser excitation (e.g., pulse widths from 0.1 ms to 1 s) can create Steep transient heating gradients that selectively target ablative or non-ablative heating for structures within various cell layers where the particles are located, for example. The pilosebaceous unit for acne treatment and pore size reduction, the targeted epidermal and dermal layers for skin resurfacing and small profile scar remodeling and hair follicle for permanent hair removal. Treatment may include, but are not limited to, hair removal, hair growth and regrowth, and skin rejuvenation and regrowth, acne removal or reduction, wrinkle reduction, pore reduction, cellulite ablation and other skin deposition. dermal lipid, wart and fungus removal, thinning or removal of scars that include hypertrophic scars, atrophic scars and keloids, abnormal pigmentation (such as port-wine stains), tattoo removal, and/or skin inconsistencies ( e.g. texture, color, tone, elasticity, hydration). Other therapeutic and preventive methods include, but are not limited to, a treatment of hyperhidrosis, anhidrosis, Frey Syndrome (gustatory perspiration), Horner Syndrome and Ross Syndrome, actinic keratosis, follicular keratosis, dermatitis,
    [0035] [0035] The objectives, features and additional advantages of the invention(s) will become evident from the following detailed description considered in conjunction with the accompanying Figures which show illustrative embodiments of the invention, in which the The following is a description of the drawings. Drawings are examples and should not be used to limit modalities. Furthermore, the mention of modalities that have mentioned resources is not intended to exclude other modalities that have additional resources or other modalities that incorporate different combinations of the mentioned resources. Furthermore, features in one modality (such as in a Figure) can be combined with descriptions (and Figures) of other modalities.
    [0036] [0036] Figure 1 illustrates the optical spectrum of a silver nanoplate solution fabricated using a photoconversion method in accordance with an embodiment of the present invention. As manufactured, such silver nanoplates, in one embodiment, have a peak optical density of less than 1 cm-1 (eg, approximately 0.8 cm-1)
    [0037] [0037] Figure 2 illustrates the optical spectrum of a silver nanoplate solution fabricated using a seeded growth method in accordance with an embodiment of the present invention. As manufactured, such silver nanoplates have a peak optical density of less than 3 cm-1.
    [0038] [0038] Figure 3A is a transmission electron microscope image of a silver nanoplate solution fabricated using a photoconversion method in accordance with an embodiment of the present invention.
    [0039] [0039] Figure 3B is a transmission electron microscope image of a silver nanoplate solution fabricated using a seeded growth method in accordance with an embodiment of the present invention.
    [0040] [0040] Figure 4 the optical spectra of silver nanoplates without the addition of a stabilizing agent and water-soluble salt according to an embodiment of the invention before tangential flow concentration and after tangential flow concentration.
    [0041] [0041] Figure 5 is the normalized optical spectra of silver nanoplates without the addition of a stabilizing agent and water-soluble salt according to an embodiment of the invention before tangential flow concentration and after concentration.
    [0042] [0042] Figure 6 are the optical spectra according to an embodiment of silver nanoplates combined with polyvinyl alcohol and a water-soluble salt before concentration and after concentration.
    [0043] [0043] Figure 7 are the optical spectra normalized according to a modality of silver nanoplates combined with polyvinyl alcohol and a water-soluble salt before concentration and after concentration.
    [0044] [0044] Figure 8 illustrates an optical quenching spectrum of high optical density nanoplate solutions processed using the methods described in various embodiments of the invention.
    [0045] [0045] Figure 9 illustrates the steps to produce a modality of silver nanoplates by manufacturing the silver nanoplates, adding stabilizing agents, concentrating the nanoplates and optionally coating the nanoplates with silica. DETAILED DESCRIPTION OF THE PREFERRED MODALITY
    [0046] [0046] Several embodiments of the present invention comprise processes for producing plasmonic nanoparticle solutions that include silver nanoplates that are suitable for performing thermomodulation of a target tissue region. In one embodiment, thermomodulation of a target tissue may be achieved when a composition comprising a plurality of plasmonic nanoparticles is administered to a subject under conditions such that an effective amount of the plasmonic nanoparticles localizes to a domain of the target tissue region. . The target tissue region is exposed to energy delivered from the excitation surface plasmon resonance source. Energy is delivered in an effective amount to induce thermomodulation of the target tissue region domain.
    [0047] [0047] Optical density (OD), which is used in this document as a synonym for absorbance, is defined to be the logarithmic ratio of the radiation incident on a material to the radiation transmitted through the material (OD = -log10 (I1/I0) where I1 is the transmitted light intensity and I0 is the incident light intensity). For solutions, the optical density is a function of the path length through the liquid sample and is expressed in units of cm-1. In some cases, optical density is expressed without the cm-1 unit – such as in cases where a standard path length of 1 cm is used. In some traditional methods for making silver nanoplates, the maximum optical density of silver nanoplates in solutions thus synthesized without any further processing is typically less than 10 cm-1 (e.g., 0.1 to 9, 9 cm-1, 1 to 9 cm-1, 3 to 7 cm-1, 1 to 5 cm-1, and/or 5 to 10 cm-1). However, in accordance with some embodiments of the present invention, silver nanoplates can be produced with increased optical densities. In general, the optical densities of solutions containing plasmon particles that include silver nanoplates are most effective with an optical density that is greater than 10 cm-1 (e.g., 11 to
    [0048] [0048] In some embodiments, nanoparticle formulations are formulated for application via a sponge applicator, cloth applicator, direct contact through a hand or gloved hand, spray, aerosol, vacuum suction, high pressure or high pressure liquid flow, roller, brush, flat surface, semi-flat surface, wax, ultrasound and other sonic forces, mechanical vibrations, hair manipulation (including pulling, massaging), physical force, thermal manipulation and/or other treatments. In some embodiments, nanoparticle formulation treatments are performed alone, in combination, sequentially, or repeated from 1 to 24 times or more. In other embodiments, plasmonic nanoparticles can selectively localize to a first component of the skin, where physical massage or pressure, ultrasound or heating increases the selective localization of the nanoparticles to the first component. Additionally, the nanoparticles are selectively removable from skin components other than the first one.
    [0049] [0049] In various embodiments, the materials described in this document are useful for performing targeted ablative or non-ablative tissue heating. For example, in one embodiment, a method is provided for performing targeted ablative or non-ablative heating of a tissue to treat a mammalian subject in need thereof, comprising the steps of (i) administering topically to a skin surface from the individual, the composition of plasmonic nanoparticles that includes silver nanoplates; (ii) provide a means of penetration to redistribute plasmonic particles from the skin surface to a dermal tissue component; and (iii) causing the skin surface to be irradiated by light. In other or additional embodiments, a method is provided wherein the light source comprises excitation of mercury, xenon, deuterium or a metal halide, phosphorescence, incandescence, luminescence, light emitting diode, in sunlight. In yet other or additional modalities, a method is provided wherein the concentration medium comprises high frequency ultrasound, low frequency ultrasound, massage, iontophoresis, high pressure air flow, high pressure liquid flow , vacuum, pretreatment with fractional photothermolysis or dermabrasion or a combination thereof. In still further embodiments, a method is provided wherein the irradiation comprises light having a wavelength of light between about 200 nm and about 10,000 nm (e.g., 300 to 9,000, 700 to 1,300, 800 to 1200, 800 to 1300, 900 to 1100, 550 to 1100, 810 to 830, 1000 to 1100 nm), a fluence of about 1 to about 100 joules/cm2 (e.g. 5 to 20, 40 to 70 , 10 to 90), a pulse width of about 1 femptosecond to about 1 second, and a repetition frequency of about 1 Hz to about 1 THz (e.g., 1 to 10, 10 to 100 , 100 to 1000, 1000 to 10,000, 10,000-100,000 Hz or more).
    [0050] [0050] An objective of an embodiment of the art described herein is to provide compositions which, when used with the appropriate methods of administration and excitation with a light-based energy source, can achieve non-invasive or minimally invasive treatment of skin and underlying tissues, or other tissue spaces accessible with the use of nanoparticles. The use of
    [0051] [0051] In one embodiment, nanoplates, such as silver nanoplates, are characterized by lengths along the three main geometric axes in which: the axial length of two of the main geometric axes is at least twice as long as the that the axial length of the shortest major axis and the shortest major axial length is less than about 500 nm (e.g. 450, 400, 350, 300, 250, 100, 150, 50, 30, 20, 10 nm). The "edge length" of the nanoplate is defined as the average of the length of the two longest principal geometric axes. The "thickness" of the nanoplate is defined with the shortest principal geometric axis.
    [0052] [0052] The ratio of edge length to thickness is called "aspect ratio". In various embodiments, the average aspect ratio of silver nanoplates is greater than 1.5; two; 3; 4; 5; 7; 10; 20; 30 or 50 and any track in it. In one embodiment, the average aspect ratio of the silver nanoplates is between 1.5 and 25; 2 and 25; 1.5 and 50; 2 and 50; 3 and 25 and/or 3 and 50.
    [0053] [0053] In various embodiments, a nanoplate has edge lengths less than 500 nm, 250 nm, 200 nm, 150 nm, 100 nm, 80 nm, 60 nm or 50 nm. In one embodiment, the nanoplate has edge lengths greater than 5 nm, 10 nm, 20 nm, 30 nm, 50 nm, or 100 nm. In various embodiments, the edge length is 30 nm to 100 nm, 20 nm to 150 nm, 10 nm to 200 nm, 10 nm to 300 nm. In various embodiments, the nanoplate has a thickness that is less than 500 nm, 300 nm, 200 nm, 100 nm, 80 nm, 60 nm, 50 nm, 40 nm, 30 nm, 20 nm and/or 10 nm and any range among them. In various embodiments, the nanoplate thickness is 5 nm to 20 nm, 5 nm to 30 nm, 10 nm to 30 nm, 10 nm to 50 nm, 10 nm to 100 nm.
    [0054] [0054] Various embodiments of silver nanoplates have a variety of different cross-sectional shapes, including, (but not limited to) circular, triangular, or shapes that have any number of distinct edges. In non-limiting modalities, nanoplates can be shaped as circular, oval, square, rectangular, rods, stars, tubes, pyramids, prisms, triangles, branches.
    [0055] [0055] Silver nanoplates have distinct advantages over other plasmonic nanoparticle formats and compositions. For example, silver nanoplates have advantages over plasmonic nanoparticle shapes and compositions that include gold nanoshells and gold nanorods because of the potential for lower production costs (less reaction residue and lower costs). material). Furthermore, the optical density (OD) per weight of metal is higher for silver nanoplates compared to gold nanorods when randomly oriented in solution and irradiated with unpolarized light, due to the fact that the flat surface of a nanoplate resonates with both incident light polarizations. Additionally, the absorbance of silver nanoplates is superior to that of gold nanowraps for the same metal weight due to the fact that a higher fraction of light is absorbed rather than scattered with a nanoplate architecture compared to a nanowrap. For many applications, such cost and absorbance benefits can only be realized if the nanoplates are stabilized at a high concentration and for long periods of time, which is the subject of an embodiment of the present invention. MANUFACTURE OF SILVER NANO PLATE
    [0056] [0056] Modern nanoparticle synthesis techniques enable the development of materials with unique optical properties for a wide range of applications that include diagnostic, obscurant and therapeutic applications. Silver nanoplates, as manufactured using current traditional methods that include photoconversion, pH controlled photoconversion, thermal growth and/or seed-mediated growth method, typically have optical densities in the range of 0.1 to 10 cm -1 (for example, for example 0.1 to 9.9 cm-1, 1 to 9 cm-1, 3 to 7 cm-1, 1 to 5 cm-1 and/or 5 to cm-1). Several technologies seek superior optical density solutions from silver nanoplates. Various embodiments of the present invention describe an innovative and non-obvious method for concentrating silver nanoplates and generating higher optical density silver nanoplate solutions. For example, in various embodiments, the methods can increase the optical density of silver nanoplate solutions to more than 10 cm-1, 20 cm-1, 30 cm-1, 50 cm-1, 80 cm-1 , 100 cm-1, 150 cm-1, 200 cm-1, 300 cm-1, 400 cm-1, 500 cm-1, 600 cm-1, 700 cm-1, 800 cm-1, 900 cm-1 and/or 1000 cm-1 or more.
    [0057] [0057] Silver nanoplates can be fabricated using photoconversion (Jin et al. 2001; Jin et al. 2003), pH controlled photoconversion (Xue 2007), thermal growth (Hao et al. 2004; Hao 2002; He 2008; Metraux 2005), molded growth (Hao et al. 2004; Hao 2002), seed-mediated growth (Aherne 2008; Chen; Carroll 2003; Chen; Carroll 2002, 2004; Chen et al. 2002; He 2008; Le Guevel 2009; Xiong et al. 2007), all of which are incorporated by way of reference or alternative methods. Alternative methods according to various embodiments of the present invention include methods wherein the silver nanoplates are formed from a solution comprising one or more stabilizing agents and a source of silver and wherein the chemical agents, biological, mixing, electromagnetic radiation, and/or heating are used to reduce the source of silver.
    [0058] [0058] An optical spectrum of silver nanoplates fabricated using one embodiment of a photoconversion method is shown in Figure 1. The peak wavelength of the optical spectra (100) is at a wavelength of 775 nm with an optical density of 0.74 cm-1. Optical spectra of silver nanoplates fabricated using one modality of a seed-mediated growth method are shown in Figure 2. The peak wavelength of the optical spectra (200) is at one wavelength of 930 nm with an optical density of 2.58 cm -1 . A transmission electron microscope image of silver nanoplates produced using a photoconversion method is shown in Figure 3A. A transmission electron microscope image of silver nanoplates produced using a seed-mediated growth method is shown in Figure 3B.
    [0059] [0059] In one embodiment, when the nanoplates thus manufactured are concentrated using tangential flow filtration, the shape of several of the nanoplates can be changed to nanospheres, so as to reduce formulation effectiveness, as evidenced by a high peak height at ~400 nm which is the peak optical resonance of spherical silver nanoparticles. Figure 4 shows the optical density of an embodiment of a solution of the nanoplates in the absence of a concentration stabilizing agent before (400) and after (410) concentration. The optical resonance peak that corresponds to the plasmonic resonance of the nanoplates shifts from 815 nm (420) to 745 nm (430), in order to demonstrate that the average edge length of the nanoplates is reduced.
    [0060] [0060] Figure 5 shows a normalized plot of the nanoplate spectra shown in Figure 4. For such a nanoplate solution, the peak intensity in the range from 700 nm to 850 nm is correlated to the amount of nanoplates in the solution. The peak intensity in the 400 nm range is correlated with the amount of spheroid particles in solution. Before concentration, the ratio of the longest wavelength peak (520) to the shortest wavelength peak (540) is 3. After concentration, the ratio of the longest wavelength peak (530) for the shortest peak wavelength (550) is 0.8. Such a ratio change demonstrates that silver nanoplates change shape and that the amount of nanoplates in the solution is reduced.
    [0061] [0061] In one embodiment, a solution of nanoplates can be stabilized. Figure 6 shows the optical density of one embodiment of a solution of nanoplates that have been stabilized using polyvinyl alcohol in a borate solution (eg, sodium borate, potassium tetraborate, etc.). The peak wavelength of the nanoplate peak is equal for both unconcentrated (620) and concentrated (630) solution, so as to indicate that the edge length of the nanoplates is equal before concentration (600) and after concentration. (610). Figure 7 shows the normalized spectrum which demonstrates that the peak spectrum shape does not change before concentration (700) nor after concentration (710) indicating, therefore, that in one embodiment, a surface coating is sufficient. to prevent the shape of the nanoparticles from being altered. In various embodiments, more than 10%, more than 20%, more than 30% or more than 50% of the silver nanoplates are shaped without a surface protection. In other embodiments, less than 20%, less than 10%, or less than 5% of the silver nanoplates undergo a shape change if the nanoplates are coated with a protective surface coating. In one embodiment, a spectrum of a nanoplate solution concentrated to have a peak optical density of ~900 cm-1 is shown in Figure 8.
    [0062] [0062] In one embodiment, the silver nanoplates are formed in a multi-step process. In one embodiment, the steps for concentrating the nanoplates are shown in Figure 9 and
    [0063] [0063] In various embodiments, the stabilizing agent can be a salt, a polymer, or a biomolecule. In one embodiment, the stabilizing agent is sodium tricitrate or another citrate derivative.
    [0064] [0064] In one embodiment, the water-soluble polymer is a polyanionic polymer that includes, but is not limited to, sulfonate-derived polymers, polystyrene sulfonate derivatives, such as an inorganic salt of polystyrene sulfonate or a salt monovalent polystyrene sulfonate. In one embodiment, the water-soluble polymer is poly(sodium styrene sulfonate) (PSSS). In one embodiment, PSSS has a molecular weight between about 3 kDa and about
    [0065] [0065] In various embodiments, the silver salt can be any water-soluble silver salt that includes, but is not limited to, silver acetate, silver perchlorate, silver nitrate, silver trifluoroacetate, or silver triflate.
    [0066] [0066] In one embodiment, a step for formulating silver nanoplates includes growing the seeds on silver nanoplates in an aqueous solution comprising silver seeds, an acid reducing agent and a salt of silver. In one embodiment, the acid reducing agent is citric acid or ascorbic acid. The silver salt for the step where the seeds are grown to form silver nanoplates can be any water-soluble silver salt that includes silver acetate, silver perchlorate, silver nitrate, silver trifluoroacetate, silver triflate or combinations thereof.
    [0067] [0067] In one embodiment, the silver nanoplates are agitated at a shear flow rate between 1 s-1 and 100,000 s-1 (e.g., at least 10, 50, 100, 200, 300, 400, 500, 1,000, 2,000,
    [0068] [0068] In one embodiment, the silver nanoplates have molecules that are adsorbed or otherwise bound to the particle surface. The molecules on the surface are the reactants or by-products.
    [0069] [0069] In various embodiments, stabilizing agents that may be used include biological or chemical agents that are physisorbed (e.g., absorbed through non-molecular binding forces) at the surface, molecularly bound to the surface. through specific interactions (eg thiol or amine), or encapsulate the surface (eg a metal oxide or metalloid oxide shell). In one embodiment, the chemical agents of specific interest include polymers. In one embodiment, chemical agents of specific interest include polymers such as polysulfonates. In a preferred embodiment, the stabilizing polymer is derivatized with sulfonates. In some embodiments, vinyl polymers, carbohydrates, ethylene oxides, phenols and carbohydrates can be used. Specific examples of such polymers include polystyrene sodium sulfonate, polyvinyl alcohol (PVA), polyvinyl pyrrolidone (PVP), polysaccharides, phenol, tannic acid, dextran, and polyethylene glycol (PEG), including PEG molecules that contain one or more more chemical groups (eg amine, thiol, acrylate, alkyne, maleimide, silane, azido, hydroxyl, lipid, disulfide, fluorescent molecule, or biomolecule chemical moieties). Molecules of specific interest include proteins, peptides, oligonucleotides, biotin, alkane thiols, lipoic and dihydrolipoic acid and derivatives of such acids, bovine serum albumin, streptavidin, neutrovidin, wheat germ agglutinin, oligonucleotide and naturally occurring peptides
    [0070] [0070] In one embodiment of this invention, the silver nanoplates are manufactured in aqueous solutions. In other embodiments, the silver nanoplates are manufactured in other solutions which may include ethanol, isopropanol or organic solvents such as heptane, toluene or butanol.
    [0071] [0071] In one embodiment an acid, base or buffering agent is added to alter the pH of the solution before, during or after the addition of a stabilizer. In one embodiment, a buffer that typically contains a water-soluble salt is added. In one embodiment, the water-soluble salt comprises borate. In one embodiment, the water-soluble salt comprises sodium borate. In one embodiment, the nanoplates are suspended in a sodium bicarbonate buffer or a sodium borate buffer. In one embodiment, the pH of the solution after the addition of the pH modifying agent is greater than pH 6, pH 7, pH 8, pH 9, or pH 10. In several embodiments, the pH of the solution after the addition of the pH modifying agent is from pH 6 to pH 8, pH 6.0 to pH 9, pH 7 to pH 10, pH 7 to pH 11, pH 8 to pH 10, pH 8 to pH 11 or pH 7 to pH 12 .
    [0072] [0072] In one embodiment, the combination of a nanoplate coating and a water-soluble salt present in a buffer provides stabilization to the nanoplate formulation.
    [0073] [0073] In various embodiments, the stabilizing agents can be solid or liquid formulations that are added to the silver nanoplate solution. Stabilizing agents have an affinity for the surface of silver nanoplates and can associate with the plate surface over wide ranges of relative concentrations. In some embodiments, molecules bound to silver nanoplates are displaced by a stabilizing agent. Alternatively, a stabilizing agent, such as a polymer, is covalently attached to a silver atom present on the surface of the nanoplate. The polymer coating can extend over all or a portion of the outer surface of a silver nanoplate. For example, at least 5%, 10%, 15%, 20%, 25%, 50%, 75%, 80%, 90%, 95%, 99%, 99.9% or more than 99, 9% of the outer surface of a silver nanoplate is coated with one type of polymer or a plurality of different types of polymers. In one embodiment, the stabilizing agent is added prior to the formation of the silver nanoplates, while in another embodiment, the stabilizing species is added after the synthesis of the silver nanoplates. In such a way, compositions containing polymer coated silver nanoplates are provided and solutions containing such compositions can have an optical density less than or equal to 10 cm -1 . Alternatively, such solutions have polymer-coated silver nanoplates and an optical density greater than 10 cm-1; such solutions can be achieved through concentration or purification of polymer-coated silver nanoplates present in a more dilute solution. In some embodiments, the stabilizers are added to the silver nanoplate solution thus manufactured. In other embodiments, the solution from the nanoplates is washed away or residual reagents are otherwise removed. In some embodiments, the suspended solution is exchanged one or more times with one or more solutions, for example, to wash the nanoplates or to change the pH of the solution before stabilizing agents are added. Kits are also provided that contain, in one or more containers, nanoplates in a solution that has an optical density greater than 10 cm-1 and a solution that contains metal oxide or that contains an oxide precursor. suitable for coating the nanoplates with a shell (or coating) of the metal oxide. Preferably, the containers are provided with instructions for their use. In some embodiments, the kits contain nanoplates that have a coating that contains a polyvinyl polymer. In other embodiments, the polyvinyl polymer contains borate. Nanoplates having a stabilizing coating are characterized as provided herein or otherwise known in the art, such as by particle analyzers or emission detectors such as NMR, Fourier transform spectroscopy, spectrometry of mass or similar tests.
    [0074] [0074] Once the stabilizing agent is added, the mixture of the stabilizer and the silver nanoplates can be subjected to several different processes, including heating, boiling,
    [0075] [0075] In one embodiment, after the stabilization step is completed, the silver nanoplates can be washed to remove residual reagents or to exchange the solution with another solution. Solution exchange can be achieved using dialysis, centrifugation, filtration, or tangential flow filtration (also known as cross-flow filtration). In various embodiments, the amount of wash volumes changed in the sample is zero, 1, 2, 3, 4, 5, 1 and 5, 5 to 10, 10 to 20 or more than 20 wash volumes, inclusive.
    [0076] [0076] Nanoparticle solutions with optical densities greater than 10 cm-1 (e.g. 11 to 5000 cm-1, 15 to 2000 cm-1, 20 to 1000 cm-1, 80 to 150 cm-1 , 90 to 110 cm-1, 900 to 1,100 cm-1, 100 cm-1,
    [0077] [0077] In various embodiments, the concentration of the silver nanoplate solution is increased to produce a final solution with optical densities greater than about 5 cm-1, greater than about 10 cm-1, greater than about 50 cm-1, greater than about 75 cm-1, greater than about 100 cm-1, greater than about 500 cm-1 and/or greater than about 1000 cm-1. In various embodiments, the concentration of the silver nanoplate solution is increased to produce a final solution with optical densities between 10 cm-1 to 100 cm-1, 30 cm-1 to 300 cm-1, 50 cm-1. 1 to 500 cm-1, 100 cm-1 to 1000 cm-1, 300 cm-1 to 3000 cm-1 or 500 cm-1 to 5000 cm-1. One embodiment of the invention is in which the concentration of the silver nanoplate solution is increased to above 106, 107, 108, 109, 1010, 1011, 1012 or 1013 particles per milliliter. In various embodiments, the concentration of the silver nanoplate solution is increased to be between 106 and 1013, 107 and 1013, 108 and 1013, 109 and 1013, 1010 and 1013, 1011 and 1013, or 1012 and 1013 particles. per milliliter. In several modalities, the plaque concentration is greater than 0.1; 1.0; two; 4; 5; 7; 8; 9 and/or 10 mg/ml. In various embodiments, the plaque concentration is between 0.1 to 1.0; 0.3 to 3.0; 0.5 to 5.0; 1.0 to 10.0; 3.0 to 30.0; 5.0 to
    [0078] [0078] In one embodiment, the concentrated silver nanoplates are encapsulated with a silica shell. The coating can extend over all or a portion of the outer surface of a silver nanoplate. For example, at least 5%, 10%, 15%, 20%, 25%, 50%, 75%, 80%, 90%, 95%, 99%, 99.9% or more than 99.9% of the outer surface of a silver nanoplate is coated with silica. Concentrated plates can be mixed with an alcohol (eg ethanol or isopropanol). In one embodiment, an aminosilane or mercaptosilane is added to the solution to bind silane molecules to the surface of the nanoplates. The binding of silane molecules to the surface of nanoplates is specific to the surface coating on the nanoplates. Some nanoparticle coatings that stabilize the nanoplates during processing will not support the formation of a silica shell. In one embodiment, the surface of the nanoplates is coated with a molecule that has an affinity for silane molecules in solution. In one embodiment, a polyvinyl-based polymer such as polyvinyl alcohol or polyvinyl pyrrolidone is bonded to the surface of the nanoplate prior to the addition of silane molecules. In other embodiments, a polyvinyl-based polymer surface is complexed with a water-soluble salt present in a buffer (e.g., one or more of the sulfates, carbonates, chromates, borates, phosphates and sulfides, acetates and nitrates) prior to addition. of the silane molecules. In other embodiments, mercaptohexadecanoic acid, mercaptoundecanoic acid or other thiol-containing acids are bound to the surface of the nanoplates. Once there are initial silanes attached to the surface of the nanoplate, the additional silane can be added to the solution through the presence of a base to form a silica shell. In one embodiment, nanoplates coated with a silica shell can be transferred to water and concentrated using a concentration method such as tangential flow filtration. In another embodiment, the silica shells are mixed with an aluminum salt solution such as aluminum chloride, a stabilizing polymer such as polyvinyl pyrrolidone or a buffer such as bicarbonate.
    [0079] [0079] It is an object of this invention to manufacture a solution comprising a concentrated solution of silver nanoplates coated with a silica shell. In one embodiment, the peak optical density of the solution as measured in a 1 cm path length cuvette is above 10, 20, 50, 100, 500, or 1000. In various embodiments, the peak optical density of the solution as measured in a 1 cm path length cuvette is between a 100, 20 to 200, 30 to 300, 50 to 500, 100 to 1000, 200 to 1000, 300 to 1000, 500 to 1000 and/or 200 to 2000 and any combinations thereof. In another embodiment, the plaque concentration is above 0.1 mg/ml, 1 mg/ml, or above 10 mg/ml. In several modalities, the plaque concentration is between 0.1 to 1.0; 0.3 to 3.0; 0.5 to 5.0; 1.0 to 10.0; 3.0 to 30.0; 5.0 to 50.0; 10.0 to 200.0; 1.0 to 200.0; 1.0 to 500.0 or 10.0 to 500.0 mg/ml and any combination thereof. In one embodiment, the silica shell thickness is between 2 and 100 nm and in another embodiment between 5 and 50 nm. In various embodiments, the silica shell thickness is between 3 and 20 nm, 5 and 20 nm, 10 and 50 nm, 10 and 50 nm, 10 and 100 nm, 1 and 10 nm, 3 and 30 nm, 5 and 50 nm and/or 5 and 200 nm and any combination thereof. The silica shell can be manufactured from a mixture of silanes that includes, but is not limited to, aminopropyl triethoxy silane, mercaptopropyl triethoxy silane, and tetraethylorthosilicate silicate. The silica shell may contain nitrogen or sulfur atoms. The silica shell may contain amine chemical moieties or mercap chemical moieties.
    [0080] [0080] In another embodiment, the solution contains a buffer, which includes a water-soluble salt (e.g., one or more of the sulfates, carbonates, chromates, borates, phosphates and sulfides, acetates and nitrates) at a concentration greater than 0.1 mM, 1.0 mM or 10.0 mM. In various embodiments, the concentration of water-soluble salt can be from 0.1 mM to 1 mM, 0.3 mM to 3 mM, 0.5 mM to 5 mM, 1 mM to 10 mM, 1 mM to 30 mM, 1 mM to 50 mM, 1 mM to 1000 mM and any combinations thereof. The solution may have a peak absorption wavelength between 500 nm and 1,500 nm, 500 nm to 1,200 nm, 500 nm to 1,000 nm, 600 nm to 1,200 nm, 700 nm to 1,200 nm, 700 nm to
    [0081] [0081] In various embodiments, the concentrated particles are stored at temperatures below -10, 0, 4, 6, 10 or 20 degrees C. In one embodiment, the particles are frozen and dried under vacuum. In one embodiment, the particles are freeze-dried. In one embodiment, the particles are supercritically dried. In one embodiment, an additional stabilizer or other cryoprotectant is added to the solution before the particles are heat-dried or freeze-dried. COMPOSITES
    [0082] [0082] In one embodiment of the invention, high optical density solutions of silver nanoplates are associated with a substrate. In various embodiments, examples of substrates include fibers, cloth, mesh, bandages, socks, wraps, other garments, sponges, high porosity substrates, particles with edge lengths greater than 1 micron, microspheres, hair, skin, paper, absorbent polymers, foam, wood, cork, foil, rough surfaces, biocompatible substrates, filters or medical implants. In various embodiments, silver nanoplate solutions at a concentration of at least 1 mg/ml, 10 mg/ml and/or 100 mg/ml are incubated with the substrate. In various embodiments, the concentration of silver nanoplate incubated with the substrate is between 0.1 to 1.0, 0.3 to 3.0; 0.5 to 5.0; 1.0 to 10.0; 3.0 to 30.0; 5.0 to 50.0; 10.0 to 20.0; 5.0 to 50.0; 3.0 to 50.0; 1.0 to 100.0 mg/ml; 10.0 to 100.0; 20.0 to 100.0; 30.0 to 100.0 mg/ml. In another embodiment, solutions of silver nanoplates incubated with the substrate have between 106 and 1013, 107 and 1013, 108 and 1013, 109 and 1013, 1010 and 1013, 1011 and 1013, 1012 and 1013 or more than 1013 particles per milliliter. In another embodiment, silver nanoplates are prepared to an optical density of at least 10, 20, 50, 100, 300, 500, 1000 and/or 2000 cm -1 prior to incubation with the substrate. In various embodiments, silver nanoplates are prepared to an optical density between 10 to 100, 20 to 200, 30 to 300, 50 to 500, 100 to 1,000, 200 to 1,000, 300 to 1,000, 500 to 1,000 or 200 The
    [0083] [0083] In one embodiment, the substrate is separated from the incubation solution and dried. The substrate can be dried using air drying, heat drying, freeze drying or supercritical drying. In another embodiment, the dried substrate may be further processed by immersing the substrate in another material, painting the substrate with another material, or exposing the substrate to another material that is in the vapor phase.
    [0084] [0084] Other embodiments of the invention will become apparent to those skilled in the art from consideration of the specification and practice of the invention disclosed herein. The specification and examples are intended to be considered only as they reveal certain embodiments of the invention, a true scope and spirit of the invention being indicated by the following claims.
    [0085] [0085] The matter described in this document may be incorporated in other specific forms without departing from the spirit or essential characteristics of the same. The aforementioned modalities must therefore be considered, in any case, as illustrative rather than limiting. While the embodiments are susceptible to various modifications and alternative forms, specific examples thereof have been shown in the drawings and are, herein, described in detail. It should be understood, however, that the invention is not to be limited to the specific forms or methods disclosed, however, on the other hand, the invention should cover all modifications, equivalents and alternatives that fall within the spirit and scope of the various embodiments described and the attached claims. Any methods disclosed in this document need not be performed in the order mentioned.
    [0086] [0086] The methods disclosed in this document include certain actions performed by a technician; however, they also include any instructions from third parties regarding such actions, either expressly or by implication. For example, actions such as "identify a target region of skin tissue" include "instruct identification of a target region of skin tissue".
    [0087] [0087] The ranges disclosed in this document also encompass any and all overlays, sub-ranges and combinations thereof. Language such as "up to", "at least", "greater than", "less than", "between" and the like includes the mentioned number. Numbers preceding a term, such as "about" or "approximately" or "substantially" include the mentioned numbers. For example, "about 3 mm" includes "3 mm". The terms "approximately", "about" and/or "substantially" as used herein represent an amount or characteristic close to the mentioned amount or characteristic that still performs a desired function or achieves a desired result. For example, the terms "approximately", "about" and "substantially" can refer to an amount that is less than 10% of, less than 5% of, less than 1% of, less than 0.1 % of and less than 0.01% of the quantity or characteristic mentioned. EXAMPLES
    [0088] [0088] The description of specific examples below is for the purpose of illustration only and is not intended to limit the scope of the invention disclosed herein. Example 1: Silver Nanoplates
    [0089] [0089] Silver nanoplates were synthesized using silver seeds prepared by reducing silver nitrate with sodium borohydride in the presence of tribasic sodium citrate and polysodium styrene sulfonate under aqueous conditions. Silver seed preparation: 21.3 ml of a 2.5 mM aqueous tribasic sodium citrate solution can be mixed under magnetic stirring. 1 ml of a 2 g/l solution of sodium polystyrene sulfonate (PSSS) was then prepared in a separate beaker. 21.3 ml of a 0.5 mM silver nitrate solution was then prepared by dissolving the salt in water. Once the above solutions were prepared, 1.33 ml of a 0.5 mM sodium borohydride solution was prepared in water at 4°C. The boron hydride and PSSS solutions were then added to the beaker containing the citrate and allowed to mix. The silver nitrate solution was then pumped into the citrate solution using a peristaltic pump at a rate of 100 ml/min. Such a seed solution can then be stirred overnight at room temperature. Silver nanoplates were prepared by mixing 1,530 ml of Milli-Q water with 35 ml of a 10 mM ascorbic acid solution. Once the solution was sufficiently mixed, the prepared silver seed was added to the reactor. 353 ml of a 2 mM silver nitrate solution was pumped into a reactor at a rate of 100 ml/min. The reaction was mixed for two hours. TEM analysis showed that over 70% of the particles are nanoplates. The optical density of the solution was 2.8 cm -1 . Example 2: Concentrated silver nanoplates
    [0090] [0090] 15 l of the silver nanoplates with a peak optical density of about 5 cm-1 were mixed with 3.5 g of polyvinyl alcohol.
    [0091] [0091] In an example for concentrating silver nanoplates, 1.2 l of silver nanoplates with a peak optical density of about 4 cm-1 were mixed with 4 l of anhydrous ethanol and about 49 ml of anhydrous ethanol solution. Ammonium hydroxide. 0.6 ml of a dilute aminopropyltriethoxysilane (APTES) was added to the solution. After 15 minutes of incubation, 6.5 ml of tetraethylorthosilicate silicate (TEOS) solution was added. After 24 hours 1 L of the solution was concentrated using a 500 kD polysulfone tangential flow membrane with 1050 cm2 of surface area. The final solution volume was decreased to 150 ml so as to increase the optical density of silver nanoparticle solution to about 40 cm -1 . Thus, according to one embodiment, a method for increasing a silver nanoplate solution from 4 cm-1 to 40 cm-1 (for example, an approximately 10-fold increase in optical density) comprises the steps adding anhydrous ethanol, ammonium hydroxide solution, aminopropyltriethoxysilane (APTES) and tetraethylorthosilicate silicate (TEOS) to the silver nanoplates and concentrating the solution with tangential flow filtration.
    [0092] [0092] The silica shell grew on the surface of 800 nm resonant (~75 nm edge length) closed silver polyvinyl pyrrolidone (PVP) nanoplates. 400 ml of an 800 nm solution of resonant PVP silver nanoplates at a concentration of 2 mg/ml (20 cm-1 OD) was added to 2.3 l of reagent grade ethanol and 190 ml of Milli water. -Q under constant stirring. 4.3 ml of diluted aminopropyl triethoxysilane (215 µl of APTES in 4.085 ml of isopropanol) were then added to the solution, followed immediately by the addition of 44 ml of 30% ammonium hydroxide. After 15 minutes of incubation, 31 ml of diluted tetraethylorthosilicate silicate (1.55 ml of TEOS in 29.45 ml of isopropanol) was then added to the solution. The solution was then left to stir overnight. The nanoplates were then centrifuged in an Ultra centrifuge at 17,000 RCF for 15 minutes and reconstituted in Milli-Q water each time and repeated twice. Silica shell thickness was 15 nm. The optical density of the concentrated material was 2040 cm-1. Example 5
    [0093] [0093] 40 ml of 40 O.D. of concentrated silver nanoplate solution stabilized with polyvinyl alcohol and sodium borate were spun at 3000 RCF for 30 minutes. The supernatant was removed and the pellet was redispersed with bath sonication. The concentrated silver nanoplates obtained an optical density greater than 900 O.D. as shown in Figure 8. Example 6: Nanoplates concentrated on a Substrate
    [0094] [0094] A 5 ml solution of 1,000 O.D. of silver nanoplates was added to a 3" x 3" section of absorbent cloth (Absorber Synthetic Drying Chamois, Clean Tools). After addition, the substrate can be air dried. Once dried, the silver nanoplates were
    [0095] [0095] Each of the references listed above is incorporated by reference in their entirety.
    权利要求:
    Claims (30)
    [1]
    1. Process to produce concentrated silver nanoplates that preserve the post-concentration format while increasing the optical density, the process being characterized by the fact that it comprises: adding a stabilizing agent to the pre-concentrated solution; wherein the pre-concentrated solution comprises silver nanoplates; wherein each of the silver nanoplates has a plate shape; wherein the pre-concentrated solution has a peak optical density at a first wavelength; increasing the concentration of silver nanoplates in the pre-concentrated solution to generate a pre-concentrated solution, where the concentrated solution has a peak optical density at a second wavelength, where the first wavelength is substantially higher. te the same as the second wavelength; in which the peak optical density of the concentrated solution is greater than the peak optical density of the preconcentrated solution, and in which at least a portion of the silver nanoplates in the preconcentrated solution retain the plate shape in the concentrated solution .
    [2]
    2. Process according to claim 1, characterized in that the stabilizing agent comprises: (i) a polymer derived with sulfonate and a molecule comprising an amine or thiol chemical group, or (ii) a polymer based on polyvinyl and a borate.
    [3]
    3. Process according to claim 2, characterized in that the sulfonate-derived polymer comprises polystyrene sodium sulfonate.
    [4]
    4. Process according to claim 2, characterized in that the amino chemical group comprises at least one of the group consisting of: an aminopropyltriethoxysilane (APTES) and an amine chemical moiety.
    [5]
    5. Process according to claim 2, characterized in that the thiol chemical group comprises at least one of the group consisting of: a lipoic acid, a mercaptohexadecanoic acid, a mercaptoundecanoic acid and a dihydrolipoic acid .
    [6]
    6. Process according to claim 2, characterized in that the polyvinyl-based polymer comprises at least one of the group consisting of: a polyvinyl pyrrolidone (PVP) and a polyvinyl alcohol (PVA).
    [7]
    7. Process according to claim 2 characterized in that the borate comprises sodium borate.
    [8]
    8. Process according to any one of claims 1 to 7, characterized in that the concentration increase is carried out using tangential flow filtration, in which the peak optical density of the concentrated solution is at least ten times the peak optical density of the preconcentrated solution, where the peak optical density of the concentrated solution is at least 100 cm-1, where the second wavelength of the concentrated solution is in a range between 300 nm and 1500 nm, and wherein at least one optical property of the concentrated solution is substantially equal to the pre-concentrated solution in the sense that the peak optical density of the pre-concentrated solution and the peak optical density of the concentrated solution occur at substantially the same wavelength, and where the portion of the silver nanoplates that retain the plate shape is more than 90% in the concentrated solution.
    [9]
    9. Process according to any one of claims 1 to 8, characterized in that the silver nanoplates are prepared through a seed-mediated growth mechanism, wherein the seed-mediated growth mechanism comprises: combining citrate, polystyrene sodium sulfonate (PSSS) and sodium borohydride in a first solution, add silver nitrate to the first solution to form a seed solution, add a portion of the seed solution to a second solution, where the second solution comprises ascorbic acid, and adding silver nitrate to the second solution to form the pre-concentrated solution.
    [10]
    10. Process according to any one of claims 1 to 9, characterized in that increasing the concentration is carried out using tangential flow filtration, in which tangential flow filtration uses a filter membrane with pores. with a molecular weight cutoff in a range between 10 kDa and 0.05 micron, where the peak optical density of the concentrated solution is at least ten times greater than the peak optical density of the pre-concentrated solution. , where the peak optical density of the concentrated solution is at least 100 cm-1.
    [11]
    Process according to any one of claims 1 to 10, characterized in that it additionally comprises coating the silver nanoplates with silica, wherein coating the silver nanoplates with silica comprises: adding ethanol to the pre-concentrate solution, add a base to the pre-concentrate solution, and add a silane to the pre-concentrate solution.
    [12]
    12. Process according to any one of claims 1 to 11, characterized in that the second wavelength is in a range between 300 nm and 1,100 nm, and in which the optical density of the preconcentrated solution is - is in a range between 0.1 to 10 cm-1 and the optical density of the concentrated solution is at least 100 cm-1.
    [13]
    Process according to any one of claims 1 to 12, characterized in that it additionally comprises forming a metal oxide shell or polystyrene shell on the surface of the silver nanoplate.
    [14]
    14. Process according to claim 13, characterized in that the metal oxide shell is any one of a group consisting of: a silica shell and a titanium dioxide shell, wherein the metal oxide shell has a thickness in the range of 1 nm to 100 nm.
    [15]
    Process according to any one of claims 1 to 14, characterized in that it additionally comprises adding any one of the group selected from: an acid, a base and a buffering agent to the pre-mixed solution. concentrated.
    [16]
    Process according to any one of claims 1 to 15, characterized in that the second wavelength is up to 10% of the first wavelength.
    [17]
    Process according to any one of claims 1 to 16, characterized in that the silver nanoplates have an edge length in a range between 10 nm and 250 nm.
    [18]
    18. Process according to any one of claims 1 to 17, characterized in that the portion of the concentrated silver nanoplates that retain the plate format after increasing the concentration is greater than 80%.
    [19]
    Process according to any one of claims 1 to 18, characterized in that the pre-concentrated solution is formed using a seed-mediated growth method.
    [20]
    Process according to any one of claims 1 to 19, characterized in that the pre-concentrated solution is centrifuged after increasing the concentration using tangential flow filtration.
    [21]
    Process according to any one of claims 1 to 20, characterized in that the pre-concentrated solution is incubated with a substrate, wherein the substrate comprises a fiber.
    [22]
    22. Composition characterized in that it comprises: a plurality of silver nanoplates in a solution comprising an optical density, in which the silver nanoplates comprise a coating on a surface of the silver nanoplates, in which the density optics is greater than 100 cm-1
    [23]
    23. Composition according to claim 22, characterized in that the coating comprises (i) a 9/17 polystyrene sodium sulfonate and at least one agent selected from the group consisting of: a molecule that contains amine and a thiol-containing molecule, or (ii) a borate and at least one agent selected from the group consisting of: a polyvinyl-based polymer
    [24]
    24. Composition according to claim 23, characterized in that the coating comprises said amine-containing molecule, wherein the amine-containing molecule comprises at least one of the group consisting of: aminopropyltriethoxysilane (AP-TES) and an amine moiety.
    [25]
    25. Composition according to claim 23, characterized in that the borate comprises at least one of a group consisting of: a sodium borate and a potassium tetraborate.
    [26]
    26. Composition according to claim 23, characterized in that the coating comprises said polyvinyl-based polymer, wherein the polyvinyl-based polymer is selected from the group consisting of: a polyvinyl pyrrolidone (PVP) and a polyvinyl alcohol (PVA).
    [27]
    27. Composition according to claim 23, characterized in that the coating comprises said thiol-containing molecule, wherein the thiol-containing molecule comprises at least one of the group consisting of: a lipoic acid, a mercaptohexadecanoic acid, a mercaptoundecanoic acid and a dihydrolipoic acid.
    [28]
    28. Composition according to any one of claims 22 to 27, characterized in that the coating additionally comprises a metal oxide shell.
    [29]
    29. Composition according to any one of claims 22 to 28, characterized in that the metal oxide shell is any one of the group consisting of: a silica shell and a titanium dioxide shell, in that the 10/17 metal oxide shell has a thickness in a fixed range between 1 nm to 100 nm.
    [30]
    30. Invention, characterized by any of its realizations or claim categories encompassed by the matter initially disclosed in the patent application or in its examples presented herein.
    11/17
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    法律状态:
    2018-01-02| B25G| Requested change of headquarter approved|Owner name: NANOCOMPOSIX, INC. (US) , SIENNA LABS, INC. (US) |
    2018-01-16| B25D| Requested change of name of applicant approved|Owner name: NANOCOMPOSIX, INC. (US) , SIENNA BIOPHARMACEUTICAL |
    2018-02-27| B25G| Requested change of headquarter approved|Owner name: NANOCOMPOSIX, INC. (US) , SIENNA BIOPHARMACEUTICAL |
    2018-11-21| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|
    2019-12-10| B06U| Preliminary requirement: requests with searches performed by other patent offices: procedure suspended [chapter 6.21 patent gazette]|
    2021-05-04| B07D| Technical examination (opinion) related to article 229 of industrial property law [chapter 7.4 patent gazette]|Free format text: DE ACORDO COM O ARTIGO 229-C DA LEI NO 10196/2001, QUE MODIFICOU A LEI NO 9279/96, A CONCESSAO DA PATENTE ESTA CONDICIONADA A ANUENCIA PREVIA DA ANVISA. CONSIDERANDO A APROVACAO DOS TERMOS DO PARECER NO 337/PGF/EA/2010, BEM COMO A PORTARIA INTERMINISTERIAL NO 1065 DE 24/05/2012, ENCAMINHA-SE O PRESENTE PEDIDO PARA AS PROVIDENCIAS CABIVEIS. |
    2021-05-18| B07G| Grant request does not fulfill article 229-c lpi (prior consent of anvisa) [chapter 7.7 patent gazette]|Free format text: NOTIFICACAO DE DEVOLUCAO DO PEDIDO POR NAO SE ENQUADRAR NO ART. 229-C DA LPI. |
    2021-08-31| B15I| Others concerning applications: loss of priority|Free format text: PERDA DA PRIORIDADE US 61/795,149 REIVINDICADA NO PCT/US2013/063920, CONFORME AS DISPOSICOES PREVISTAS NA LEI 9.279 DE 14/05/1996 (LPI) ART. 167O, ITEM 28 DO ATO NORMATIVO 128/97 E NO ART. 29 DA RESOLUCAO INPI-PR 77/2013. ESTA PERDA SE DEU PELO FATO DE O DEPOSITANTE CONSTANTE DA PETICAO DE REQUERIMENTO DO PEDIDO PCT SER DISTINTO DAQUELES QUE DEPOSITARAM A PRIORIDADE REIVINDICADA E NAO APRESENTOU DOCUMENTO DE CESSAO REGULARIZADO DENTRO DO PRAZO DE 60 DIAS A CONTAR DA DATA DA PUBLICACAO DA EXIGENCIA, CONFORME AS DISPOSICOES PREVISTAS NA LEI 9.279 DE 14/05/1996 (LPI) ART. 166O, ITEM 27 DO ATO NORMATIVO 128/97 E NO ART. 28 DA RESOLUCAO INPI-PR 77/2013. |
    2021-10-13| B07A| Application suspended after technical examination (opinion) [chapter 7.1 patent gazette]|
    2022-01-18| B09B| Patent application refused [chapter 9.2 patent gazette]|
    优先权:
    申请号 | 申请日 | 专利标题
    US201261795149P| true| 2012-10-11|2012-10-11|
    PCT/US2013/063920|WO2014058904A1|2012-10-11|2013-10-08|Silver nanoplate compositions and methods|
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