Quaternary ammonium based broad spectrum disinfectant

Abstract

Various examples disclosed relate to a broad-spectrum disinfectant. The present disclosure includes a quaternary-ammonium based formulation for a disinfectant solution useable on hard surfaces. The formulation can include an active ingredient including didecyl dimethyl ammonium chloride (DDAC), a surfactant including alkyl polyethylene glycol ether, and at least one solvent component. The disinfectant solution can have a neutral pH, such as of about 6.0 to about 8.5.

Description

QUATERNARY AMMONIUM BASED BROAD SPECTRUM DISINFECTANTCROSS-REFERENCE TO RELATED APPLICATION

[0001] This application claims the benefit of priority to U.S. Provisional Patent Application Serial No. 63 / 485,143 entitled “Quaternary Ammonium Based Broad Spectrum Disinfectant with Neutral pH,” filed Feb 15, 2023, the disclosure of which is incorporated herein in its entirety by reference.BACKGROUND

[0002] A variety of disinfectants, including quaternary ammonium disinfectants, are on the market, and can be used for treatment of surfaces to remove or reduce microbials thereon. Many of these come as dilutable disinfectants, or as ready-to-use disinfectants. These disinfectants are generally alkaline in nature.SUMMARY OF THE DISCLOSURE

[0003] In an example, a formulation for a disinfectant solution useable on hard surfaces can include an active agent including didecyl dimethyl ammonium chloride (DDAC); a surfactant including alkyl polyethylene glycol ether; and at least one solvent component. The formulation has a pH of about 6.0 to about 8.5.

[0004] In an example, a formulation for a disinfectant can include didecyl dimethyl ammonium chloride (DDAC) in an amount of about 10.00 wt.% of the formulation; alkyl polyethylene glycol ether in an amount of about 1.00 wt.% of the formulation; and isopropyl alcohol in an amount of about 5.50 wt.% of the formulation.DETAILED DESCRIPTION

[0005] Reference will now be made in detail to certain examples of the disclosed subject matter. While the disclosed subject matter will be described in conjunction with the enumerated claims, it will be understood that the exemplified subject matter is not intended to limit the claims to the disclosed subject matter.

[0006] Quaternary-ammonium based disinfectants currently on the market are typically alkaline in nature and can have pH ranges that are harsh on certain surfaces. While alkalinity can help efficacy, too high of alkalinity can damage surfaces, and negatively impact safety profiles associated with those disinfectants. An effective, but pH neutral, disinfectant could be beneficial.

[0007] Additionally, some disinfectants leave noticeable residue that can interfere with later work on the surface. In some cases, consumers prefer to alternate various disinfectants. In this case, residue from a first disinfectant can interfere with a second disinfectant applied to the same surface. Moreover, disinfectant residuals can build up over time, causing unsightly surfaces and potential slip hazards. Higher residue disinfectants can also lower productivity by causing the user to repeatedly rinse the surface.

[0008] Discussed herein is a formulation for a broad-spectrum disinfectant that is quaternary ammonium based. The formulation includes didecyl dimethyl ammonium chloride (DDAC) as an active ingredient, with alkyl polyethylene glycol ether as a surfactant.

[0009] The disinfectant sufficiently passes test for disinfectants under EPA and EU regulatory standards, has a non-alkaline pH, is relatively stable under irradiation, and produces a low residual profile. The disinfectant formulation discussed herein can be prepared, for example, with 10 wt.% DDAC and designed to be used at a 2% v / v dilution.

[0010] The formulation discussed herein can have a broad-spectrum use, such as to maintain a low microbial contamination within the treated environment, such as by disinfecting efficacy with a variety of microbial agents such as bacteria, viruses, and fungi. The formulation includes an oxirane, methyl-, polymer with oxirane, mono(2 -propylheptyl) ether, nonionic surfactant, that shows excellent wetting properties and has synergistic effects with the active DDAC when tested for efficacy.

[0011] The disinfectant formulation has a pH in a range of about 6.0 to about 8.5, much lower than some formulation that are alkaline in nature. Existing quaternary ammonium-based disinfectants are in use, but they can tend to damage surfaces due to alkalinity. The neutral pH of this formulation provides substantial benefit that allows application to a wide variety of surfaces without such damage.

[0012] Additionally, the formulation (in a concentrate form) is stable in use dilution over extended periods of time, such as over a month. The formulation maintains its stability under irradiation such as gamma and x-ray irradiation. Specifically, the use of the straight chain DDAC as the active agent can allow for a stable disinfectant formulation under radiation. An alternative ready to use formulation can also be used. For example, a ready to use version of the formulation can be provided as a 2% solution, instead of a concentrate.

[0013] Finally, the formulation also provides lower residuals, which can reduce slip tendencies. The formulation discussed herein may also be suitable as a rotational pair disinfectant due to low residuals.Broad-Spectrum Disinfectant Composition

[0014] Various example disinfectant formulations herein include didecyl dimethyl ammonium chloride (DDAC) as the active agent, in combination with isopropyl alcohol as a co-solvent and alkyl polyethylene glycol ether as a surfactant. The surfactant and the active agent together can improve the contact of the disinfectant with surfaces being disinfected. In some examples, citric acid and potassium hydroxide, or other appropriate weak acids and basic salts can be used to make minor pH adjustments and bring the pH of the disinfectant formulation to a range of about 6.0 to about 8.5.

[0015] The example formulations herein are intended to be diluted for use, such as diluted wt. 2.0% v / v for standard use, or for example from about 1.0% to about 3.0% v / v. For example, the formulation can include an active agent including didecyl dimethyl ammonium chloride (DDAC), a surfactant including alkyl polyethylene glycol ether, at least one solvent component, and optionally pH adjusters. The formulation can have a pH of about 6.0 to about 8.5.

[0016] In the example formulations here, the active agent is DDAC, a quaternary ammonium compound often used as an antiseptic or disinfectant. DDAC is a straight chain polymer having a chemical formula of C22H48CIN, a molar mass of 362.08 g / mol, and a density of 0.87 g / cm3at 20 °C. DDAC acts as an antimicrobial agent by disrupting intermolecular interactions and dissociating lipid bilayers. DDAC is a broad spectrum biocidal against bacteria and fungi.

[0017] In the formulations discussed herein, the DDAC can be in an amount of about 5.00 wt.% to about 20.00 wt.% of the formulation, in an amount of about 8.00 wt.% to about 15.00 wt.% of the formulation, or in an amount of about 9.00 wt.% to about 12. 00 wt.% of the formulation. In the formulations discussed herein, the DDAC can be in an amount of about 1,000 ppm to about 4,000 ppm, or of about 2,000 ppm once the product is diluted to use levels.

[0018] In the example formulations here, the surfactant is alkyl polyethylene glycol ether, a cleaning agent or surfactant that works by emulsifying contaminant that remains. The active agent DDAC has a synergistic effect with the alkyl polyethylene glycol ether, helping improve broad spectrum efficacy as illustrated below in the Examples.

[0019] The surfactant can be provided as about 0.05 wt.% to about 2.00 wt.% of the formulation, about 0.08 wt.% to about 1.80 wt.% of the formulation, about 0.09 wt.% to about 1.30 wt.% of the formulation, or about 0.10 wt.% to about 1.00 wt.% of the formulation.

[0020] The formulation can further include one or more solvent components, such as two cosolvents. In an example, the one or more solvent components can include deionized water, isopropyl alcohol, n-propanol, ethanol, or a combination thereof. In an example, the one or more solvent components can be up to about 95.00 wt.% of the formulation.

[0021] In an example, a solvent component can be isopropyl alcohol, being about 5.10 to about 5.90 wt.% of the formulation, about 5.00 to about 6.00 wt.% of the formulation, or about 4.00 to about 7.00 wt.% of the formulation.

[0022] In an example, a solvent component can include deionized water being about 75.00 to about 90.00 wt.% of the formulation, about 80.00 to about 86.00 wt.% of the formulation, or about 82.00 to about 85.00 wt.% of the formulation.

[0023] In an example, the formulation can include one or more pH adjusters. For example, the formulation can include one or more weak acids, such as an organic acid. Examples of such acids can include citric acid, lactic acid, acetic acid, formic acid, oxalic acid, uric acid, malic acid, tartaric acid, or combinations thereof. The organic acid can be up to about 0.0010 wt.% of the formulation, up to about 0.0005 wt.% of the formulation, or up to about 0.0001 wt.% of the formulation.

[0024] In an example, the formulation can include a base, such as a salt, or a hydroxide salt, as a pH adjuster. For example, the base can include potassium hydroxide or sodium hydroxide. The base can be up to about 0.0010 wt.% of the formulation, up to about 0.0005 wt.% of the formulation, or up to about 0.0001 wt.% of the formulation.

[0025] The pH adjusters can be used to tailor the pH of the formulation, such as to about 6.0 to about 8.8, about 6.4 to about 8.6, or about 6.5 to about 8.5, such that the formulation has a neutral pH.Ready to Use Formulation

[0026] In another example, the formulation can be prepared as a ready-to-use formulation instead of a concentrate. For example, the ready-to-use formulation can include about 2% of the formulation in a solvent. Example ready to use formulations can include, for example, the concentrate formulations discussed above, in combination with one or more solvents and / or buffers.

[0027] In an example, the concentrate formulation can be provided in the ready to use formulation at an amount of about 1.0 wt.% to about 3.0 wt.%, or of about 1.0, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2.0, 2.1, 2.2, 2.3, 2.4, 2.5, 2.6, 2.7, 2.8. 2.9. or about 3.0 wt.% of the total ready to use formulation.

[0028] In an example, the overall amount of DDAC in the ready to use formulation can be about 1,500 ppm or more, about 1,700 ppm or more, or about 2,000 ppm or more, such as about 1,500, 1,600, 1,700, 1,800, 1,900, or 2,000 ppm. In an example, the DDAC in the ready to use formulation can be about 0.15 wt.% to about 0.25 wt.% of the formulation. In an example, alkyl polyethylene glycol ether (from the concentrate) can be in an amount of about 0.01 wt.% to about 0.03 wt.% of the formulation.

[0029] In an example, the solvents in the ready to use formulation can include water, isopropyl alcohol, N-propyl alcohol, or combinations thereof. In an example, the water in the ready to use formulation can be about 85.0 wt.% to about 95.0 wt.% of the formulation. In an example, the isopropyl alcohol in the ready to use formulation can be in an amount of about 10.0 wt.% to about 10.5 wt.% of the formulation.

[0030] In an example, the buffers in the ready to use formulation can include an acid and a base, such as those discussed above. In an example, citric acid can be provided in an amount of about 0.005 wt.% to about 0.02 wt.% of the formulation. In an example, potassium hydroxide can be provided in an amount of about 0.01 wt.% to about 0.05 wt.% of the formulation

[0031] Such a ready to use formulation can be provided in a package such as a trigger sprayer to prevent user interactions with the concentrated disinfectant.Method of Making Broad-Spectrum Disinfectant

[0032] The formulation discussed herein can be prepared in a variety of ways, such as by using any suitable preparation method. For example, the formulation can be made by combining the active agent, the surfactant, and the one or more solvent components, and optionally pH adjusters. All the components can be stirred or otherwise mixed to form the final formulation.

[0033] The ready to use formulation can be prepared by mixing the concentrate with one or more solvents and / or buffers. For example, the concentrate formulation can be combined with water, n-propyl alcohol, and / or isopropyl alcohol, such as by stirring. In an example, a stir bar can be used at a low speed to mix the components until a homogenous solution is made, for example about three to five minutes. In some cases, buffers such as acids or bases as discussed above, can also be added.Method of Using Broad-Spectrum Disinfectant

[0034] The formulation discussed herein can be applied to surfaces for disinfecting in a variety of ways. In some cases, the concentrated formulation can be diluted, such as with water, at an amount of about 2% v / v. In some cases, such a diluted formulation can beapplied to the surface by spraying, dropping, wiping, or other appropriate methods. In some examples, the formulation can be prepared as a ready to use formulation, instead of a dilutable concentrate.

[0035] When applied to a surface, wiped, and allowed to sit for a day, the formulation can have little to no visual residue. In some cases, little to no residue can be visually observed after 10 minutes, 30 minutes, 1 hour, 6 hours, 12 hours, 18 hours, or 24 hours.

[0036] When applied to a surface, the formulation can kill a sufficient amount of microbials to pass according to the AOAC UDT protocol (2013), the ASTM E1053 protocol (2020), the EN13697 (2015), EN1276 (2019), EN1650 (2019), EN16777 (2018) , and EN14476 protocols (2013), and combinations thereof, with a contact time of ten minutes or more.

[0037] The formulation can be relatively stable, having a 98.0 wt.% or better recovery of the active agent when irradiated with a dose of 50 kGy or more.

[0038] For the ready to use formulation, a package such as a trigger sprayer can be used. In this case, the user can use the trigger sprayer to spray the ready to use formulation onto a surface. The surface can be wiped as described above.Definitions

[0039] Throughout this document, values expressed in a range format should be interpreted in a flexible manner to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a range of “about 0.1% to about 5%” or “about 0.1% to 5%” should be interpreted to include not just about 0.1% to about 5%, but also the individual values (e.g., 1%, 2%, 3%, and 4%) and the sub-ranges (e.g., 0.1% to 0.5%, 1.1% to 2.2%, 3.3% to 4.4%) within the indicated range. The statement “about X to Y” has the same meaning as “about X to about Y,” unless indicated otherwise. Likewise, the statement “about X, Y, or about Z” has the same meaning as “about X, about Y, or about Z,” unless indicated otherwise.

[0040] In this document, the terms “a,” “an,” or “the” are used to include one or more than one unless the context clearly dictates otherwise. The term “or” is used to refer to a nonexclusive “or” unless otherwise indicated. The statement “at least one of A and B” has the same meaning as “A, B, or A and B.” In addition, it is to be understood that the phraseology or terminology employed herein, and not otherwise defined, is for the purpose of description only and not of limitation. Any use of section headings is intended to aid readingof the document and is not to be interpreted as limiting; information that is relevant to a section heading may occur within or outside of that particular section.

[0041] In the methods described herein, the acts can be carried out in any order without departing from the principles of the disclosure, except when a temporal or operational sequence is explicitly recited. Furthermore, specified acts can be carried out concurrently unless explicit claim language recites that they be carried out separately. For example, a claimed act of doing X and a claimed act of doing Y can be conducted simultaneously within a single operation, and the resulting process will fall within the literal scope of the claimed process.

[0042] The term “about” as used herein can allow for a degree of variability in a value or range, for example, within 10%, within 5%, or within 1% of a stated value or of a stated limit of a range and includes the exact stated value or range.

[0043] The term “substantially” as used herein refers to a majority of, or mostly, as in at least about 50%, 60%, 70%, 80%, 90%, 95%, 96%, 97%, 98%, 99%, 99.5%, 99.9%, 99.99%, or at least about 99.999% or more, or 100%.

[0044] The term “ready to use” as used herein can refer to a formulation that is prediluted and ready for use to disinfect a surface or other object.

[0045] The term “room temperature” as used herein refers to a temperature of about 15 °C to 28 °C. The term “standard temperature and pressure” as used herein refers to 20 °C and 101 kPa.

[0046] The term “solvent” as used herein refers to a liquid that can dissolve a solid, liquid, or gas. Non-limiting examples of solvents are silicones, organic compounds, water, alcohols, ionic liquids, and supercritical fluids.

[0047] The term “surface” as used herein refers to a boundary or side of an object, wherein the boundary or side can have any perimeter shape and can have any three- dimensional shape, including flat, curved, or angular, wherein the boundary or side can be continuous or discontinuous. While the term surface generally refers to the outermost boundary of an object with no implied depth, when the term ‘pores’ is used in reference to a surface, it refers to both the surface opening and the depth to which the pores extend beneath the surface into the substrate.Examples

[0048] Various examples of the present disclosure can be better understood by reference to the following Examples which are offered by way of illustration. The present disclosure is not limited to the Examples given herein.

[0049] Example 1. Disinfectant Concentrated Formulation Samples

[0050] Sample formulations of a dilutable concentrate disinfectant were produced to test for efficacy, pH, residue, and stability. The samples were prepared by mixing together an active component, didecyl dimethyl ammonium chloride (DDAC), with various surfactants, solvents, and other components. The samples were prepared by combing the DDAC with the other components and mixing with a stir bar at a low speed for approximately 3 to 5 minutes at room temperature. For the below samples, deionized water, IP A, DDAC, and the remaining ingredients were mixed together. The materials are miscible, so no additional heating or extended mix times were needed to create a homogeneous solution.

[0051] The samples produced by this method are summarized below in Table 1 :Table 1. Samples of Disinfectant Formulations

[0052] Here, Samples A and B are comparative samples with alternative surfactants. Samples C, D, E, and F use the inventive formulation including DDAC and alkyl polyethylene glycol ether in combination, which had a beneficial synergy.

[0053] Each of these samples were made with DDAC (Bardac 2280, Lonza Inc., Charlotte, NC, U.S.) as the active agent. The comparative samples A and B used either PEG- 15 cocomine (Ethomeen C / 25 A, Noury on, Houston, TX, U.S.) or C6-10 EOPO alcohol (Plurafac SL-62, BASF, Rexdale, ON, Canada) as the surfactant, while the Samples C, D, E and F used alkyl polyethylene glycol ether (Lutensol® XL80, BASF Corporation, Ludwigshafen, Germany) as the surfactant. The samples contained solvent components including isopropyl alcohol (Isopropanol, Anhydrous USP, Exxon, Milton, WI, U.S.) and deionized water. In comparative Samples A and B, trisodium ethylene diamine disuccinate (Natrlquest E30, Innospec Inc., Engelwood, Colorado, U.S.) was additionally used. In inventive Sample D, citric acid (Citric Acid, USP, Jungbunzlauer Inc., Port Colborne, Canada) and potassium hydroxide (45% caustic potash, Membrane Grade, Occidental Chemical Co., Taft, LA, U.S.) were used as additional components.

[0054] A Standard Use Dilution Test (UDT) was conducted on stainless steel surfaces with the Samples A to D. Here, the Samples were prepared with the same active ingredient (DDAC) but differing surfactants to observe the synergistic effect of the active ingredient with the surfactant. In the UDT test, the formulations were diluted at a use dilution of 2% v / v and were applied for a 4.75-minute contact time against Pseudomonas aeruginosa. Sixty replicates were conducted for each sample.

[0055] Samples D, using the DDAC active agent in combination with the alkyl polyethylene glycol ether surfactant, performed surprisingly and significantly better than the comparative Samples A and B using conventional surfactants (PEG- 15 cocomine and C6-10 EOPO alcohol, respectively). Specifically, the comparative Samples A and B provided 4 positives out of 60 replicates. By comparison, the inventive Sample D provide zero positive out of 60 replicates. The formulation Sample D containing the combination of DDAC, and alkyl polyethylene glycol ether outperformed even a formulation in Sample A or Sample B having 5 wt.% more of the active agent DDAC.

[0056] Example 2, Broad-Spectrum Efficacy of the Disinfectant Formulation

[0057] The inventive Sample D summarized in Table 1 was further tested for antimicrobial efficacy testing to demonstrate its broad-spectrum efficacy. The Sample was tested under methods recognized by the EPA and EU regulatory agencies. The Sample was tested under AOAC UDT, the ASTM E1053 test, and the EN13697, EN1276, EN1650, EN16777, and EN1446 test protocols with a 10-minute contact time.

[0058] Under these tests, the disinfectant formulation Sample was tested against various bacteria, fungi, and viruses. In these tests, a ten minute contact time was used underdirty conditions (e.g., with the formula diluted in hard water). The results of these tests are summarized below in Table 2 and Table 3.Table 2. EP A Standard Efficacy Testing.

[0059] Summarized in Table 2, the Sample was tested for disinfectant efficacy compared to several bacterium (Staphylococcus aureus, Pseudomonas aeruginosa, Staphylococcus epidermidis, Enterobacteria cloacae, Serratia marcescens, Burkholderia cepacian, Listeria monocytogenes, Mycoplasma gallisepticum), a fungus (Candida albicans'), and several viruses (Influenza A2, Avian Influenza Virus, Minute virus of Mouse, Caliciviridae), with standard protocol followed by the EPA.

[0060] The AOAC Use Dilution Test (UDT) protocol1, Nos. AOAC 955.14; 955.15; 964.02, includes test protocols for bacteria and fungi. Here, the Samples were tested by soaking stainless steel carriers in bacteria (or other microbes), then treating them with the disinfectant, and finally placing the carriers in growth broth to determine if any still have surviving bacteria (or other microbes).1Under the AOAC UDT protocols, the Samples were tested with a 48-hour culture of the microbe on small, cylindrical stainless steel test surfaces. The carriers were soaked in the microbial culture, and subsequently dried. Each dry, contaminated test carrier was transferred to a test tube filled with 10 mL disinfectant, where they were incubated for a set period of time. The treated test surfaces were incubated in neutralizing growth medium for 48 horns, then analyzed. Additional detail can be found under AOAC specific protocols 955.14; 955.15; 964.02.

[0061] The ASTM E10532protocol includes test protocols for viruses. Here, the Samples were tested by first preparing the virus(es) and inoculating the carriers. An aliquot of the test liquid substance was applied to the dried virus film. A neutralization / infectivity assay was prepared and reviewed. Various controls were used under the ASTM E1053 protocols.

[0062] Under these EPA approved protocols, the inventive Sample D passed every test, including compared to bacteria, fungi, and viruses, sufficiently killing these various microbes. The samples were additionally tested under EU approved protocols, summarized in Table 3 below.Table 3. EU Standard Efficacy Testing.

[0063] Summarized in Table 3, the Samples were tested for disinfectant efficacy compared to several bacterium (Staphylococcus aureus, Pseudomonas aeruginosa, Escherichia coli, and Enterococcus hirae), fungi (Candida albicans and Aspergillus brasiliensis), and a virus (Vaccinia virus), with standard protocol followed by the EU regulatory agencies.

[0064] The protocols used here are European Standards. The EN13697 protocol3was used to analyze the disinfectant formulation efficacy with bacteria and fungi. The EN136972Under the ASTM 1053 protocol, 100 x 15 mm petri dishes were used as carriers. The test virus was prepared by thawing and diluting as appropriate. The carriers were inoculated with the virus using sterile bent pipette tips, and the inoculated carriers were dried. The sample disinfectant formulations were applied as a liquid aliquot to the dried vims film. The surviving microbes were determined.3Under the EN13697 protocol, a test suspension of bacteria or fungus is inoculated onto the surface of stainless steel and allowed to dry. Sample disinfectant, diluted in hard water, are applied to the surface of the dried microbial film and maintained in contact for a predetermined time period and time. Subsequently, the surface isprotocol is a quantitative non-porous surface test for the evaluation of bacterial and / or fungal activity of chemical disinfectants. The EN1276 protocol4was used to analyze the disinfectant formulation efficacy with bacteria. The EN1276 protocol specifies a suspension test for establishing whether a chemical disinfectant or antiseptic has bactericidal activity. The EN1650 protocol5was used to analyze the disinfectant formulation efficacy with fungi. The EN1650 protocol is a quantitative suspension test for evaluation of fungicidal activity of disinfectants. The EN16777 protocol6was used to analyze the disinfectant formulation efficacy with viruses. The EN16777 protocol includes a test method for virucidal activity of chemical disinfectants that form a homogeneous physically stable preparation when diluted with water. The EN14476 protocol7was used to analyze the disinfectant formulation efficacy with viruses. The EN14476 protocol is a quantitative suspension test for the evaluation of virucidal activity of disinfectants.

[0065] Under these EU approved protocols, the inventive Sample D passed every test, including compared to bacteria, fungi, and viruses, sufficiently killing these various microbes.

[0066] Example 3, pH Testing of the Disinfectant Formulation

[0067] During testing of the inventive Samples D and E, the pH (neat) was measured. The pH of the samples listed were taken when the samples were tested for chemical characterization after the samples went through the irradiation process discussed below in Example 5. A pH meter that included an ATC probe calibrated at 4.0, 7.0, and 10.0 was used to measure the pH of each sample. Specifically, three lots of samples of the inventive formulation (that were used in the efficacy testing of Example 3) were found to have pH of 6.47, 6.66, and 6.67.

[0068] Example 4, Residue Profiles of the Disinfectant Formulation transferred to a neutralizing solution to extract the remaining microbials. A plating method is used to enumerate the surviving microbials.4Under the EN1276 protocol, several microorganisms are used to challenge the product. The microorganisms are exposed to the test solution under controlled conditions. Then, the number of viable bacteria is determined and the reduction in viability is calculated.5Under the EN1650 protocol, a disinfectant is diluted at three or more different concentrations. Fungal spores are prepared to create a test suspension. The contact temperature and time are chosen, and an aliquot of the test suspension is contact with the disinfectant accordingly. A neutralized is then used, and the results are analyzed.6Under the EN16777 protocol, the viral suspension is mixed with interfering substances and spread over stainless steel test surfaces. The disinfectant is applied to the test surfaces at a specific temperature and contact time. A neutralizer solution is then used. The neutralizing extract is plated to enumerate the remaining viable microorganisms.7Under the EN14476 protocol, a viral suspension is prepared and used to test the disinfectant samples. After appropriate contact time at a selected temperature, the test products are neutralized. The suspensions are allowed to incubate.

[0069] Residue profile testing was conducted on both the inventive Sample D and a new comparative containing Vesta Sy de SQ disinfectant (Steris, St. Louis, MO, U.S.). Each of the samples was diluted with deionized water. The Sample D was prepared at a 2% use dilution, which contained 2000ppm of active DDAC. The Comparative Vest Syde SQ Sample was prepared at a 1.56% use dilution, containing approximately 1600ppm of DDAC per the products label claims.

[0070] Ceramic tiles were used as the surfaces for residue testing. The ceramic tiles were rinsed and dried prior to testing. A ImL dose of the use dilution was spread over the tile and allowed to dry overnight. Pictures were taken to document the resulting residue. Even with more active content, the Sample D formulation had a more favorable residue profile, showing less residue after the allocated time.

[0071] Example 5, Stability Under Irradiation of the Disinfectant Formulation

[0072] Stability testing of the inventive Sample D was conducted. This analysis was done to analyze stability, specifically of the active ingredient, after irradiation. In this test, Sample D was gamma irradiated with a dose of 53.5 IkGy. A non-irradiated Sample D was simultaneously analyzed. The results are summarized below in Table 4:Table 4. Stability Testing of Sample D.

[0073] The irradiated sample, along with a non-irradiated retain of the same lot were analyzed by titration method to determine the weight percent of active quaternary ammonium chloride in solution. The percent recoveries are based on the average of the results for each formulation. The results were within 2% of the average and are considered to be within the variability of the test method.

[0074] As such, the weight percent of active quaternary ammonium chloride found in the room temperature retain sample was statistically the same as the of active quaternary ammonium chloride determined for the sample that had undergone irradiation.

[0075] Example 6, Ready to Use Formulation

[0076] A ready to use formulation was prepared for Example 6. An example of the production of a ready to use formulation is shown in Table 5 below:

[0077] Table 5. Example formulation of ready to use sample.

[0078] Table 5 shows how the ready to use version would be manufactured from the concentrated product. For the example the formula already described in Table 1, sample D was used. The comparison of the Sample D (concentrate) and the ready to use formulation are shown in Table 6 below:

[0079] Table 6. Comparison of dilutable concentrate and ready to use formulations.

[0080] Table 6 shows the breakdown of the ingredients and their respective weight percentages. This shows the comparison between the dilutable concentrate at its recommended 2% use dilution and the RTU version of the product.

[0081] For additional testing of the ready to use formulation, two sample concentrate formulations A and D (summarized in Table 1) were used to produce several additional samples ready to use formulations shown in Table 7 below:

[0082] Table 7. Ready to use formulation samples.

[0083] Here, the dilutable concentrate formulations A and D were used to create stable and effective ready to use disinfectant formulation samples. For these samples 1 to 8, a sufficient amount of the dilutable concentrate formulation was used to prepare a ready to use dilution with greater than 1,500 ppm of DDAC. The prepared samples 1 to 8 were readily soluble and were mixed with the solvent(s) and / or buffer(s) at a low speed with a stir bar for approximately 3 to 5 minutes at room temperature until the solution was homogenous. For samples 1-8, either Water for Injection (WFI, water that meets the specifications of purity for an injectable drug), Deionized water, or soft water was used.

[0084] The ready to use samples 1 to 8 were sterilized using x-ray irradiation at a max dose of 57.4kGy. The samples were then stored at room temperature and 54°C for 2 weeks before being analyzed to determine the impact of the irradiation dose on the active DDAC after storage at elevated temperature conditions. Analysis of the samples showed 1%or less change in the concentration of DDAC of each of the solutions tested. The result of this testing is summarized in Table 8 below:

[0085] Table 8. Irradiation of ready to use samples.

[0086] The change in DDAC for each of these formulations can be seen after irradiation and storage. The ready to use samples 6 and 4, using isopropyl alcohol as a solvent, performed better than the samples 2 and 8 using N-propyl alcohol. The samples with a smaller amount of solvent (5.00%) performed better than those with more solvent (20.00%). The better performing samples had less overall DDAC loss.

[0087] The terms and expressions that have been employed are used as terms of description and not of limitation, and there is no intention in the use of such terms and expressions of excluding any equivalents of the features shown and described or portions thereof, but it is recognized that various modifications are possible within the scope of the examples of the present disclosure. Thus, it should be understood that although the present disclosure has been specifically disclosed by specific examples and optional features, modification and variation of the concepts herein disclosed may be resorted to by those of ordinary skill in the art, and that such modifications and variations are considered to be within the scope of examples of the present disclosure.

[0088] Additional Examples.

[0089] The following exemplary examples are provided, the numbering of which is not to be construed as designating levels of importance:

[0090] Example 1 includes a formulation for a disinfectant solution useable on hard surfaces, the formulation comprising: an active agent including didecyl dimethyl ammonium chloride (DDAC); and a surfactant including alkyl polyethylene glycol ether; and at least one solvent component; wherein the formulation has a pH of about 6.0 to about 8.5.

[0091] Example 2 can include the formulation of Example 1, wherein the active agent is about 5.00 wt.% to about 20.00 wt.% of the formulation.

[0092] Example 3 can include the formulation of any of Examples 1-2, wherein the active agent is about 8.00 wt.% to about 15.00 wt.% of the formulation.

[0093] Example 4 can include the formulation of any of Examples 1-3, wherein the surfactant is about 0.05 wt.% to about 2.00 wt.% of the formulation.

[0094] Example 5 can include the formulation of any of Examples 1-4, wherein the surfactant is about 0.50 wt.% to about 1.40 wt.% of the formulation.

[0095] Example 6 can include the formulation of any of Examples 1-5, wherein the at least one solvent comprises deionized water, isopropyl alcohol, or a combination thereof.

[0096] Example 7 can include the formulation of any of Examples 1-6, wherein the at least one solvent component comprises one or more solvents adding up to about 95.00 wt.% of the formulation.

[0097] Example 8 can include the formulation of any of Examples 1-6, wherein the at least one solvent component comprises isopropyl alcohol being about 5.00 to about 6.00 wt.% of the formulation.

[0098] Example 9 can include the formulation of any of Examples 1-6, wherein the at least one solvent component comprises deionized water being about 80.00 to about 86.00 wt.% of the formulation.

[0099] Example 10 can include the formulation of any of Examples 1-9, further comprising an organic acid.

[0100] Example 11 can include the formulation of any of Examples 1-10, wherein the organic acid comprises citric acid, lactic acid, acetic acid, formic acid, oxalic acid, uric acid, malic acid, tartaric acid, or combinations thereof.

[0101] Example 12 can include the formulation of any of Examples 1-10, wherein the organic acid comprises about 0.0001 wt.% or more of the formulation.

[0102] Example 13 can include the formulation of any of Examples 1-12, further comprising a base.

[0103] Example 14 can include the formulation of any of Examples 1-13, wherein the base comprises potassium hydroxide or sodium hydroxide.

[0104] Example 15 can include the formulation of any of Examples 1-14, wherein the base comprises about 0.0001 wt.% or more of the formulation.

[0105] Example 16 can include the formulation of any of Examples 1-15, wherein the pH of the formulation is about 6.5 to about 7.9.

[0106] Example 17 can include the formulation of any of Examples 1-16, wherein the pH of the formulation is about 7.0 to about 7.8.

[0107] Example 18 can include the formulation of any of Examples 1-17, wherein following application of the formulation in a diluted form, there is little to no visual presence of formulation residue after the product has dried.

[0108] Example 19 can include the formulation of any of Examples 1-18, wherein the formulation kills a sufficient amount of microbials so as to pass according to an AO AC UDT protocol.

[0109] Example 20 can include the formulation of any of Examples 1-19, wherein the formulation kills a sufficient amount of microbials so as to pass according to an ASTM El 053 protocol.

[0110] Example 21 can include the formulation of any of Examples 1-20, wherein the formulation kills a sufficient amount of microbials so as to pass according to EN13697, EN1276, EN1650, EN16777, and EN14476 protocols.

[0111] Example 22 can include the formulation of any of Examples 1-21, wherein the formulation has a 98.0 wt.% or better recovery of the active agent when gamma irradiated with a dose of 50 kGy or more.

[0112] Example 23 include a method of making the formulation of any one of Examples 1-22 comprising mixing together the active agent, the surfactant, and the at least one solvent.

[0113] Example 24 include a method of disinfecting a surface comprising applying the formulation of any one of Examples 1-22 to the surface.

[0114] Example 25 includes a formulation for a disinfectant, the formulation comprising: didecyl dimethyl ammonium chloride (DDAC) in an amount of about 10.00 wt.% of the formulation; alkyl polyethylene glycol ether in an amount of about 1.00 wt.% of the formulation; and isopropyl alcohol in an amount of about 5.50 wt.% of the formulation.

[0115] Example 26 can include the formulation of Example 25, further comprising citric acid in an amount of about 0.0001 wt.% or more of the formulation.

[0116] Example 27 can include the formulation of any of Examples 25-26, further comprising potassium hydroxide in an amount of about 0.0001 wt.% or more of the formulation.

[0117] Example 28 can include the formulation of any of Examples 25-27, further comprising deionized water.

[0118] Example 29 includes a method of making the formulation of any one of Examples 25-28 comprising mixing together the didecyl dimethyl ammonium chloride, the alkyl polyethylene glycol ether, and the isopropyl alcohol.

[0119] Example 30 includes a method of disinfecting a surface comprising applying the formulation of any one of Example 25-29 to the surface.

Claims

CLAIMSWhat is claimed is:

1. A formulation for a disinfectant solution useable on hard surfaces, the formulation comprising: an active agent including didecyl dimethyl ammonium chloride (DDAC); a surfactant including alkyl polyethylene glycol ether; and at least one solvent component, wherein the formulation has a pH of 6.0 to 8.5.

2. The formulation of claim 1, wherein the active agent is about 5.00 wt.% to about 20.00 wt.% of the formulation.

3. The formulation of claim 1, wherein the active agent is about 8.00 wt.% to about 15.00 wt.% of the formulation.

4. The formulation of claim 1, wherein the surfactant is about 0.05 wt.% to about 2.00 wt.% of the formulation.

5. The formulation of claim 4, wherein the surfactant is about 0.50 wt.% to about 1.40 wt.% of the formulation.

6. The formulation of claim 1, wherein the at least one solvent component comprises deionized water, isopropyl alcohol, or a combination thereof.

7. The formulation of claim 1, wherein the at least one solvent component comprises one or more solvents adding up to about 95.00 wt.% of the formulation.

8. The formulation of claim 1, wherein the at least one solvent component comprises isopropyl alcohol being about 5.00 to about 6.00 wt.% of the formulation.

9. The formulation of claim 1, wherein the at least one solvent component comprises deionized water being about 80.00 to about 86.00 wt.% of the formulation.

10. The formulation of claim 1, further comprising an organic acid being about 0.0001 wt.% or more of the formulation.

11. The formulation of claim 1, further comprising a base being about 0.0001 wt.% or more of the formulation.

12. The formulation of claim 1, wherein following application of the formulation in a diluted form, there is little to no visual residue of the formulation after the formulation dries.

13. The formulation of claim 1, wherein the formulation kills a sufficient amount of microbials so as to pass according to an AO AC UDT protocol.

14. The formulation of claim 1, wherein the formulation kills a sufficient amount of microbials so as to pass according to an ASTM E1053 protocol.

15. The formulation of claim 1, wherein the formulation kills a sufficient amount of microbials so as to pass according to EN13697, EN1276, EN1650, EN16777, and EN14476 protocols.

16. The formulation of claim 1, wherein the formulation has a 98.0 wt.% or better recovery of the active agent when gamma irradiated with a dose of 50 kGy or more.

17. A formulation for a ready to use disinfectant, the formulation comprising: didecyl dimethyl ammonium chloride (DDAC) in an amount of about 0.15 wt.% to about 0.25 wt.% of the formulation; alkyl polyethylene glycol ether in an amount of about 0.01 wt.% to about 0.03 wt.% of the formulation; and isopropyl alcohol in an amount of about 10.0 wt.% to about 10.5 wt.% of the formulation.

18. The formulation of claim 17, further comprising citric acid in an amount of about 0.001 wt.% to about 0.02 wt.% of the formulation.

19. The formulation of claim 17, further comprising potassium hydroxide in an amount of about 0.001 wt.% to about 0.05 wt.% of the formulation.

20. The formulation of claim 17, further comprising water in an amount of about 85.0 wt.% to about 95.0 wt.% of the formulation.

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