Cosmetic preparation containing PQQ disodium salt and its preparation method and application

Abstract

The present invention relates to the field of cosmetics, and in particular to cosmetic preparations containing PQQ disodium salt, as well as their preparation and use. The cosmetic preparations provided herein include PQQ-2Na, a humectant, an emulsifier, and water; the humectant is glycerol and / or butylene glycol; and the emulsifier is at least one of EMULPHARMA 1000, potassium cetearyl phosphate, polyglycerol-6 distearate, or hydrogenated lecithin. The preparations provided herein screen and optimize the excipients used in conjunction with PQQ-2Na. The resulting product not only ensures the stability of PQQ-2Na but also achieves excellent skincare benefits, such as enhanced moisturizing, hydration, antioxidant properties, and / or skin condition improvement.

Description

Technical Field

[0001] The present invention relates to the technical field of cosmetics, and in particular to a cosmetic preparation containing PQQ disodium salt, and a preparation method and application thereof. Background Art

[0002] Pyrroloquinoline quinone (PQQ), a novel oxidoreductase coenzyme, was discovered in methylotrophic bacteria and subsequently confirmed to be widely present in Gram-negative bacteria, higher plants and animals. It possesses a variety of physiological functions, including antioxidant and anti-inflammatory properties, promoting cellular metabolism, and protecting mitochondrial function. These properties make PQQ an ideal skincare ingredient in cosmetics. Its antioxidant capacity effectively protects skin cells from free radical damage, delaying skin aging and reducing the appearance of wrinkles. Its anti-inflammatory properties help alleviate inflammation and soothe sensitive skin. Its cellular metabolism-boosting properties accelerate skin turnover, improve dullness, brighten the complexion, and create a healthy, radiant complexion. Therefore, PQQ holds broad application prospects in a variety of cosmetics, including anti-aging, whitening, and repair products.

[0003] However, the stability of PQQ has long been a major challenge for cosmetics developers. PQQ disodium salt (hereinafter referred to as PQQ) has a high redox potential and is highly reactive, readily reacting with amino acids to form IPQ. Furthermore, during actual formulation development, PQQ disodium salt has been found to readily react with certain emulsifiers, oils, and moisturizers, affecting PQQ's activity and reducing its efficacy.

[0004] The difficulty in ensuring PQQ's stability presents numerous challenges for cosmetics development. To ensure consistent efficacy throughout the product's shelf life, developers are forced to reduce the amount of PQQ added, which in turn limits its effectiveness. Furthermore, improving PQQ's stability requires rigorous screening of cosmetic excipients, which not only increases R&D costs but also potentially compromises the effectiveness of these excipients. Furthermore, PQQ's instability complicates product quality control, leading to potential variations in efficacy between batches, impacting consumer experience and market reputation.

[0005] It can be seen that PQQ-related skin care products are still difficult to develop and face the risk of instability during the shelf life. It is still difficult to develop a PQQ emulsified formula that meets both high stability and high efficacy. Summary of the Invention

[0006] In view of this, the technical problem to be solved by the present invention is to provide a highly stable cosmetic preparation containing PQQ disodium salt, and a preparation method and application thereof.

[0007] The cosmetic preparation containing PQQ disodium salt includes PQQ-2Na, a moisturizer, an emulsifier and water;

[0008] The moisturizing agent is glycerin and / or butylene glycol;

[0009] The emulsifier is at least one of EMULPHARMA 1000, potassium cetearyl phosphate, polyglyceryl-6 distearate or hydrogenated lecithin.

[0010] The cosmetic preparation of the present invention further comprises oil, thickener and / or pH adjuster;

[0011] The pH regulator is sodium hydroxide and / or aminomethyl propanol;

[0012] The thickener is at least one of acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, ammonium acryloyldimethyltaurate / VP copolymer, or hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer;

[0013] The oil is at least one of caprylic and capric triglyceride, polydimethylsiloxane or isononyl isononanoate.

[0014] The cosmetic preparation provided by the present invention utilizes rationally selected excipients, thereby reducing the loss of PQQ disodium salt. At a 0.02% addition level, the stability of PQQ disodium salt in the cosmetic is ensured. This ensures that the physiological activities of PQQ disodium salt are fully exerted, such as its antioxidant properties. Furthermore, due to the rational selection and appropriate content of each component, the resulting cosmetic preparation exhibits excellent moisturizing, hydrating, and skin-improving effects.

[0015] In an embodiment of the present invention, the moisturizing agent is one type, which is glycerin or butylene glycol, or the moisturizing agent is two types, which is a combination of glycerin and butylene glycol. Specifically, the mass ratio of glycerin to butylene glycol is (1-5):(1-5), for example, 1:1, 2:1, 3:1, 4:1, 5:1, 1:2, 1:3, 1:4, or 1:5.

[0016] In embodiments of the present invention, the thickener is one type, which is an acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, ammonium acryloyldimethyl taurate / VP copolymer, or hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer. There are two types of thickeners, which are acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer + ammonium acryloyldimethyl taurate / VP copolymer, or acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer + hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, or ammonium acryloyldimethyl taurate / VP copolymer + hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer. There are three types of thickeners, which are acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer + ammonium acryloyldimethyl taurate / VP copolymer + hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer. The present invention does not limit the ratio of the various components in the thickener. As a feasible example, when three thickeners are present, the mass ratio of acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer + ammonium acryloyldimethyl taurate / VP copolymer + hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer is (0.05-0.15): (0.2-0.4): (0.3-0.5). In a specific embodiment, the mass ratio is 0.1:0.3:0.4.

[0017] In an embodiment of the present invention, the emulsifier is one, which is EMULPHARMA 1000, potassium cetearyl phosphate, polyglyceryl-6 distearate or hydrogenated lecithin. The emulsifier is two, which is EMULPHARMA 1000 + potassium cetearyl phosphate, or EMULPHARMA 1000 + polyglyceryl-6 distearate, or EMULPHARMA 1000 + hydrogenated lecithin, or potassium cetearyl phosphate + polyglyceryl-6 distearate, or potassium cetearyl phosphate + hydrogenated lecithin, or polyglyceryl-6 distearate + hydrogenated lecithin. There are two types of emulsifiers, namely EMULPHARMA 1000 + potassium cetearyl phosphate + polyglyceryl-6 distearate, or EMULPHARMA 1000 + potassium cetearyl phosphate + hydrogenated lecithin, or EMULPHARMA 1000 + polyglyceryl-6 distearate + hydrogenated lecithin, or potassium cetearyl phosphate + polyglyceryl-6 distearate + hydrogenated lecithin. There are four types of emulsifiers, namely EMULPHARMA 1000 + potassium cetearyl phosphate + polyglyceryl-6 distearate + hydrogenated lecithin. The present invention does not limit the ratio of the components in the emulsifier. As a feasible example, when there are four emulsifiers, the mass ratio of EMULPHARMA 1000 + potassium cetearyl phosphate + polyglyceryl-6 distearate + hydrogenated lecithin is (0.4-0.6): (0.4-0.6): (0.4-0.6). In a specific embodiment, the mass ratio is 0.5:0.5:0.5:0.5.

[0018] In an embodiment of the present invention, the oil is one type, which is caprylic capric triglyceride, polydimethylsiloxane, or isononyl isononanoate. The oil is two types, which are caprylic capric triglyceride + polydimethylsiloxane, or caprylic capric triglyceride + isononyl isononanoate, or polydimethylsiloxane + isononyl isononanoate. The oil is three types, which are caprylic capric triglyceride + polydimethylsiloxane + isononyl isononanoate. The present invention does not limit the ratio of the components in the oil. As a feasible example, when the oil is three types, the mass ratio of caprylic capric triglyceride + polydimethylsiloxane + isononyl isononanoate is (4-6): (2-3): (2-3). In a specific embodiment, the mass ratio is 5:2.5:2.5.

[0019] In an embodiment of the present invention, the pH adjuster is a single agent, which is sodium hydroxide or aminomethyl propanol. The pH adjusters are two agents, which are sodium hydroxide and aminomethyl propanol. Specifically, the mass ratio of sodium hydroxide to aminomethyl propanol is (0.01-0.03):(0.05-0.07). In a specific embodiment, the mass ratio is 0.02:0.06.

[0020] In the present invention, the cosmetic preparation may be in the form of an aqueous solution, for example, a toner, a toner, a moisturizing lotion, a serum, a makeup lotion, or an aftershave lotion. Alternatively, if ingredients such as oils are added to the cosmetic preparation, the cosmetic preparation may be in the form of a face cream, lotion, body cream, hand cream, eye cream, neck cream, day cream, night cream, sleeping mask, or massage cream. The present invention is not limited thereto.

[0021] In the cosmetic preparations of the present invention, one or more of each type of excipient may be selected, and the present invention is not limited thereto. The examples describe cases where one excipient of each type is selected, and also describe cases where more than one excipient of each type is selected. For example, the following examples describe cases where one excipient of each type is selected:

[0022] The cosmetic formulation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, caprylic / capric triglyceride, and sodium hydroxide.

[0023] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, caprylic / capric triglyceride, and aminomethyl propanol.

[0024] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, polydimethylsiloxane, and sodium hydroxide.

[0025] Alternatively, the cosmetic formulation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, polydimethylsiloxane, and aminomethyl propanol.

[0026] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, isononyl isononanoate, and sodium hydroxide.

[0027] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, isononyl isononanoate, and aminomethyl propanol.

[0028] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.

[0029] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethyl propanol.

[0030] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.

[0031] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and aminomethyl propanol.

[0032] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.

[0033] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol.

[0034] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.

[0035] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethyl propanol.

[0036] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.

[0037] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethyl propanol.

[0038] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.

[0039] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethyl propanol.

[0040] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.

[0041] Alternatively, the cosmetic formulation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethyl propanol.

[0042] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.

[0043] Alternatively, the cosmetic formulation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, dimethicone, and aminomethyl propanol.

[0044] Alternatively, the cosmetic preparation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.

[0045] Alternatively, the cosmetic formulation includes glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, isononyl isononanoate, and aminomethyl propanol.

[0046] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, caprylic / capric triglyceride, and sodium hydroxide.

[0047] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, caprylic / capric triglyceride, and aminomethyl propanol.

[0048] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, polydimethylsiloxane, and sodium hydroxide.

[0049] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, polydimethylsiloxane, and aminomethyl propanol.

[0050] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, isononyl isononanoate, and sodium hydroxide.

[0051] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, isononyl isononanoate, and aminomethyl propanol.

[0052] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.

[0053] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethyl propanol.

[0054] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.

[0055] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, dimethicone, and aminomethyl propanol.

[0056] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.

[0057] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol.

[0058] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.

[0059] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethyl propanol.

[0060] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.

[0061] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, dimethicone, and aminomethyl propanol.

[0062] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.

[0063] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethyl propanol.

[0064] Alternatively, the cosmetic formulation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.

[0065] Alternatively, the cosmetic formulation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethyl propanol.

[0066] Alternatively, the cosmetic preparation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.

[0067] Alternatively, the cosmetic formulation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, dimethicone, aminomethyl propanol.

[0068] Alternatively, the cosmetic formulation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.

[0069] Alternatively, the cosmetic formulation includes glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, isononyl isononanoate, aminomethyl propanol.

[0070] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, caprylic / capric triglyceride, and sodium hydroxide.

[0071] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, caprylic / capric triglyceride, and aminomethyl propanol.

[0072] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, polydimethylsiloxane, and sodium hydroxide.

[0073] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, polydimethylsiloxane, and aminomethyl propanol.

[0074] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, isononyl isononanoate, and sodium hydroxide.

[0075] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, potassium cetearyl phosphate, isononyl isononanoate, and aminomethyl propanol.

[0076] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.

[0077] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethyl propanol.

[0078] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.

[0079] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and aminomethyl propanol.

[0080] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.

[0081] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol.

[0082] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.

[0083] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethyl propanol.

[0084] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.

[0085] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethyl propanol.

[0086] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.

[0087] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethyl propanol.

[0088] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.

[0089] Alternatively, the cosmetic formulation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethyl propanol.

[0090] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.

[0091] Alternatively, the cosmetic formulation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, dimethicone, and aminomethyl propanol.

[0092] Alternatively, the cosmetic preparation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.

[0093] Alternatively, the cosmetic formulation includes butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA, isononyl isononanoate, and aminomethyl propanol.

[0094] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, caprylic capric triglyceride, and sodium hydroxide.

[0095] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, caprylic capric triglyceride, and aminomethyl propanol.

[0096] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, polydimethylsiloxane, and sodium hydroxide.

[0097] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, polydimethylsiloxane, and aminomethyl propanol.

[0098] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, isononyl isononanoate, and sodium hydroxide.

[0099] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, potassium cetearyl phosphate, isononyl isononanoate, and aminomethyl propanol.

[0100] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.

[0101] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethyl propanol.

[0102] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.

[0103] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, dimethicone, and aminomethyl propanol.

[0104] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.

[0105] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol.

[0106] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.

[0107] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethyl propanol.

[0108] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.

[0109] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethyl propanol.

[0110] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.

[0111] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethyl propanol.

[0112] Alternatively, the cosmetic formulation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.

[0113] Alternatively, the cosmetic formulation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethyl propanol.

[0114] Alternatively, the cosmetic preparation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.

[0115] Alternatively, the cosmetic formulation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, dimethicone, aminomethyl propanol.

[0116] Alternatively, the cosmetic formulation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.

[0117] Alternatively, the cosmetic formulation includes butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, isononyl isononanoate, aminomethyl propanol.

[0118] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, potassium cetearyl phosphate, caprylic capric triglyceride, and sodium hydroxide.

[0119] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, potassium cetearyl phosphate, caprylic capric triglyceride, and aminomethyl propanol.

[0120] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, potassium cetearyl phosphate, dimethicone, and sodium hydroxide.

[0121] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, potassium cetearyl phosphate, dimethicone, and aminomethyl propanol.

[0122] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, potassium cetearyl phosphate, isononyl isononanoate, and sodium hydroxide.

[0123] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, potassium cetearyl phosphate, isononyl isononanoate, and aminomethyl propanol.

[0124] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, caprylic capric triglyceride, and sodium hydroxide.

[0125] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, caprylic capric triglyceride, and aminomethyl propanol.

[0126] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, dimethicone, and sodium hydroxide.

[0127] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, dimethicone, and aminomethyl propanol.

[0128] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.

[0129] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol.

[0130] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.

[0131] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethyl propanol.

[0132] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.

[0133] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, dimethicone, and aminomethyl propanol.

[0134] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.

[0135] Alternatively, the cosmetic preparation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethyl propanol.

[0136] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, caprylic capric triglyceride, and sodium hydroxide.

[0137] Alternatively, the cosmetic formulation includes butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, caprylic / capric triglyceride, aminomethyl propanol.

[0138] Alternatively, the cosmetic formulation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, dimethicone, sodium hydroxide.

[0139] Alternatively, the cosmetic formulation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, dimethicone, aminomethyl propanol.

[0140] Alternatively, the cosmetic formulation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, isononyl isononanoate, sodium hydroxide.

[0141] Alternatively, the cosmetic formulation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, isononyl isononanoate, aminomethyl propanol.

[0142] In the present invention, the mass fraction of each component in the cosmetic preparation is not limited and can be present at a concentration suitable for use, or 2 to 100 times the concentration suitable for use. For example, it can be 2 times, 5 times, 10 times, 20 times, 25 times, 50 times, or 100 times the concentration used.

[0143] In the embodiment of the present invention, the mass fractions of the components in the cosmetic are: PQQ-2Na 0.01% to 0.03%, moisturizer 3% to 7%, thickener 0.2% to 0.8%, emulsifier 1% to 3%, oil 8% to 12%, pH adjuster 0.02% to 0.08%, and the balance is water.

[0144] Specifically, within the aforementioned concentration range and by selecting the aforementioned excipients, a stable cosmetic formulation with excellent activity can be obtained. As a feasibility example, the mass fractions of the components in the cosmetic are: PQQ-2Na 0.02%, humectant 5%, thickener 0.2%-0.8%, emulsifier 2%, oil 10%, pH adjuster 0.02%-0.08%, and the balance water.

[0145] In some embodiments, the cosmetic comprises PQQ-2Na, glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, EMULPHARMA 1000, caprylic / capric triglyceride, and sodium hydroxide; in this embodiment, the cosmetic comprises the following components by mass: 0.02% PQQ-2Na, 5% glycerin, 0.2% acrylates / C10-30 alkyl acrylate crosspolymer, 2% EMULPHARMA 1000, 10% caprylic / capric triglyceride, and 0.04% sodium hydroxide, with the remainder being water.

[0146] In some embodiments, the cosmetic comprises PQQ-2Na, butylene glycol, ammonium acryloyldimethyl taurate / VP copolymer, potassium cetearyl phosphate, dimethicone, and aminomethyl propanol; in this embodiment, the cosmetic comprises the following components by mass: 0.02% PQQ-2Na, 5% butylene glycol, 0.8% ammonium acryloyldimethyl taurate / VP copolymer, 2% potassium cetearyl phosphate, 10% dimethicone, and 0.02% aminomethyl propanol, with the balance being water;

[0147] In some embodiments, the cosmetic comprises PQQ-2Na, glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol; in this embodiment, the cosmetic comprises the following components by mass: 0.02% PQQ-2Na, 5% glycerin, 0.8% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 2% polyglyceryl-6 distearate, and 10% isononyl isononanoate, with the remainder being water;

[0148] In some embodiments, the cosmetic comprises PQQ-2Na, glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, caprylic capric triglyceride, hydrogenated lecithin, and sodium hydroxide. In this embodiment, the cosmetic comprises the following components by mass: 0.02% PQQ-2Na, 5% glycerin, 0.2% acrylates / C10-30 alkyl acrylate crosspolymer, 10% caprylic capric triglyceride, 2% hydrogenated lecithin, and 0.04% sodium hydroxide, with the remainder being water.

[0149] In some embodiments, the cosmetic comprises PQQ-2Na, glycerin, butylene glycol, acrylates / C10-30 alkyl acrylate crosspolymer, ammonium acryloyldimethyl taurate / VP copolymer, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA 1000, potassium cetearyl phosphate, polyglyceryl-6 distearate, hydrogenated lecithin, caprylic / capric triglyceride, dimethicone, isononyl isononanoate, sodium hydroxide, and aminomethyl propanol. In this embodiment, the cosmetic includes the following components by mass fraction: 0.02% PQQ-2Na, 2% glycerin, 3% butylene glycol, 0.1% acrylates / C10-30 alkyl acrylate crosspolymer, 0.3% ammonium acryloyldimethyltaurate / VP copolymer, 0.4% hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, 0.5% EMULPHARMA 1000, 0.5% potassium cetearyl phosphate, 0.5% polyglyceryl-6 distearate, 0.5% hydrogenated lecithin, 5% caprylic / capric triglyceride, 2.5% polydimethylsiloxane, 2.5% isononyl isononanoate, 0.02% sodium hydroxide and 0.06% aminomethyl propanol, and the balance is water.

[0150] Furthermore, the present invention also provides a method for preparing the cosmetic preparation, comprising:

[0151] Mix the humectant, thickener and water and heat to obtain phase A;

[0152] Mix the emulsifier and oil and heat to obtain phase B;

[0153] Phase B is added to phase A and homogenized, and then PQQ-2Na and a pH adjuster are added while cooling, and stirred until uniformly dispersed to prepare the cosmetic preparation.

[0154] In a specific embodiment, the heating temperature of phase A is 80-85° C. The heating temperature of phase B is 80-85° C. After phases A and B are homogenized, the temperature is lowered to 45° C.

[0155] In a specific embodiment, the homogenization conditions include a rotation speed of 3000 rps for 5 minutes.

[0156] Furthermore, the present invention also provides the use of the cosmetic preparation as described above or the cosmetic preparation prepared by the preparation method as described above in the preparation of products for anti-oxidation, hydration, moisturizing and / or improving skin condition.

[0157] In the present invention, the improvement of skin condition includes improving skin gloss, improving skin elasticity and / or improving skin firmness.

[0158] Furthermore, the present invention also provides a method for anti-oxidation, hydration, moisturizing and / or improving skin condition, which comprises applying the cosmetic preparation as described above or the cosmetic preparation prepared by the preparation method as described above to the skin surface.

[0159] In the present invention, the manner of applying includes but is not limited to smearing, wiping, patting, massaging, spotting, patting, spreading evenly, thick application or thin application.

[0160] In the present invention, the skin surface includes but is not limited to facial skin, neck skin, hand skin, arm skin, leg skin, foot skin, chest skin, abdominal skin, back skin, shoulder skin, buttocks skin, skin around the eyes or skin around the lips.

[0161] In the cosmetic preparation provided by the present invention, the excipients for use with PQQ-2Na are screened and optimized. The resulting product not only ensures the stability of PQQ-2Na but also achieves excellent skin care effects, for example, enhancing moisturizing, hydrating, anti-oxidation, and / or improving skin condition. DETAILED DESCRIPTION

[0162] The present invention provides cosmetic formulations containing PQQ disodium salt, as well as methods for their preparation and use. Those skilled in the art can draw upon the disclosure herein and appropriately modify process parameters to achieve the desired results. It is particularly important to note that all similar substitutions and modifications readily apparent to those skilled in the art are considered encompassed by the present invention. The methods and uses of the present invention have been described using preferred embodiments. It is readily apparent to those skilled in the art that modifications, variations, and combinations thereof, without departing from the disclosure, spirit, and scope of the present invention, can be made to implement and apply the present technology.

[0163] The numerical ranges and parameters involved in this disclosure are presented as precisely as possible in the specific examples. However, any numerical value inherently and inevitably contains standard deviations resulting from individual testing methods. Therefore, unless otherwise expressly stated, it should be understood that all numerical ranges or specific data used in this disclosure are subject to reasonable deviation within a certain range, for example, within ±10%, ±5%, ±1%, or ±0.5%.

[0164] The Examples and Comparative Examples of the present invention describe some examples. These examples illustrate certain implementations of the present invention. However, this does not mean that the effects of the present invention are achieved only in these examples. In fact, good effects can be achieved at any concentration of the components between the two endpoints shown in the Examples.

[0165] Each excipient in the cosmetic formulations provided by this invention has undergone rigorous screening. Preliminary experiments have identified suitable components from a large pool of excipients. For example, for moisturizers, the present invention screened 25 moisturizers (such as glycerin, butylene glycol, dipropylene glycol, 1,3-propanediol, methylpropylene glycol, polyethylene glycol-8, glycereth-26, propylene glycol, panthenol, and hydroxyethyl urea) and found that glycerin and butylene glycol can coexist with PQQ, while the degradation rate of PQQ-2Na is less than 7%. However, other moisturizers can cause significant degradation of PQQ. Similarly, the present invention also screened suitable components from 20 thickeners, 30 emulsifiers, 25 oils, and 6 pH adjusters. Excluded thickeners due to incompatibility with PQQ and resulting in product color change include, but are not limited to, ammonium acryloyldimethyltaurate / beheneth-25 methacrylate crosspolymer, xanthan gum, and sclerotium gum. Excluded emulsifiers include, but are not limited to, MONTANOV L, hydrogenated lecithin, Olivem® 1000, sodium stearoyl glutamate, ResPharma, sucrose stearate, and GLUCAMATES SE-20. Excluded oils include, but are not limited to, olive oil, cetearyl alcohol, behenyl alcohol, shea butter, and isohexadecane. Excluded pH adjusters include, but are not limited to, arginine and triethanolamine. These excluded excipients can cause a PQQ-2Na degradation rate exceeding 10%, and are not further detailed in the specific examples.

[0166] It should be understood that, in different embodiments of the present invention, the order of step numbers does not represent the priority of execution. Some or all steps may be implemented in parallel or in any order. The specific execution process should be determined based on functional logic and should not be considered as a limitation on the implementation methods of this application.

[0167] The test materials used in the present invention are all common commercial products and can be purchased on the market. The present invention is further described below with reference to the following examples:

[0168] Example

[0169] 1. Examples and Comparative Examples

[0170] In Examples 1 to 4, the polyols, thickeners, emulsifiers, oils, and pH adjusters are different. In Examples 5 and 6, the formula modules are compound raw materials. The purpose is to verify the effect of different raw materials on stability after compounding. The formulas of Comparative Examples 1 to 4 are based on Example 1, but the polyols, thickeners, emulsifiers, and oils are replaced respectively. The specific formulas are shown in Table 1:

[0171] Table 1 Recipe

[0172]

[0173] 1.2 Reagents

[0174] EMULPHARMA 1000 comes from Shanghai Yiheng Chemical, and MONTANOV L comes from SEPPIC.

[0175] 1.3 Preparation method

[0176] Mix the moisturizer, thickener and water, and heat to 80-85°C to obtain phase A; mix the emulsifier and oil, and heat to 80-85°C to obtain phase B; add phase B to phase A and homogenize for 5 minutes to obtain a uniform material, cool to 45°C, add PQQ and pH adjuster, stir until uniformly dispersed, degas, cool and discharge to obtain the finished cream.

[0177] 2. Stability investigation

[0178] Examples 1-6 and Comparative Examples 1-4 were stored at 25°C, 4°C, 40°C, and 48°C for 4 weeks, and the color and pH value of each sample at the initial state, 2 weeks, and 4 weeks were observed. The results are shown in Table 2-1 and Table 2-2.

[0179] 2.1 PQQ disodium salt loss rate detection

[0180] Detection method

[0181] 2.1.1 Principle

[0182] PQQ disodium salt was dissolved, separated by reverse-phase high performance liquid chromatography, detected by ultraviolet detector, and quantified by standard curve method.

[0183] 2.2 Reagents and Materials

[0184] Unless otherwise stated, all reagents used in this method (e.g., dipotassium hydrogen phosphate trihydrate, tetrabutylammonium bromide, phosphoric acid) were of analytical grade.

[0185] The water used was Grade 1 water as specified in GB / T 6682-2008 Specifications and test methods for water used in analytical laboratories.

[0186] Acetonitrile: chromatographic grade.

[0187] PQQ disodium salt standard: purity ≥97.0%.

[0188] Aqueous phase microporous membrane: 0.22 μm.

[0189] 10 mmol / L potassium hydrogen phosphate (K2HPO4)-15 mmol / L tetrabutylammonium bromide (pH 7.4) mixed solution: Weigh 2.28 g of K2HPO4 trihydrate and 4.84 g of tetrabutylammonium bromide into a beaker. Add 800 mL of water and sonicate to dissolve. Adjust the pH to 7.4 with phosphoric acid. Transfer the mixture to a 1000 mL volumetric flask, ditto the volume with water, and shake well. Vacuum filter through a 0.22 μm aqueous microporous membrane, then sonicate until free of bubbles.

[0190] Acetonitrile-water solution (volume ratio 1:3): Measure 250 mL of acetonitrile and 750 mL of water respectively, add them to the reagent bottle, and mix well.

[0191] 2.3 Instruments and Equipment

[0192] High performance liquid chromatography, equipped with UV detector and autosampler.

[0193] Electronic balance: sensitivity is 0.01 mg.

[0194] 2.4 Analysis steps

[0195] 2.4.1 Preparation of Standard Solutions Weigh 40 mg (accurate to 0.01 mg) of PQQ disodium salt standard into a 100 mL volumetric flask. Dissolve in acetonitrile-water solution and dilute to the mark. Shake well to obtain a 0.4 mg / mL stock solution of PQQ disodium salt standard. Prepare a series of PQQ disodium salt standard solutions with concentrations of 0.04 mg / mL, 0.08 mg / mL, 0.12 mg / mL, 0.16 mg / mL, 0.20 mg / mL, and 0.24 mg / mL from this solution.

[0196] 2.4.2 Sample Preparation Weigh 20 mg (accurate to 0.01 mg) of each sample from Examples 1-6 and Comparative Examples 1-4 into a 50 mL volumetric flask. Dissolve the sample in acetonitrile and dilute to the mark with aqueous acetonitrile solution. Shake well. Then, accurately pipette 5.0 mL of the above solution into a 10 mL volumetric flask, dilute to the mark with aqueous acetonitrile solution, shake well, and filter the filtrate through a 0.22 μm aqueous microporous filter membrane under vacuum for determination.

[0197] 2.4.3 Liquid chromatography reference conditions

[0198] Chromatographic column: PFchrom EP C18 88031205-4625 (4.6 mm × 250 mm, 5 μm, 120A) or chromatographic column with equivalent performance.

[0199] 2.4.4 Determination

[0200] Under the specified chromatographic conditions, 20 μL of each standard solution and sample solution were injected into a liquid chromatograph for chromatographic analysis. The peak area of ​​PQQ disodium salt in the resulting chromatograms for each standard solution and sample solution was recorded. A standard curve was plotted with the peak area of ​​PQQ disodium salt in the standard solution as the Y-axis and the corresponding standard solution concentration as the X-axis to obtain the PQQ disodium salt standard curve. The concentration of PQQ disodium salt in the sample solution was calculated from the standard curve based on the peak area of ​​PQQ disodium salt in the sample solution chromatogram.

[0201] 2.5 Result calculation

[0202] 2.5.1 Calculation of PQQ disodium salt content

[0203] The content of PQQ disodium salt in the sample is expressed as its mass fraction W1, and the value is expressed as percentage (%), calculated according to formula (1):

[0204]

[0205] (1) Where:

[0206] C is the concentration of pyrroloquinoline quinone disodium salt in the sample solution obtained from the standard curve, in milligrams per milliliter (mg / mL);

[0207] V —— dilution volume of sample, in milliliters (mL);

[0208] f——Purity of PQQ disodium salt standard;

[0209] m —— the mass of the sample, in milligrams (mg);

[0210] W2——The mass fraction of water in the sample, expressed as a percentage (%).

[0211] The arithmetic mean of the parallel determination results is taken as the determination result, and the result is expressed to two decimal places.

[0212] 2.5.2 Calculation of PQQ disodium salt loss rate

[0213] PQQ disodium salt loss rate = (PQQ disodium salt content in initial sample - PQQ disodium salt content in stability sample) / PQQ disodium salt content in initial sample × 100%

[0214] 2.6 Precision

[0215] The relative standard deviation of two independent measurements obtained under repeatability conditions was no more than 2.0%.

[0216] 2.7 Stability test results

[0217] Table 2-1 Stability test results of Examples 1 to 6

[0218]

[0219] Table 2-2 Stability test results of Comparative Examples 1 to 4

[0220]

[0221] The data in Tables 2-1 and 2-2 demonstrate that the four-week stability appearance and viscosity of Examples 1-6 met requirements, and the loss rate of pqq-2Na was less than 10%, which is within the loss range of relatively active actives in the industry. All of these ingredients passed the stability test. This indicates that the following ingredients in the cream formula are well compatible with pqq-2Na, allowing for a stable formulation: humectants (glycerin and butylene glycol); thickeners (acrylates / C10-30 alkyl acrylate crosspolymer, ammonium acryloyldimethyltaurate / VP copolymer, or hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer); emulsifiers (EMULPHARMA 1000, potassium cetearyl phosphate, polyglyceryl-6 distearate, or hydrogenated lecithin); oils (caprylic / capric triglyceride, dimethicone, or isononyl isononanoate); and pH adjusters (sodium hydroxide and aminomethyl propanol).

[0222] Comparative Examples 1-4 exhibited varying degrees of discoloration during the stability assessment, and all exhibited PQQ loss rates exceeding 10%, failing the stability assessment. This suggests that the raw materials, dipropylene glycol, HMB, MONTANOV L, and olive oil, substituted in Example 1 are incompatible with PQQ, possibly due to a reaction that caused the PQQ loss.

[0223] 3 efficacy test

[0224] Test sample: Example 1

[0225] 3.1 Antioxidant test

[0226] Experimental content:

[0227] 3.1.1 Solution preparation

[0228] (1) Stock solution:

[0229] ABTS stock solution (7.4 mmol / L): Take 48 mg of ABTS and add 12.5 mL of distilled water.

[0230] K2S2O8 stock solution (2.6mmol / L): Take 189.2mg of K2S2O8 and add 5mL of distilled water.

[0231] (2) ABTS+K2S2O8 working solution: Mix 5 ml of 7.4 mmol / L ABTS stock solution with 88 µL of 2.6 mmol / L K2S2O8 and let it stand for 12-16 hours to prepare the ABTS+K2S2O8 working solution.

[0232] (3) Sample to be tested: In a 50 ml beaker, weigh 3.5 g of sample 1 red gel and 23 g of sample 2 white emulsion and mix them evenly. Then take 1 g of the mixture and add 4 g of pure water to dilute it to 20% of the liquid to be tested.

[0233] 3.1.2 Test steps

[0234] Take 0.4 mL of ABTS+K2S2O8 working solution and dilute it with pure water to an absorbance of 0.7 ± 0.02 at 734 nm at room temperature. Add 0.2 mL of ABTS+K2S2O8 working solution to a 96-well plate and mix with 10 μL of sample of varying concentrations. Incubate at room temperature in the dark for 6 minutes. Measure the absorbance at 734 nm. Repeat three times.

[0235] The ABTS free radical scavenging ability was calculated by the following formula:

[0236] Clearance = (1 - (Asample - Ablank) / Acontrol) * 100% Where:

[0237] Sample (sample group): 10ul sample solution + 200ul ABTS + K2S2O8 working solution;

[0238] Blank group: 10ul sample solution + 200ul pure water;

[0239] Control group: 10ul pure water + 200ul ABTS + K2S2O8 working solution.

[0240] 3.1.3 Experimental results:

[0241] ABTS + K2S2O8 clearance = (1 - (0.2602 - 0.0808) / 0.7072) × 100% = 74.63%

[0242] Table 3

[0243]

[0244] This shows that sample Example 1 has good antioxidant effect. The amount of PQQ added in several examples is consistent, and the samples of each example have been previously tested to be stable. Therefore, it is inferred that the antioxidant properties of the samples prepared in several examples are comparable.

[0245] 4 Human efficacy tests

[0246] Recruit more than 30 people to use the product of Example 1 and conduct instrument testing and consumer questionnaire surveys, with before-and-after comparisons to preliminarily verify the skin firming, repairing, moisturizing, and nourishing effects of the product after use.

[0247] 4.1 Water content of the skin stratum corneum

[0248] The subjects were tested five times using a Cornemeter CM825 instrument: before use, 15 minutes after use, 24 hours after use, 14 days after use, and 28 days after use. The results were recorded and the average value was used for final analysis. Parameter Interpretation: A higher test value indicates a higher moisture content in the skin's stratum corneum. Result Interpretation: If the moisture content of the stratum corneum in the test area significantly increases compared to the initial value after use, it indicates that the test sample has improved skin hydration.

[0249] 4.2 Transepidermal water loss

[0250] The subjects were tested five times using a Teaxmeter TM300: before use, 15 minutes after use, 24 hours after use, 14 days after use, and 28 days after use. The values ​​were recorded and the average value was used for final analysis. Parameter Explanation: Higher values ​​indicate higher transepidermal water loss and poorer skin barrier function. Lower values ​​indicate lower transepidermal water loss and better skin barrier function.

[0251] 4.3 Skin glossiness

[0252] Subjects were tested five times: before use, 15 minutes after use, 24 hours after use, 14 days after use, and 28 days after use. The average of three tests using a Glossymeter GL200 was used. Parameter Explanation: A higher test value indicates better skin gloss.

[0253] Result determination: If the skin glossiness of the test area increases significantly after use of the product compared to before use, it means that the test sample has the effect of improving skin glossiness.

[0254] 4.4 Skin elasticity and firmness

[0255] Before use, 15 minutes after use, 24 hours after use, 14 days after use, and 28 days after use, the subjects were tested 5 times in total. At each visit node, the Cutometer dual MPA580 was used to test and read the three R 2 The value and the tightness F value are averaged. 2 The value represents the total elasticity of the skin; higher values, closer to 100%, are better. For skin firmness, lower values ​​are better. If the skin firmness of the test area after product use is significantly lower than the initial value before use, it indicates that the test sample has an effect on improving skin firmness.

[0256] 4.5 Test results:

[0257] Table 4

[0258]

[0259] After 30 subjects used the formula in Example 1, the moisture content of the stratum corneum, transepidermal water loss, and skin gloss in the test area were significantly improved compared to the initial values ​​15 minutes, 24 hours, 14 days, and 28 days after use. Elasticity in the test area was also significantly improved 15 minutes, 14 days, and 28 days after use, compared to the initial values. This demonstrates that Example 1 has moisturizing, repairing, and nourishing effects.

[0260] The above are only preferred embodiments of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principles of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A cosmetic preparation containing PQQ disodium salt, characterized in that Including PQQ-2Na, humectant, emulsifier, oil, thickener and water; The moisturizing agent is glycerin and / or butylene glycol; The emulsifier is at least one of EMULPHARMA 1000, potassium cetearyl phosphate, polyglyceryl-6 distearate or hydrogenated lecithin; The thickener is at least one of acrylic acid (esters) / C10-30 alkyl acrylate crosspolymer, ammonium acryloyldimethyltaurate / VP copolymer, or hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer; The oil is at least one of caprylic and capric triglyceride, polydimethylsiloxane or isononyl isononanoate.

2. The cosmetic preparation according to claim 1, characterized in that The invention also includes a pH regulator, which is sodium hydroxide and / or aminomethyl propanol.

3. The cosmetic preparation according to claim 1 or 2, characterized in that The mass fractions of the components are: PQQ-2Na 0.02%, humectant 5%, thickener 0.2%~0.8%, emulsifier 2%, oil 10%, pH adjuster 0.02~0.08%, and the balance is water.

4. The cosmetic preparation according to claim 3, characterized in that Including PQQ-2Na, Glycerin, Acrylates / C10-30 Alkyl Acrylate Crosspolymer, EMULPHARMA 1000, Caprylic / Capric Triglyceride and Sodium Hydroxide; or including PQQ-2Na, butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, potassium cetearyl phosphate, dimethicone, and aminomethyl propanol; or including PQQ-2Na, glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol; Or include PQQ-2Na, glycerin, acrylates / C10-30 alkyl acrylate crosspolymer, caprylic / capric triglyceride, hydrogenated lecithin and sodium hydroxide; Alternatively, it may include PQQ-2Na, Glycerin, Butylene Glycol, Acrylates / C10-30 Alkyl Acrylate Crosspolymer, Ammonium Acryloyldimethyl Taurate / VP Copolymer, Hydroxyethyl Acrylate / Sodium Acryloyldimethyl Taurate Copolymer, EMULPHARMA 1000, Potassium Cetearyl Phosphate, Polyglyceryl-6 Distearate, Hydrogenated Lecithin, Caprylic / Capric Triglyceride, Dimethicone, Isononyl Isononanoate, Sodium Hydroxide, and Aminomethyl Propanol.

5. The cosmetic preparation according to claim 4, characterized in that The following components are included in the mass fraction: 0.02% PQQ-2Na, 5% glycerin, 0.2% acrylates / C10-30 alkyl acrylate crosspolymer, 2% EMULPHARMA 1000, 10% caprylic / capric triglyceride and 0.04% sodium hydroxide, the balance is water; Alternatively, it includes 0.02% PQQ-2Na, 5% butylene glycol, 0.8% ammonium acryloyldimethyltaurate / VP copolymer, 2% potassium cetearyl phosphate, 10% dimethicone and 0.02% aminomethyl propanol, with the balance being water; Alternatively, it includes 0.02% PQQ-2Na, 5% glycerin, 0.8% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 2% polyglyceryl-6 distearate and 10% isononyl isononanoate, and the balance is water; Or include 0.02% PQQ-2Na, 5% glycerin, 0.2% acrylates / C10-30 alkyl acrylate crosspolymer, 10% caprylic / capric triglyceride, 2% hydrogenated lecithin and 0.04% sodium hydroxide, the balance is water; Alternatively, it may include 0.02% PQQ-2Na, 2% glycerin, 3% butylene glycol, 0.1% acrylates / C10-30 alkyl acrylate crosspolymer, 0.3% ammonium acryloyldimethyl taurate / VP copolymer, 0.4% hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, 0.5% EMULPHARMA 1000, 0.5% potassium cetearyl phosphate, 0.5% polyglyceryl-6 distearate, 0.5% hydrogenated lecithin, 5% caprylic / capric triglyceride, 2.5% dimethicone, 2.5% isononyl isononanoate, 0.02% sodium hydroxide, and 0.06% aminomethyl propanol, with the balance being water.

6. The method for preparing the cosmetic preparation according to any one of claims 2 to 5, characterized in that: include: Mix the humectant, thickener and water and heat to obtain phase A; Mix the emulsifier and oil and heat to obtain phase B; Phase B is added to phase A and homogenized, and then PQQ-2Na and a pH adjuster are added while cooling, and stirred until uniformly dispersed to prepare the cosmetic preparation.

7. The preparation method according to claim 6, characterized in that The heating temperature of the phase A is 80-85°C; The heating temperature of the B phase is 80-85°C; After the phases A and B are homogenized, the temperature is lowered to 45°C.

8. The preparation method according to claim 6, characterized in that The homogenization conditions include a rotation speed of 3000 rps and 5 min.

9. Use of the cosmetic preparation according to any one of claims 1 to 5 or the cosmetic preparation prepared by the preparation method according to any one of claims 6 to 8 in the preparation of antioxidant, hydrating, and moisturizing products.

10. Use of the cosmetic preparation according to any one of claims 1 to 5 or the cosmetic preparation prepared by the preparation method according to any one of claims 6 to 8 in preparing a product for improving skin condition.

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