Cosmetic preparation containing PQQ disodium salt and preparation method and application thereof
By optimizing the composition of auxiliary materials in cosmetic preparations, the problem of poor stability of PQQ disodium salt in cosmetics is solved, and its stability and efficacy in cosmetics is improved, providing antioxidant, moisturizing and improving skin condition.
Patent Information
- Application Number
- CN202510766246.8
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-06-10
- Publication Date
- 2025-07-08
- Estimated Expiration
- 2045-06-10
AI Technical Summary
PQQ disodium salt has poor stability in cosmetics and is easy to react with other ingredients, resulting in reduced efficacy and affecting product quality and consumer experience.
By selecting suitable moisturizers, emulsifiers, thickeners, oils and pH regulators, a stable cosmetic preparation system is formed to ensure the stability of PQQ disodium salt in cosmetics.
At an added amount of 0.02%, maintain the physiological activity of PQQ disodium salt, achieve good antioxidant properties, and provide moisturizing, hydrating and improving skin condition.
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Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of cosmetics, in particular to a cosmetic preparation containing PQQ disodium salt and a preparation method and application thereof. Background Art
[0002] Pyrroloquinoline quinone (PQQ) was discovered in methylotrophic bacteria as a new type of oxidoreductase coenzyme. It was subsequently confirmed to be widely present in Gram-negative bacteria and higher plants and animals. It has multiple physiological functions, including anti-oxidation, anti-inflammation, promotion of cell metabolism, and protection of mitochondrial function. In the field of cosmetics, these properties of PQQ make it an ideal skin care ingredient. Its antioxidant capacity enables it to effectively resist the damage of free radicals to skin cells, delay skin aging, and reduce the formation of wrinkles; its anti-inflammatory effect helps relieve skin inflammation and soothe sensitive skin; and its promotion of cell metabolism can accelerate skin metabolism, improve dull skin tone, brighten skin tone, and make the skin glow with health. Therefore, PQQ has broad application prospects in many types of cosmetics such as anti-aging, whitening, and repair.
[0003] However, the stability of PQQ has always been a major problem for cosmetics developers. The structure of PQQ disodium salt (hereinafter referred to as PQQ) has a high redox potential and very high reactivity, and it is easy to react with amino acids to form IPQ. In addition, in actual formula development, it is found that PQQ disodium salt is also easy to react with some emulsifiers, oils, moisturizers, etc., which affects the activity of PQQ and leads to reduced efficacy.
[0004] Since the stability of PQQ is difficult to guarantee, it brings many difficulties to the development of cosmetics. On the one hand, in order to ensure that the product maintains stable efficacy during the validity period, R&D personnel have to reduce the amount of PQQ added, which limits its skin care effect to a certain extent. On the other hand, in order to improve the stability of PQQ, it is necessary to strictly screen the auxiliary materials of cosmetics, which not only increases the R&D cost of the product, but the auxiliary materials obtained by screening may not be conducive to the skin care effect. In addition, the instability of PQQ also makes it difficult to control product quality. Different batches of products may have different efficacy, affecting consumers' experience and the market reputation of the product.
[0005] It can be seen that PQQ-related skin care products are still difficult to develop and have 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 high-stability cosmetic preparation containing PQQ disodium salt and a preparation method and application thereof.
[0007] The cosmetic preparation containing disodium PQQ comprises PQQ-2Na, a humectant, an emulsifier and water; The humectant is glycerol and / or butanediol; The emulsifier is at least one of EMULPHARMA 1000, potassium cetyl phosphate, polyglyceryl-6 distearate or hydrogenated lecithin.
[0008] The cosmetic preparation of the present invention further comprises an oil, a thickener and / or a pH regulator; The pH regulator is sodium hydroxide and / or aminomethylpropanol; The thickener is at least one of acrylic acid (ester) / C10-30 alkanol acrylate crosslinked polymer, acryloyldimethyltaurine ammonium / VP copolymer or hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer; The oil is at least one of caprylic / capric triglyceride, polydimethylsiloxane or isononyl isononanoate.
[0009] In the cosmetic preparation provided by the present invention, the selection of excipients is reasonable, thereby reducing the loss of disodium PQQ. At an addition amount of 0.02%, the stability of disodium PQQ in the cosmetic is ensured. Thus, the physiological activity of disodium PQQ is ensured to be exerted, for example, its antioxidant performance is well retained. At the same time, due to the reasonable selection and content of each component, the prepared cosmetic preparation can have good moisturizing, water replenishing and skin condition improving effects.
[0010] In the examples of the present invention, the humectant is one kind, which is glycerol or butanediol, or the humectant is two kinds, which is a combination of glycerol and butanediol. Specifically, the mass ratio of glycerol to butanediol 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.
[0011] In the embodiments of the present invention, the thickener is one kind, which is an acrylic acid (ester) / C10-30 alkanol acrylate cross-linked polymer, an acryloyldimethyltaurine ammonium / VP copolymer, or a hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer. The thickener is two kinds, which are acrylic acid (ester) / C10-30 alkanol acrylate cross-linked polymer + acryloyldimethyltaurine ammonium / VP copolymer, or acrylic acid (ester) / C10-30 alkanol acrylate cross-linked polymer + hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, or acryloyldimethyltaurine ammonium / VP copolymer + hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer. The thickener is three kinds, which are acrylic acid (ester) / C10-30 alkanol acrylate cross-linked polymer + acryloyldimethyltaurine ammonium / VP copolymer + hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer. The present invention does not limit the proportion of each component in the thickener. As a feasible example, when the thickener is three kinds, the mass ratio of acrylic acid (ester) / C10-30 alkanol acrylate cross-linked polymer + acryloyldimethyltaurine ammonium / VP copolymer + hydroxyethyl acrylate / sodium acryloyldimethyltaurate 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.
[0012] In the embodiments of the present invention, there is one type of emulsifier, which is EMULPHARMA 1000, potassium cetostearyl phosphate, polyglyceryl-6 distearate, or hydrogenated lecithin. There are two types of emulsifiers, which are EMULPHARMA 1000 + potassium cetostearyl phosphate, or EMULPHARMA 1000 + polyglyceryl-6 distearate, or EMULPHARMA 1000 + hydrogenated lecithin, or potassium cetostearyl phosphate + polyglyceryl-6 distearate, or potassium cetostearyl phosphate + hydrogenated lecithin, or polyglyceryl-6 distearate + hydrogenated lecithin. There are three types of emulsifiers, which are EMULPHARMA 1000 + potassium cetostearyl phosphate + polyglyceryl-6 distearate, or EMULPHARMA 1000 + potassium cetostearyl phosphate + hydrogenated lecithin, or EMULPHARMA 1000 + polyglyceryl-6 distearate + hydrogenated lecithin, or potassium cetostearyl phosphate + polyglyceryl-6 distearate + hydrogenated lecithin. There are four types of emulsifiers, which are EMULPHARMA 1000 + potassium cetostearyl phosphate + polyglyceryl-6 distearate + hydrogenated lecithin. The present invention does not limit the proportion of each component in the emulsifier. As a feasible example, when there are four types of emulsifiers, the mass ratio of EMULPHARMA 1000 + potassium cetostearyl phosphate + polyglyceryl-6 distearate + hydrogenated lecithin is (0.4 - 0.6):(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.
[0013] In the embodiments of the present invention, there is one type of oil, which is caprylic / capric triglyceride, polydimethylsiloxane, or isononyl isononanoate. There are two types of oils, which are caprylic / capric triglyceride + polydimethylsiloxane, or caprylic / capric triglyceride + isononyl isononanoate, or polydimethylsiloxane + isononyl isononanoate. There are three types of oils, which are caprylic / capric triglyceride + polydimethylsiloxane + isononyl isononanoate. The present invention does not limit the proportion of each component in the oil. As a feasible example, when there are three types of oils, 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.
[0014] In the embodiments of the present invention, there is one kind of pH regulator, which is sodium hydroxide or aminomethylpropanol. There are two kinds of pH regulators, which are sodium hydroxide and aminomethylpropanol. Specifically, the mass ratio of sodium hydroxide to aminomethylpropanol is (0.01~0.03):(0.05~0.07). In specific embodiments, the mass ratio is 0.02:0.06.
[0015] In the present invention, the dosage form of the cosmetic preparation may be an aqueous solution. For example, it may be lotion, toner, softening lotion, moisturizing lotion, essence lotion, makeup lotion or aftershave lotion. Or, if components such as oils are added to the preparation of the cosmetic, the dosage form of the cosmetic may also be cream, emulsion, body cream, hand cream, eye cream, neck cream, day cream, night cream, sleeping mask or massage cream. The present invention does not make any limitation in this regard.
[0016] In the cosmetic preparation of the present invention, one or more of each type of auxiliary material can be selected, and the present invention does not make any limitation in this regard. The examples record cases where one kind of each type of auxiliary material is selected, and also record cases where multiple kinds of each type of auxiliary material are selected. Taking the selection of one kind of each type of auxiliary material as an example: The cosmetic preparation includes glycerin, acrylate / C10-30 alkyl acrylate cross-linked polymer, cetearyl alcohol phosphate potassium, caprylic / capric triglyceride, sodium hydroxide.
[0017] Or the cosmetic preparation includes glycerin, acrylate / C10-30 alkyl acrylate cross-linked polymer, cetearyl alcohol phosphate potassium, caprylic / capric triglyceride, aminomethylpropanol.
[0018] Or the cosmetic preparation includes glycerin, acrylate / C10-30 alkyl acrylate cross-linked polymer, cetearyl alcohol phosphate potassium, polydimethylsiloxane, sodium hydroxide.
[0019] Or the cosmetic preparation includes glycerin, acrylate / C10-30 alkyl acrylate cross-linked polymer, cetearyl alcohol phosphate potassium, polydimethylsiloxane, aminomethylpropanol.
[0020] Or the cosmetic preparation includes glycerin, acrylate / C10-30 alkyl acrylate cross-linked polymer, cetearyl alcohol phosphate potassium, isononyl isononanoate, sodium hydroxide.
[0021] Or the cosmetic preparation includes glycerin, acrylate / C10-30 alkyl acrylate cross-linked polymer, cetearyl alcohol phosphate potassium, isononyl isononanoate, aminomethylpropanol.
[0022] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.
[0023] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethylpropanol.
[0024] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.
[0025] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, polydimethylsiloxane, and aminomethylpropanol.
[0026] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.
[0027] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethylpropanol.
[0028] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.
[0029] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethylpropanol.
[0030] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.
[0031] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethylpropanol.
[0032] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.
[0033] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, isononyl isononanoate, and aminomethyl propanol.
[0034] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.
[0035] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethyl propanol.
[0036] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.
[0037] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, polydimethylsiloxane, and aminomethyl propanol.
[0038] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.
[0039] Alternatively, the cosmetic preparation comprises glycerin, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, isononyl isononanoate, and aminomethyl propanol.
[0040] Alternatively, the cosmetic preparation comprises glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, cetearyl alcohol phosphate potassium, caprylic / capric triglyceride, and sodium hydroxide.
[0041] Alternatively, the cosmetic preparation comprises glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, cetearyl alcohol phosphate potassium, caprylic / capric triglyceride, and aminomethyl propanol.
[0042] Alternatively, the cosmetic preparation comprises glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, cetearyl alcohol phosphate potassium, polydimethylsiloxane, and sodium hydroxide.
[0043] Alternatively, the cosmetic preparation comprises glycerin, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, cetearyl alcohol phosphate potassium, polydimethylsiloxane, and aminomethyl propanol.
[0044] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, potassium cetyl phosphate, isononyl isononanoate, and sodium hydroxide.
[0045] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, potassium cetyl phosphate, isononyl isononanoate, and aminomethylpropanol.
[0046] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.
[0047] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethylpropanol.
[0048] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.
[0049] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and aminomethylpropanol.
[0050] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.
[0051] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethylpropanol.
[0052] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.
[0053] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethylpropanol.
[0054] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.
[0055] Alternatively, the cosmetic preparation comprises glycerin, sodium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethylpropanol.
[0056] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.
[0057] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethylpropanol.
[0058] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.
[0059] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethylpropanol.
[0060] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.
[0061] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, polydimethylsiloxane, and aminomethylpropanol.
[0062] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.
[0063] Alternatively, the cosmetic preparation comprises glycerol, sodium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, isononyl isononanoate, and aminomethylpropanol.
[0064] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosspolymer, potassium cetyl phosphate, caprylic / capric triglyceride, and sodium hydroxide.
[0065] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosspolymer, potassium cetyl phosphate, caprylic / capric triglyceride, and aminomethylpropanol.
[0066] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosspolymer, potassium cetyl phosphate, polydimethylsiloxane, and sodium hydroxide.
[0067] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, cetearyl alcohol phosphate potassium, polydimethylsiloxane, and aminomethylpropanol.
[0068] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, cetearyl alcohol phosphate potassium, isononyl isononanoate, and sodium hydroxide.
[0069] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, cetearyl alcohol phosphate potassium, isononyl isononanoate, and aminomethylpropanol.
[0070] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.
[0071] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethylpropanol.
[0072] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.
[0073] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, polydimethylsiloxane, and aminomethylpropanol.
[0074] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.
[0075] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethylpropanol.
[0076] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.
[0077] Alternatively, the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethylpropanol.
[0078] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.
[0079] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethylpropanol.
[0080] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.
[0081] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, hydrogenated lecithin, isononyl isononanoate, and aminomethylpropanol.
[0082] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.
[0083] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethylpropanol.
[0084] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.
[0085] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, polydimethylsiloxane, and aminomethylpropanol.
[0086] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.
[0087] Or the cosmetic preparation comprises butylene glycol, acrylate / C10-30 alkyl acrylate crosslinked polymer, EMULPHARMA, isononyl isononanoate, and aminomethylpropanol.
[0088] Or the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, cetearyl alcohol phosphate potassium, caprylic / capric triglyceride, and sodium hydroxide.
[0089] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, potassium cetyl phosphate, caprylic / capric triglyceride, and aminomethyl propanol.
[0090] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, potassium cetyl phosphate, polydimethylsiloxane, and sodium hydroxide.
[0091] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, potassium cetyl phosphate, polydimethylsiloxane, and aminomethyl propanol.
[0092] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, potassium cetyl phosphate, isononyl isononanoate, and sodium hydroxide.
[0093] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, potassium cetyl phosphate, isononyl isononanoate, and aminomethyl propanol.
[0094] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.
[0095] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethyl propanol.
[0096] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.
[0097] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and aminomethyl propanol.
[0098] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.
[0099] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethyl propanol.
[0100] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.
[0101] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethyl propanol.
[0102] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.
[0103] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethyl propanol.
[0104] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.
[0105] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethyl propanol.
[0106] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.
[0107] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethyl propanol.
[0108] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.
[0109] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, polydimethylsiloxane, and aminomethyl propanol.
[0110] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.
[0111] Alternatively, the cosmetic preparation comprises butylene glycol, hydroxyethyl acrylate / sodium acryloyldimethyl taurate copolymer, EMULPHARMA, isononyl isononanoate, and aminomethyl propanol.
[0112] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, potassium cetylstearyl phosphate, caprylic / capric triglyceride, and sodium hydroxide.
[0113] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, potassium cetylstearyl phosphate, caprylic / capric triglyceride, and aminomethylpropanol.
[0114] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, potassium cetylstearyl phosphate, polydimethylsiloxane, and sodium hydroxide.
[0115] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, potassium cetylstearyl phosphate, polydimethylsiloxane, and aminomethylpropanol.
[0116] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, potassium cetylstearyl phosphate, isononyl isononanoate, and sodium hydroxide.
[0117] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, potassium cetylstearyl phosphate, isononyl isononanoate, and aminomethylpropanol.
[0118] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and sodium hydroxide.
[0119] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, polyglyceryl-6 distearate, caprylic / capric triglyceride, and aminomethylpropanol.
[0120] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and sodium hydroxide.
[0121] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, polyglyceryl-6 distearate, polydimethylsiloxane, and aminomethylpropanol.
[0122] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and sodium hydroxide.
[0123] Alternatively, the cosmetic preparation comprises butylene glycol, acryloyldimethyltaurine / VP copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethylpropanol.
[0124] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and sodium hydroxide.
[0125] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, caprylic / capric triglyceride, and aminomethylpropanol.
[0126] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, polydimethylsiloxane, and sodium hydroxide.
[0127] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, polydimethylsiloxane, and aminomethylpropanol.
[0128] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, isononyl isononanoate, and sodium hydroxide.
[0129] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, hydrogenated lecithin, isononyl isononanoate, and aminomethylpropanol.
[0130] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, caprylic / capric triglyceride, and sodium hydroxide.
[0131] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, caprylic / capric triglyceride, and aminomethylpropanol.
[0132] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, polydimethylsiloxane, and sodium hydroxide.
[0133] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, polydimethylsiloxane, and aminomethylpropanol.
[0134] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, isononyl isononanoate, and sodium hydroxide.
[0135] Alternatively, the cosmetic preparation comprises butylene glycol, ammonium acryloyldimethyltaurate / VP copolymer, EMULPHARMA, isononyl isononanoate, and aminomethylpropanol.
[0136] In the present invention, the mass fractions of the components in the cosmetic preparation are not limited, and they can be concentrations suitable for use, or can be present in an amount 2 to 100 times the concentration suitable for use. For example, it is 2 times, 5 times, 10 times, 20 times, 25 times, 50 times or 100 times the use concentration.
[0137] In the examples of the present invention, the mass fractions of the components in the cosmetic are as follows: PQQ-2Na 0.01% - 0.03%, humectant 3% - 7%, thickener 0.2% - 0.8%, emulsifier 1% - 3%, oil 8% - 12%, pH regulator 0.02% - 0.08%, and the balance is water.
[0138] Specifically, within the concentration range described above, by selecting the excipients described above, a stable cosmetic preparation with good activity can be obtained. As a feasible case, the mass fractions of the components in the cosmetic are as follows: PQQ-2Na 0.02%, humectant 5%, thickener 0.2% - 0.8%, emulsifier 2%, oil 10%, pH regulator 0.02% - 0.08%, and the balance is water.
[0139] In some embodiments, the cosmetic includes PQQ-2Na, glycerol, acrylate / C10-30 alkanol acrylate cross-linked polymer, EMULPHARMA 1000, caprylic / capric triglyceride, and sodium hydroxide; in this embodiment, the cosmetic includes the following components in mass fractions: 0.02% PQQ-2Na, 5% glycerol, 0.2% acrylate / C10-30 alkanol acrylate cross-linked polymer, 2% EMULPHARMA 1000, 10% caprylic / capric triglyceride, and 0.04% sodium hydroxide, and the balance is water.
[0140] In some embodiments, the cosmetic includes PQQ-2Na, butanediol, acryloyldimethyltaurate / VP copolymer, cetylstearyl phosphate potassium, polydimethylsiloxane, and aminomethylpropanol; in this embodiment, the cosmetic includes the following components in mass fractions: 0.02% PQQ-2Na, 5% butanediol, 0.8% acryloyldimethyltaurate / VP copolymer, 2% cetylstearyl phosphate potassium, 10% polydimethylsiloxane, and 0.02% aminomethylpropanol, and the balance is water; In some embodiments, the cosmetic contains PQQ-2Na, glycerol, sodium acryloyldimethyltaurate / VP copolymer, polyglyceryl-6 distearate, isononyl isononanoate, and aminomethylpropanol; in this embodiment, the cosmetic contains the following components by mass fraction: 0.02% PQQ-2Na, 5% glycerol, 0.8% sodium acryloyldimethyltaurate / VP copolymer, 2% polyglyceryl-6 distearate, and 10% isononyl isononanoate, with the balance being water; In some embodiments, the cosmetic contains PQQ-2Na, glycerol, acrylate / C10-30 alkyl acrylate crosslinked polymer, caprylic / capric triglyceride, hydrogenated lecithin, and sodium hydroxide; in this embodiment, the cosmetic contains the following components by mass fraction: 0.02% PQQ-2Na, 5% glycerol, 0.2% acrylate / C10-30 alkyl acrylate crosslinked polymer, 10% caprylic / capric triglyceride, 2% hydrogenated lecithin, and 0.04% sodium hydroxide, with the balance being water; In some embodiments, the cosmetic contains PQQ-2Na, glycerol, butanediol, acrylate / C10-30 alkyl acrylate crosslinked polymer, ammonium acryloyldimethyltaurate / VP copolymer, sodium acryloyldimethyltaurate / VP copolymer, EMULPHARMA 1000, potassium cetylstearyl phosphate, polyglyceryl-6 distearate, hydrogenated lecithin, caprylic / capric triglyceride, polydimethylsiloxane, isononyl isononanoate, sodium hydroxide, and aminomethylpropanol. In this embodiment, the cosmetic contains the following components by mass fraction: 0.02% PQQ-2Na, 2% glycerol, 3% butanediol, 0.1% acrylate / C10-30 alkyl acrylate crosslinked polymer, 0.3% ammonium acryloyldimethyltaurate / VP copolymer, 0.4% sodium acryloyldimethyltaurate / VP copolymer, 0.5% EMULPHARMA 1000, 0.5% potassium cetylstearyl 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% aminomethylpropanol, with the balance being water.
[0141] Furthermore, the present invention also provides a method for preparing the cosmetic preparation, comprising: Mixing a humectant, a thickener, and water, and heating to obtain Phase A; Mixing an emulsifier and an oil, and heating to obtain Phase B; Adding Phase B to Phase A for homogenization, then cooling and adding PQQ-2Na and a pH regulator, and stirring until evenly dispersed to obtain the cosmetic preparation.
[0142] In specific embodiments, the heating temperature of the A phase is 80 - 85°C, and the heating temperature of the B phase is 80 - 85°C. After homogenizing the A and B phases, the temperature is lowered to 45°C.
[0143] In specific embodiments, the conditions for homogenization include a rotation speed of 3000 rps for 5 minutes.
[0144] 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 antioxidant, moisturizing, hydration and / or improving skin condition.
[0145] In the present invention, the improvement of skin condition includes enhancing skin gloss, improving skin elasticity and / or increasing skin firmness.
[0146] Furthermore, the present invention also provides a method for antioxidant, moisturizing, hydration and / or improving skin condition, which includes applying the cosmetic preparation as described above or the cosmetic preparation prepared by the preparation method as described above on the skin surface.
[0147] In the present invention, the application methods include, but are not limited to, spreading, wiping, patting, massaging, dotting, tapping, evenly spreading, thick application or thin application.
[0148] 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, hip skin, skin around the eyes or skin around the lips.
[0149] In the cosmetic preparation provided by the present invention, excipients in combination with PQQ-2Na are screened and optimized. The finally obtained product can not only ensure the stability of PQQ-2Na, but also achieve good skin care effects. For example, it can improve the effects of moisturizing, hydration, antioxidant and / or improving skin condition. Detailed implementation mode
[0150] The present invention provides a cosmetic preparation containing PQQ disodium salt, its preparation method and application. Those skilled in the art can draw on the content of this article and appropriately modify the process parameters to achieve. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art, and they are all considered to be included in the present invention. The methods and applications of the present invention have been described through preferred embodiments. Relevant personnel can obviously make changes or appropriate alterations and combinations to the methods and applications in this article without departing from the content, spirit and scope of the present invention to implement and apply the technology of the present invention.
[0151] The numerical ranges and parameters involved in the present invention are presented as precisely as possible in the specific embodiments. However, any numerical value inevitably contains standard deviations caused by individual testing methods. Therefore, unless otherwise clearly stated, it should be understood that all numerical ranges or specific data used in this disclosure may have certain reasonable deviations within a certain range, for example: within ±10%, ±5%, ±1% or ±0.5%.
[0152] Some cases are recorded in the embodiments and comparative examples of the present invention. Among them, the embodiments show certain implementation manners of the present invention. However, this does not mean that the effects of the present invention can only be achieved in these cases. In fact, good effects can be achieved at any concentration of each component between the two endpoint values shown in the embodiments.
[0153] Each auxiliary material in the cosmetic preparation provided by the present invention has been strictly screened. In the preliminary experiment, available components were screened from a large number of auxiliary materials. For example, for the humectant, the present invention screened from 25 humectants (such as glycerol, butanediol, dipropylene glycol, 1,3 - propanediol, methylpropanediol, polyethylene glycol - 8, glycerol polyether - 26, propylene glycol, panthenol, hydroxyethylurea, etc.) and obtained that glycerol, butanediol and PQQ can coexist, and the degradation rate of PQQ - 2Na is less than 7%, while other humectants will cause a large amount of degradation of PQQ. Similarly, the present invention also screened suitable components from 20 thickeners, 30 emulsifiers, 25 oils and fats, and 6 pH regulators. The thickeners excluded due to inability to coexist with PQQ, causing color change of the product, etc. include but are not limited to acryloyldimethyltauramide / sorbitan - 25 methacrylate cross - polymer, xanthan gum, scleroglucan. The emulsifiers excluded include but are not limited to MONTANOV L, hydrogenated lecithin, Olivem®1000, sodium stearoyl glutamate, ResPharma, sucrose stearate, GLUCAMATE SSE - 20. The oils and fats excluded include but are not limited to olive fruit oil, cetearyl alcohol, behenyl alcohol, shea butter, isocetane. The pH regulators excluded include but are not limited to arginine, triethanolamine. The degradation rate of PQQ - 2Na caused by these excluded auxiliary materials reaches more than 10% and will not be elaborated in the specific embodiments.
[0154] It should be understood that in different embodiments of the present invention, the magnitude of the step numbers does not represent the priority of the execution order. Some or all steps can be implemented in parallel or executed in any order, and the specific execution process should be determined based on the functional logic and should not be regarded as a limitation to the implementation manner of this application.
[0155] The test materials used in the present invention are all ordinary commercially available products and can be purchased in the market. The present invention will be further elaborated below in combination with the embodiments: Embodiment 1. Examples and Comparative Formulations In Examples 1 to 4, the polyols, thickeners, emulsifiers, oils and fats, and pH regulators are different. In Examples 5 and 6, each formulation module is a compound raw material, and the purpose is to verify the effect of the compound of different raw materials on stability. The formulations of Comparative Examples 1 to 4 replace the polyols, thickeners, emulsifiers, and oils and fats respectively on the basis of Example 1. The specific formulations are shown in Table 1: Table 1 Formulation Table
[0156]
[0157] 1.2 Reagents EMULPHARMA 1000 is from Shanghai Yiheng Chemical Industry, and MONTANOV L is from SEPPIC.
[0158] 1.3 Preparation Method Mix the humectant, thickener and water, and heat to 80 - 85 °C to obtain Phase A; mix the emulsifier and oil and fat, and heat to 80 - 85 °C to obtain Phase B; add Phase B to Phase A and homogenize for 5 minutes to obtain a homogeneous mass, cool to 45 °C, then add PQQ and pH regulator, stir until evenly dispersed, defoam, cool and discharge to obtain the finished cream product.
[0159] 2. Stability Investigation Place Examples 1 - 6 and Comparative Examples 1 - 4 at 25 °C, 4 °C, 40 °C, and 48 °C for 4 weeks respectively, and observe the initial state, color, and pH value of each sample at 2 weeks and 4 weeks. The results are shown in Tables 2 - 1 and 2 - 2.
[0160] 2.1 Detection of PQQ Disodium Salt Loss Rate Detection Method 2.1.1 Principle PQQ disodium salt is dissolved, separated by reverse - phase high - performance liquid chromatography, detected by an ultraviolet detector, and quantified by the standard curve method.
[0161] 2.2 Reagents and Materials Unless otherwise specified, all reagents used in this method (such as dipotassium hydrogen phosphate trihydrate, tetrabutylammonium bromide, phosphoric acid) are of analytical grade, The water is the first - grade water specified in the "Specifications and Test Methods for Laboratory Water" of GB / T 6682 - 2008.
[0162] Acetonitrile: Chromatographic grade.
[0163] PQQ disodium salt standard: Purity ≥ 97.0%.
[0164] Water - phase microporous filter membrane: 0.22 μm.
[0165] 10 mmol / L Dipotassium Hydrogen Phosphate - 15 mmol / L Tetrabutylammonium Bromide Mixed Solution (pH 7.4): Weigh 2.28 g of dipotassium hydrogen phosphate trihydrate and 4.84 g of tetrabutylammonium bromide into a beaker, add 800 mL of water, dissolve by ultrasonic treatment, adjust the pH to 7.4 with phosphoric acid, transfer to a 1000 mL volumetric flask, make up the volume with water, and shake well. Vacuum filter with a 0.22 μm aqueous microporous membrane, and then ultrasonic until there are no bubbles.
[0166] Acetonitrile - Water Solution (volume ratio 1:3): Measure 250 mL of acetonitrile and 750 mL of water respectively, add them to a reagent bottle, and mix well.
[0167] 2.3 Instruments and Equipment High - performance liquid chromatograph equipped with an ultraviolet detector and an automatic sampler.
[0168] Electronic balance: The sensitivity is 0.01 mg.
[0169] 2.4 Analysis Procedures 2.4.1 Preparation of Standard Solution Weigh 40 mg of PQQ disodium salt standard (accurate to 0.01 mg), place it in a 100 mL volumetric flask, add acetonitrile - water solution to dissolve and make up the volume to the mark, shake well, and obtain a PQQ disodium salt standard stock solution with a concentration of 0.4 mg / mL. Dilute this solution to 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.
[0170] 2.4.2 Sample Treatment Weigh 20 mg of each sample of Examples 1 - 6 and Comparative Examples 1 - 4 (accurate to 0.01 mg), place them in 50 mL volumetric flasks, add acetonitrile - water solution to dissolve and make up the volume to the mark, shake well; then accurately pipette 5.0 mL of the above solution into a 10 mL volumetric flask, dilute to the mark with acetonitrile - water solution, shake well, and vacuum filter the filtrate with a 0.22 μm aqueous microporous membrane for determination.
[0171] 2.4.3 Reference Conditions for Liquid Chromatography Chromatographic column: PFchrom EP C18 88031205 - 4625 (4.6 mm × 250 mm, 5 μm, 120A) or a chromatographic column with equivalent performance.
[0172] 2.4.4 Determination Under the specified chromatographic conditions, take 20 μL of each standard solution and sample solution, inject them into the liquid chromatograph respectively, conduct chromatographic analysis, and record the peak areas of sodium PQQ in the chromatograms of the obtained standard solutions and sample solutions. Using the peak area of sodium PQQ in the standard solution as the Y-axis and the corresponding standard solution concentration as the X-axis, plot the standard curve to obtain the sodium PQQ standard curve. Based on the peak area of sodium PQQ in the sample solution chromatogram, calculate the concentration of sodium PQQ in the sample solution from the standard curve.
[0173] 2.5 Result Calculation 2.5.1 Result Calculation of Sodium PQQ Content The content of sodium PQQ in the sample is calculated as its mass fraction W1, and the value is expressed as a percentage (%), calculated according to formula (1):
[0174] (1) In the formula: C —— The concentration of sodium pyrroloquinoline quinone disodium salt in the sample solution obtained from the standard curve, unit: milligram per milliliter (mg / mL); V —— The dilution volume of the sample, unit: milliliter (mL); f —— The purity of the sodium PQQ standard; m —— The mass of the sample, unit: milligram (mg); W2 —— The mass fraction of water in the sample, and the value is expressed as a percentage (%).
[0175] Take the arithmetic mean of the parallel determination results as the determination result, and express the result to two decimal places.
[0176] 2.5.2 Result Calculation of Sodium PQQ Loss Rate Sodium PQQ loss rate = (content of sodium PQQ in the initial sample - content of sodium PQQ in the stability sample) / content of sodium PQQ in the initial sample × 100% 2.6 Precision The relative standard deviation of two independent determinations obtained under repeatability conditions is not greater than 2.0%.
[0177] 2.7 Stability Test Results Table 2-1 Stability Test Results of Examples 1 to 6
[0178]
[0179] Table 2-2 Stability Test Results of Comparative Examples 1 to 4
[0180]
[0181] The data results in Table 2-1 and Table 2-2 show that: the appearance and viscosity of Examples 1-6 meet the requirements after 4 weeks of stability, and the loss rate of pqq-2Na is less than 10%, within the loss range of active substances that are relatively active in the industry, and the stability passes. It shows that the following raw materials in the cream formula have good compatibility with pqq-2Na and can form a stable formula: the humectant raw materials glycerol and butanediol, the thickener raw materials acrylic (ester) / C10-30 alkanol acrylate cross-linked polymer, acryloyldimethyltaurine ammonium / VP copolymer or hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, the emulsifier raw materials EMULPHARMA 1000, potassium cetylstearyl phosphate, polyglyceryl-6 distearate or hydrogenated lecithin, the oil raw materials caprylic / capric triglyceride, polydimethylsiloxane or isononyl isononanoate, the pH regulators sodium hydroxide and aminomethylpropanol.
[0182] During the stability investigation of Comparative Examples 1-4, there were varying degrees of discoloration problems, and the phenomenon that the pqq loss rate was higher than 10% occurred in all cases, and the stability judgment did not pass. It shows that the raw materials dipropylene glycol, HMB, MONTANOV L and olive fruit oil replaced on the basis of Example 1 in the comparative examples are incompatible with pqq, and it may be that some reaction occurs resulting in pqq loss.
[0183] 3 Efficacy Tests Test sample: Example 1 3.1 Antioxidant Test Experimental content: 3.1.1 Solution preparation (1) Stock solution: ABTS stock solution (7.4 mmol / L): Take 48 mg of ABTS and add 12.5 mL of distilled water.
[0184] K2S2O8 stock solution (2.6 mmol / L): Take 189.2 mg of K2S2O8 and add 5 mL of distilled water.
[0185] (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.
[0186] (3) Test sample: Weigh 3.5 g of sample 1 red gel and 23 g of sample 2 white emulsion in a 50 ml beaker and mix them evenly. Then take 1 g of the mixture and dilute it with 4 g of pure water to a 20% test liquid.
[0187] 3.1.2 Test steps Take 0.4 mL of ABTS+K2S2O8 working solution and dilute it with pure water, requiring an absorbance value of 0.7±0.02 at 734 nm at room temperature. Add 0.2 mL of ABTS+K2S2O8 working solution and 10 μL of samples with different concentrations to a 96-well plate, mix well, and let it stand in the dark at room temperature for 6 min. Measure the absorbance at a wavelength of 734 nm, and repeat the measurement 3 times in parallel.
[0188] The ABTS free radical scavenging ability is calculated by the following formula: Scavenging rate = (1 - (Asample - Ablank) / Acontrol) * 100% Where: sample (sample group): 10 μL of sample solution + 200 μL of ABTS+K2S2O8 working solution; blank (blank group): 10 μL of sample solution + 200 μL of pure water; control (control group): 10 μL of pure water + 200 μL of ABTS+K2S2O8 working solution.
[0189] 3.1.3 Experimental results: ABTS+K2S2O8 scavenging rate = (1 - (0.2602 - 0.0808) / 0.7072) × 100% = 74.63% Table 3
[0190]
[0191] It shows that Sample Example 1 has good antioxidant efficacy. The addition amount of the antioxidant active substance PQQ in several examples is the same, and the samples of each example were previously determined to be stable. Therefore, it is inferred that the antioxidant properties of the samples prepared in several examples are quite comparable.
[0192] 4 Human efficacy test Recruit more than 30 people for instrumental testing and consumer questionnaire surveys after using the product of Example 1, with before-and-after comparison, to preliminarily verify the effects of firming, repairing, moisturizing, and nourishing the skin after using the product.
[0193] 4.1 Skin stratum corneum water content Before use, 15 min after use, 24 h after use, 14 days after use, and 28 days after use, a total of 5 times, instrumentally test the subjects using a Cornemeter CM825 3 times, record the values, and finally analyze and take the average value. Parameter explanation: The higher the test value, the higher the skin stratum corneum water content. Result determination: If the water content of the stratum corneum in the test area significantly increases compared with the initial value after using the product, it indicates that the test sample has the effect of improving skin moisture.
[0194] 4.2 Transdermal water loss of the skin Before use, 15 minutes after use, 24 hours after use, 14 days after use, and 28 days after use, a total of 5 times, the subjects were tested with an instrument. The Teaxmeter TM300 was used to test 3 times, and the values were recorded. Finally, the average value was taken for analysis. Parameter explanation: The higher the test value, the higher the transdermal water loss of the skin and the worse the skin barrier function. The lower the test value, the lower the transdermal water loss of the skin and the better the skin barrier function.
[0195] 4.3 Skin glossiness Before use, 15 minutes after use, 24 hours after use, 14 days after use, and 28 days after use, a total of 5 times, the subjects were tested with an instrument. The Glossymeter GL200 was used to test 3 times and the average value was taken. Parameter explanation: The higher the test value, the better the glossiness of the skin surface.
[0196] Result determination: If the glossiness of the skin in the test area is significantly increased after the product is used compared with that before use, it indicates that the test sample has the effect of improving the skin gloss.
[0197] 4.4 Skin elasticity and firmness Before use, 15 minutes after use, 24 hours after use, 14 days after use, and 28 days after use, a total of 5 times, the subjects were tested with an instrument. At each visit node, the Cutometer dual MPA580 was used for testing, and three R 2 values and the firmness F value were read, and the average was taken. The R 2 value represents the total skin elasticity. The higher the value, the closer it is to 100% is better. The lower the skin firmness F value is, the better. If the skin firmness in the test area after the product is used is significantly lower than the initial value before use, it indicates that the test sample has the effect of improving skin firmness.
[0198] 4.5 Test results: Table 4
[0199]
[0200] After 30 subjects used the test sample Example 1 of the formulation of Example 1, 15 minutes, 24 hours, 14 days, and 28 days later, the water content of the stratum corneum, transdermal water loss, and skin glossiness of the skin in the test area were improved compared with the initial values, and there were significant differences in the values; 15 minutes, 14 days, and 28 days after using the test sample Example 1, the elasticity of the skin in the test area was improved compared with the initial value, and there were significant differences in the values. It shows that Example 1 of the sample has the effects of moisturizing, repairing, and nourishing.
[0201] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.
Claims
1. A cosmetic preparation containing PQQ disodium salt, characterized in that, It includes PQQ-2Na, a humectant, an emulsifier and water; The humectant is glycerol and / or butanediol; The emulsifier is at least one of EMULPHARMA 1000, potassium cetyl phosphate, polyglyceryl-6 distearate or hydrogenated lecithin.
2. The cosmetic preparation according to claim 1, characterized in that, It also includes an oil, a thickener and / or a pH regulator; The pH regulator is sodium hydroxide and / or aminomethylpropanol; The thickener is at least one of acrylate / C10-30 alkanol acrylate cross-linked polymer, acryloyldimethyltauramide / VP copolymer or hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer; The oil is at least one of caprylic / capric triglyceride, polydimethylsiloxane or isononyl isononanoate.
3. The cosmetic preparation according to claim 1 or 2, characterized in that Among them, the mass fractions of each component are: 0.02% of PQQ-2Na, 5% of humectant, 0.2% - 0.8% of thickener, 2% of emulsifier, 0 - 10% of oil, 0.02 - 0.08% of pH regulator, and the balance is water.
4. The cosmetic preparation according to claim 3, characterized in that it includes PQQ-2Na, glycerol, acrylate / C10-30 alkanol acrylate cross-linked polymer, EMULPHARMA1000, caprylic / capric triglyceride and sodium hydroxide; or it includes PQQ-2Na, butanediol, acryloyldimethyltauramide / VP copolymer, potassium cetyl phosphate, polydimethylsiloxane and aminomethylpropanol; or it includes PQQ-2Na, glycerol, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, polyglyceryl-6 distearate, isononyl isononanoate and aminomethylpropanol; or it includes PQQ-2Na, glycerol, acrylate / C10-30 alkanol acrylate cross-linked polymer, caprylic / capric triglyceride, hydrogenated lecithin and sodium hydroxide; or it includes PQQ-2Na, glycerol, butanediol, acrylate / C10-30 alkanol acrylate cross-linked polymer, acryloyldimethyltauramide / VP copolymer, hydroxyethyl acrylate / sodium acryloyldimethyltaurate copolymer, EMULPHARMA 1000, potassium cetyl phosphate, polyglyceryl-6 distearate, hydrogenated lecithin, caprylic / capric triglyceride, polydimethylsiloxane, isononyl isononanoate, sodium hydroxide and aminomethylpropanol.
5. The cosmetic preparation according to claim 4, characterized in that, It includes components with the following mass fractions: 0.02% of PQQ-2Na, 5% of glycerol, 0.2% of acrylate / C10-30 alkanol acrylate cross-linked polymer, 2% of EMULPHARMA 1000, 10% of caprylic / capric triglyceride and 0.04% of sodium hydroxide, and the balance is water; or it includes 0.02% of PQQ-2Na, 5% of butanediol, 0.8% of acryloyldimethyltauramide / VP copolymer, 2% of potassium cetyl phosphate, 10% of polydimethylsiloxane and 0.02% of aminomethylpropanol, and the balance is water; Or it contains 0.02% PQQ-2Na, 5% glycerol, 0.8% sodium acryloyldimethyltaurate / VP copolymer, 2% diglyceryl distearate, and 10% isononyl isononanoate, with the balance being water; Or it contains 0.02% PQQ-2Na, 5% glycerol, 0.2% acrylate / C10-30 alkyl acrylate crosspolymer, 10% caprylic / capric triglyceride, 2% hydrogenated lecithin, and 0.04% sodium hydroxide, with the balance being water; Or it contains 0.02% PQQ-2Na, 2% glycerol, 3% butylene glycol, 0.1% acrylate / C10-30 alkyl acrylate crosspolymer, 0.3% ammonium acryloyldimethyltaurate / VP copolymer, 0.4% sodium acryloyldimethyltaurate / VP copolymer, 0.5% EMULPHARMA 1000, 0.5% potassium cetyl phosphate, 0.5% diglyceryl 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. A method for preparing the cosmetic preparation according to any one of claims 1 to 5, characterized in that, It includes: Mix a humectant, a thickener, and water, and heat to obtain Phase A; Mix an emulsifier and an oil, and heat to obtain Phase B; Add Phase B to Phase A for homogenization, then cool down and add PQQ-2Na and a pH regulator, and stir until evenly dispersed to obtain the cosmetic preparation.
7. The preparation method according to claim 6, wherein, The heating temperature of Phase A is 80-85°C; The heating temperature of Phase B is 80-85°C; After homogenization of Phase A and Phase B, cool down to 45°C.
8. The preparation method according to claim 6, characterized in that, The conditions for the homogenization include a rotation speed of 3000 rps for 5 minutes.
9. Use of the cosmetic preparation according to any one of claims 1-5 or the cosmetic preparation prepared by the preparation method according to any one of claims 6-8 in the preparation of a product for antioxidant, moisturizing, hydrating and / or improving skin condition.
Citation Information
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