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CN107929129A - A kind of preparation method of pure natural fleece-flower root shampoo - Google Patents

A kind of preparation method of pure natural fleece-flower root shampoo Download PDF

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CN107929129A
CN107929129A CN201711282438.3A CN201711282438A CN107929129A CN 107929129 A CN107929129 A CN 107929129A CN 201711282438 A CN201711282438 A CN 201711282438A CN 107929129 A CN107929129 A CN 107929129A
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eluent
extract
under reduced
reduced pressure
shampoo
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刘成有
刘杰凤
刘韩
尹爱国
韩寒冰
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Guangdong University of Petrochemical Technology
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/35Ketones, e.g. benzophenone
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60Sugars; Derivatives thereof
    • A61K8/602Glycosides, e.g. rutin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/63Steroids; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q17/00Barrier preparations; Preparations brought into direct contact with the skin for affording protection against external influences, e.g. sunlight, X-rays or other harmful rays, corrosive materials, bacteria or insect stings
    • A61Q17/005Antimicrobial preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/006Antidandruff preparations
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/02Preparations for cleaning the hair
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00Preparations for care of the hair
    • A61Q5/12Preparations containing hair conditioners
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q7/00Preparations for affecting hair growth
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

本发明涉及一种纯天然何首乌洗发液的制备方法,该方法是分别将油茶饼粕、皂荚、何首乌和生姜进行提取,然后将它们的提取液按一定比例充分混合,加入0.01~0.05%的防腐剂山莉酸钾,搅拌均匀得洗发液。本发明产品健康环保,既有强力的清洁和抑菌作用,又可以起到止痒、去屑和乌发的功效。The invention relates to a preparation method of pure natural Polygonum multiflorum shampoo. The method is to extract oil tea cake, acacia, Polygonum multiflorum and ginger respectively, then fully mix their extracts in a certain proportion, and add 0.01-0.05% of preservative potassium behenate, and stir evenly to obtain a shampoo. The product of the invention is healthy and environment-friendly, has powerful cleaning and antibacterial effects, and can also play the effects of relieving itching, removing dandruff and blackening hair.

Description

一种纯天然何首乌洗发液的制备方法A kind of preparation method of pure natural Polygonum multiflorum shampoo

技术领域technical field

本发明属于化妆品技术领域,具体地说,是涉及一种源自植物的洗发液及其制备方法。The invention belongs to the technical field of cosmetics, and in particular relates to a plant-derived shampoo and a preparation method thereof.

背景技术Background technique

伴随着人们生活水平的提高,对绿色、低碳环保、节能的意识也越来越强,对洗发液的质量及效果也在逐步提高;人们对洗发液不仅仅停留在去污去垢的层面上,如何在绿色、低碳环保的基础上,注重对头发要有保健、保养等功效,如黑发,治疗头油、脱发、断发等功能。目前,市场上名目繁多的洗发液中的化学成分,对脱发及保养头发等有很大的差异,大多数的洗发水中或多或少会含有化工原料,这些化工原料虽然能起到基本的除污去屑作用,但是仍然会对头发起到一定的副作用,并且在加工过程中会产生不利于环保的废水废渣。随着生活水平的不断提高,人们追求健康的意识也随之增强,在满足最基本的洗发需求之外,更注重对发质的养护,更倾向于使用能够健康洗发去屑的洗发液。头皮上的头屑是真菌在头皮上大量繁殖引起头皮角质层的过度增生,从而促使角质层细胞以白色或灰色鳞屑的形式脱落,如能够提供一种既能够有效的抑制真菌,又能同时养发护发的中药洗发水是未来人们追求的产品,也是技术人员创新的要点。With the improvement of people's living standards, people's awareness of green, low-carbon environmental protection, and energy saving is becoming stronger and stronger, and the quality and effect of shampoo are also gradually improving; people's shampoo is not only limited to decontamination and descaling On the level of green, low-carbon and environmental protection, how to pay attention to the functions of health care and maintenance of hair, such as black hair, treatment of scalp oil, hair loss, hair breakage and other functions. At present, the chemical ingredients in various shampoos on the market have great differences in hair loss and hair maintenance. Most shampoos contain more or less chemical raw materials. Although these chemical raw materials can play a basic role It has the decontamination and anti-dandruff effect, but it still has certain side effects on the hair, and waste water and waste residues that are not conducive to environmental protection will be produced during the processing. With the continuous improvement of living standards, people's awareness of pursuing health has also increased. In addition to meeting the most basic shampoo needs, they pay more attention to the maintenance of hair quality and tend to use shampoos that can wash hair healthy and dandruff. liquid. Dandruff on the scalp is caused by the excessive proliferation of fungus on the scalp causing the stratum corneum of the scalp, thereby prompting the stratum corneum cells to fall off in the form of white or gray scales. Chinese medicine shampoo for hair care is the product that people will pursue in the future, and it is also the key point for technicians to innovate.

油茶饼粕含茶皂素约13%,茶皂素是一类醣甙化合物,是一种优良的天然非离子表面活性剂,具有乳化、分散、稳泡等多种表面活性,同时具有杀菌、杀虫、溶血等方面的作用。过去,人们直接利用油茶饼粕粉碎泡水过滤后洗发,去污效果好,头发乌黑油亮。Camellia oleifera cake contains about 13% tea saponin. Tea saponin is a kind of glycoside compound and an excellent natural nonionic surfactant. Insecticide, hemolysis and other aspects of the role. In the past, people directly used camellia oleifera cake to be crushed, soaked in water and filtered to wash their hair. The decontamination effect is good, and the hair is black and shiny.

皂荚中含三萜皂甙(皂荚甙、皂荚皂甙)、鞣质、蜡醇、廿九烷、豆甾醇、谷甾醇等,皂荚中所含有的皂苷素是三萜烯类和低聚糖,是天然表面活性剂,去头油,治疗脂溢性脱发、脂溢性皮炎,有抗菌消炎作用,长期使用能促进头发黑色素沉淀,使头发蓬松柔软,乌黑富有光泽。Acacia contains triterpene saponins (saponin, acacia saponin), tannin, wax alcohol, nonacane, stigmasterol, sitosterol, etc. The saponins contained in acacia are triterpenes and oligosaccharides, which are natural Surfactant, hair oil removal, treatment of seborrheic alopecia, seborrheic dermatitis, antibacterial and anti-inflammatory effects, long-term use can promote hair melanin precipitation, make hair fluffy, soft, black and shiny.

何首乌是天然养发护发的植物,解毒、止痒、乌发养发为一体,长期使用可增强发根的免疫功能,促进血液循环,能充分滋润发根及毛囊深处,对于断发有很好的改善作用,并令发质柔软,富有弹性。Polygonum multiflorum is a natural hair care plant that detoxifies, relieves itching, and nourishes hair. Long-term use can enhance the immune function of hair roots, promote blood circulation, and fully moisturize hair roots and hair follicles. It is effective for hair loss. Very good improvement effect, and make the hair soft and elastic.

生姜,能有效起到杀菌、消炎、活血的作用,能使皮下血管得以扩充,促进血液循环,加快新陈代谢,对于长期使用,对头皮搔痒及脂溢性皮炎起到很好的治疗效果,同时还能促进毛囊再生头发,经常用热姜水洗头,对秃头亦有一定治疗效果。Ginger can effectively sterilize, reduce inflammation, and activate blood. It can expand subcutaneous blood vessels, promote blood circulation, and accelerate metabolism. For long-term use, it has a good therapeutic effect on scalp itching and seborrheic dermatitis. It can promote hair follicles to regenerate hair, often wash your hair with hot ginger water, and it also has a certain therapeutic effect on baldness.

发明内容Contents of the invention

本发明的目的在于提供一种纯天然何首乌洗发液的制备方法,以解决上述背景技术中提出的问题。The object of the present invention is to provide a kind of preparation method of pure natural Radix Polygoni Multiflori shampoo, to solve the problem proposed in the above-mentioned background technology.

为实现上述目的,本发明提供如下技术方案:To achieve the above object, the present invention provides the following technical solutions:

一种纯天然何首乌洗发液的制备方法,该方法包括如下步骤:A preparation method of pure natural Polygonum multiflorum shampoo, the method comprises the steps of:

步骤(1):将油茶饼粕150~200g粉碎,过40~60目筛,用沸水湿样均匀装入直径为5~6cm的玻璃层析柱中柱中浸泡60~90 min,再用沸水洗脱,洗脱液流速600~900 mL/h,收集洗脱液900~1200 mL,减压浓缩至600~800 mL;Step (1): Crush 150-200g of Camellia oleifera cake, pass through a 40-60 mesh sieve, put the wet sample in boiling water evenly into a glass chromatography column with a diameter of 5-6cm, soak for 60-90 minutes, and then use boiling water For elution, the flow rate of the eluent is 600-900 mL/h, the eluate is collected at 900-1200 mL, and concentrated under reduced pressure to 600-800 mL;

以上所述用沸水提取洗脱是因为油茶饼粕中茶皂素是一种优良的天然非离子表面活性剂,易溶于水,尤其热水;The above-mentioned extraction and elution with boiling water is because the tea saponin in the camellia oleifera cake is a kind of excellent natural non-ionic surfactant, which is easily soluble in water, especially hot water;

以上所述用柱层析法提取洗脱,溶剂从柱上端的物料向下端移动,在层析柱的下端收集提取液。As mentioned above, column chromatography is used for extraction and elution, the solvent moves from the material at the upper end of the column to the lower end, and the extract is collected at the lower end of the column.

步骤(2):将皂荚150~200g粉碎,过40~60目筛,提取和洗脱方法同步骤(1),收集洗脱液900~1200 mL,减压浓缩至600~800 mL;Step (2): Grind 150-200 g of acacia, pass through a 40-60 mesh sieve, use the same extraction and elution methods as in step (1), collect 900-1200 mL of the eluent, and concentrate under reduced pressure to 600-800 mL;

以上所述用沸水提取洗脱是因为皂荚中皂苷是一种优良的天然非离子表面活性剂,易溶于水,尤其热水;The above-mentioned extraction and elution with boiling water is because saponin in saponins is a kind of excellent natural nonionic surfactant, which is easily soluble in water, especially hot water;

以上所述用柱层析法提取洗脱,溶剂从柱上端的物料向下端移动,在层析柱的下端收集提取液。As mentioned above, column chromatography is used for extraction and elution, the solvent moves from the material at the upper end of the column to the lower end, and the extract is collected at the lower end of the column.

步骤(3):将何首乌150~200g粉碎,过40~60目筛,用30~50%乙醇溶液(v/v)湿样均匀装入直径为5~6 cm的玻璃层析柱中,柱中浸泡60~90 min,用相同浓度乙醇溶液洗脱,洗脱液流速600~900 mL/h,收集洗脱液900~1200 mL,减压浓缩至600~800 mL;Step (3): Crush 150-200 g of Polygonum multiflorum, pass through a 40-60 mesh sieve, and evenly load the wet sample with 30-50% ethanol solution (v/v) into a glass chromatography column with a diameter of 5-6 cm. Soak in water for 60-90 min, elute with the same concentration of ethanol solution, the flow rate of eluent is 600-900 mL/h, collect 900-1200 mL of eluate, and concentrate under reduced pressure to 600-800 mL;

以上所述用30%乙醇溶液是因为何首乌中二苯乙烯苷和蒽醌等活性成分易溶于乙醇溶液;The above-mentioned use of 30% ethanol solution is because the active ingredients such as stilbene glycosides and anthraquinone in Polygonum multiflorum are easily soluble in ethanol solution;

以上所述收集的洗脱液要减压浓缩主要是为了移去提取液的乙醇成分;The eluent collected above will be concentrated under reduced pressure mainly in order to remove the ethanol component of the extract;

步骤(4):将生姜切片晒干,烘干,取20~50g粉碎,过40~60目筛,用40~60%乙醇(v/v)湿样均匀装入直径2~3 cm的玻璃层析柱中,柱中浸泡60~90min,再用相同浓度乙醇溶液洗脱,洗脱液流速200~300 mL/h,收集洗脱液100~250 mL,减压浓缩60~150 mL;Step (4): Dry the ginger slices in the sun, dry them, take 20-50g and crush them, pass through a 40-60 mesh sieve, and evenly fill the wet sample with 40-60% ethanol (v/v) into a glass with a diameter of 2-3 cm In the chromatography column, soak in the column for 60-90min, then elute with ethanol solution of the same concentration, the flow rate of the eluent is 200-300 mL/h, collect 100-250 mL of the eluent, and concentrate under reduced pressure for 60-150 mL;

以上所述用40~60%乙醇溶液洗脱是因为生姜中的姜辣素,即姜酚,溶于乙醇溶液,难溶于水;The above-mentioned elution with 40-60% ethanol solution is because the gingerol in ginger, i.e. gingerol, is soluble in ethanol solution and hardly soluble in water;

以上所述收集的洗脱液要减压浓缩主要是为了移去提取液的乙醇成分;The eluent collected above will be concentrated under reduced pressure mainly in order to remove the ethanol component of the extract;

步骤(5):将步骤(1)、步骤(2)、步骤(3)和(4)的浓缩液充分混合,每隔1~2 小时搅拌一次,一共搅拌5次,再进行沉淀和过滤;Step (5): Thoroughly mix the concentrated solution of step (1), step (2), step (3) and (4), stir once every 1 to 2 hours, stir 5 times in total, and then precipitate and filter;

步骤(6):将步骤(5)混合滤液与0.01~0.05%的防腐剂山莉酸钾充分混合,得本发明的纯天然何首乌洗发液。Step (6): Fully mix the mixed filtrate of step (5) with 0.01-0.05% preservative potassium behenate to obtain the pure natural Polygonum multiflorum shampoo of the present invention.

本发明的优点一: 本发明充分利用油茶饼粕的茶皂素、皂荚皂苷等表面活性剂清洁功能、抑菌作用,何首乌的二苯乙烯苷清除自由基、延缓衰老、黑发和护发作用,生姜的姜辣素的杀菌、消炎、活血的作用,纯天然植物制作提取液,来源简单方便,配方温和无刺激性;茶皂素和三萜皂甙具有起泡和清洁作用,泡沫丰富,手感细腻,去污力强,为天然无公害洗发液,同时具有抑菌、去屑、防脱、滋润皮肤的作用。本发明的优点二、以上所述柱层析法提取洗脱,溶剂从柱上端的物料向下端移动,溶剂与物料的吸附与解吸附中,大大增加了溶剂与物料的接触面积,且提取液是单方向向下移动,收集洗脱液为物料5倍(v/g)时,目标成分提取率达到90%以上,溶剂用量少,提取率高、成本低和绿色环保等。Advantage 1 of the present invention: The present invention makes full use of the cleaning function and antibacterial effect of surfactants such as tea saponin and saponin of camellia oleifera cake, and the stilbene glycosides of Polygonum multiflorum have the functions of scavenging free radicals, delaying aging, black hair and hair care , gingerol of ginger has the functions of sterilization, anti-inflammation, and blood circulation. The extract is made of pure natural plants. The source is simple and convenient, and the formula is mild and non-irritating; tea saponin and triterpene saponins have foaming and cleaning effects, rich foam, and feel Delicate and strong in detergency, it is a natural pollution-free shampoo, which also has the functions of antibacterial, anti-dandruff, anti-shedding and moisturizing the skin. Advantage 2 of the present invention, the above-mentioned column chromatography extraction and elution, the solvent moves from the material at the upper end of the column to the lower end, and in the adsorption and desorption of the solvent and the material, the contact area between the solvent and the material is greatly increased, and the extraction liquid It moves downward in one direction, and when the collected eluent is 5 times (v/g) of the material, the extraction rate of the target component reaches more than 90%, the amount of solvent is less, the extraction rate is high, the cost is low, and it is environmentally friendly.

具体实施方式Detailed ways

下面将结合本发明实施例对本发明的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Apparently, the described embodiments are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.

实施例1Example 1

步骤(1):将新鲜刚压榨的油茶饼粕150g粉碎,过40目筛,用沸水湿样均匀装入直径为5cm的玻璃层析柱中,柱中浸泡60 min,沸水洗脱,洗脱液流速600 mL/h,收集洗脱液900 mL,减压浓缩至600 mL;Step (1): Crush 150g of freshly squeezed Camellia oleifera cake, pass through a 40-mesh sieve, put the wet sample in boiling water evenly into a glass chromatography column with a diameter of 5cm, soak in the column for 60 minutes, and elute with boiling water. The liquid flow rate was 600 mL/h, and 900 mL of the eluent was collected, concentrated to 600 mL under reduced pressure;

步骤(2):将新鲜皂荚晒干或烘干,称取200g,粉碎,过40目筛,用沸水湿样均匀装入直径为 6 cm的玻璃层析柱中,柱中浸泡90 min,沸水洗脱,洗脱液流速800 mL/h,收集洗脱液1200 mL;Step (2): Sun-dry or dry fresh acacia, weigh 200g, crush, pass through a 40-mesh sieve, put the wet sample in boiling water evenly into a glass chromatography column with a diameter of 6 cm, soak in the column for 90 min, boil water For elution, the eluent flow rate is 800 mL/h, and the eluent is collected at 1200 mL;

步骤(3):将生何首乌切片,烘干,取150 g粉碎,过40目筛,用30%乙醇(v/v)湿样均匀装入直径为5 cm的玻璃层析柱中,柱中浸泡60 min,再用30%乙醇(v/v)洗脱,洗脱液流速700mL/h,收集洗脱液600 mL,减压浓缩420 mL;Step (3): Slice the raw Polygonum multiflorum, dry it, take 150 g and crush it, pass it through a 40-mesh sieve, put the wet sample with 30% ethanol (v/v) evenly into a glass chromatography column with a diameter of 5 cm, and put it in the column. Soak for 60 min, then elute with 30% ethanol (v/v), the eluent flow rate is 700mL/h, collect 600 mL of eluent, and concentrate under reduced pressure to 420 mL;

步骤(4):将生姜切片晒干,烘干,取20 g粉碎,过40 目筛,用40%乙醇(v/v)湿样均匀装入直径为2 cm的玻璃层析柱中,柱中浸泡60 min,用相同浓度乙醇溶液洗脱,洗脱液流速200 mL/h,收集洗脱液100 mL,减压浓缩至60 mL;Step (4): Dried the ginger slices in the sun, dried them, took 20 g and crushed them, passed through a 40-mesh sieve, and evenly loaded the wet sample with 40% ethanol (v/v) into a glass chromatography column with a diameter of 2 cm. Soak in water for 60 min, elute with the same concentration of ethanol solution, the flow rate of the eluent is 200 mL/h, collect 100 mL of the eluate, and concentrate it to 60 mL under reduced pressure;

步骤(5):将步骤(1)的提取液、步骤(2)的提取液、步骤(3)提取液和步骤(4)的提取液充分混合,每隔1小时搅拌一次,一共搅拌5次,再进行沉淀和过滤;Step (5): Fully mix the extract of step (1), the extract of step (2), the extract of step (3) and the extract of step (4), stir once every 1 hour, and stir 5 times in total , and then precipitate and filter;

步骤(6)将步骤(5)滤液与0.015%的防腐剂山莉酸钾充分混合,得本发明的纯天然何首乌洗发液。Step (6) fully mix the filtrate of step (5) with 0.015% preservative potassium behenate to obtain the pure natural Polygonum multiflorum shampoo of the present invention.

实施例2Example 2

步骤(1):将新鲜刚压榨的油茶饼粕200g粉碎,过60目筛,用沸水湿样均匀装入直径为6cm的玻璃层析柱中,柱中浸泡90 min,沸水洗脱,洗脱液流速800 mL/h,收集洗脱液1200mL,减压浓缩至800 mL;Step (1): Crush 200g of freshly squeezed Camellia oleifera cake, pass through a 60-mesh sieve, put the wet sample in boiling water into a glass chromatography column with a diameter of 6cm, soak in the column for 90 minutes, and elute with boiling water. The liquid flow rate was 800 mL/h, and the eluate was collected at 1200 mL, concentrated under reduced pressure to 800 mL;

步骤(2):将新鲜皂荚晒干或烘干,称取150 g,粉碎,过 60目筛,用沸水湿样均匀装入直径为5 cm的玻璃层析柱中,柱中浸泡80 min,沸水洗脱,洗脱液流速800 mL/h,收集洗脱液1200 mL,减压浓缩至800 mL;Step (2): Sun-dry or dry fresh acacia, weigh 150 g, crush, pass through a 60-mesh sieve, put the wet sample in boiling water evenly into a glass chromatography column with a diameter of 5 cm, soak in the column for 80 min, Elute with boiling water, the eluent flow rate is 800 mL/h, collect 1200 mL of eluent, and concentrate under reduced pressure to 800 mL;

步骤(3):将生何首乌切片,烘干,取200g粉碎,过50目筛,用50%乙醇(v/v)湿样均匀装入直径为5 cm的玻璃层析柱中,柱中浸泡90 min,用相同乙醇溶液洗脱,洗脱液流速700mL/h,收集洗脱液900 mL,减压浓缩至600 mL;Step (3): Slice the raw Polygonum multiflorum, dry it, take 200g and crush it, pass it through a 50-mesh sieve, put the wet sample with 50% ethanol (v/v) evenly into a glass chromatography column with a diameter of 5 cm, and soak in the column 90 min, elute with the same ethanol solution, the flow rate of the eluent is 700mL/h, collect 900 mL of the eluent, and concentrate it to 600 mL under reduced pressure;

步骤(4):将生姜切片晒干,烘干,取50g粉碎,过60目筛,用60%乙醇(v/v)湿样均匀装入直径3 cm的玻璃层析柱中,柱中浸泡90min,再用相同浓度乙醇溶液洗脱,洗脱液流速300mL/h,收集洗脱液250 mL,减压浓缩150 mL; Step (4): Dry ginger slices in the sun, dry them, take 50g and crush them, pass through a 60-mesh sieve, put the wet sample with 60% ethanol (v/v) evenly into a glass chromatography column with a diameter of 3 cm, and soak in the column 90min, then elute with the same concentration of ethanol solution, the flow rate of the eluent is 300mL/h, collect 250mL of the eluent, and concentrate under reduced pressure to 150mL;

步骤(5):将步骤(1)的提取液、步骤(2)的提取液、步骤(3)提取液和步骤(4)的提取液充分混合,每隔2 小时搅拌一次,一共搅拌5次,再进行沉淀和过滤; Step (5): Fully mix the extract of step (1), the extract of step (2), the extract of step (3) and the extract of step (4), stir once every 2 hours, and stir 5 times in total , and then precipitate and filter;

步骤(6)将步骤(5)滤液与0.05%的防腐剂山莉酸钾充分混合,得本发明的纯天然何首乌洗发液。Step (6) fully mix the filtrate of step (5) with 0.05% preservative potassium behenate to obtain the pure natural Polygonum multiflorum shampoo of the present invention.

实施例3Example 3

步骤(1):将新鲜刚压榨的油茶饼粕180 g粉碎,过50目筛,用沸水湿样均匀装入直径为5.5 cm的玻璃层析柱中,柱中浸泡70 min,沸水洗脱,洗脱液流速800 mL/h,收集洗脱液1000 mL;Step (1): crush 180 g of freshly squeezed Camellia oleifera cake, pass through a 50-mesh sieve, put the wet sample in boiling water into a glass chromatography column with a diameter of 5.5 cm, soak in the column for 70 min, and elute with boiling water. The flow rate of eluent is 800 mL/h, and 1000 mL of eluent is collected;

步骤(2):将新鲜皂荚晒干或烘干,称取180g,粉碎,过50目筛,用沸水湿样均匀装入直径为5.5 cm的玻璃层析柱中,柱中浸泡80 min,沸水洗脱,洗脱液流速700 mL/h,收集洗脱液1000 mL,减压浓缩至700 mL;Step (2): Sun-dry or dry the fresh saponins, weigh 180g, crush, pass through a 50-mesh sieve, put the wet sample in boiling water evenly into a glass chromatography column with a diameter of 5.5 cm, soak the column for 80 min, boil water For elution, the flow rate of the eluent is 700 mL/h, and 1000 mL of the eluent is collected and concentrated to 700 mL under reduced pressure;

步骤(3):将生何首乌切片,烘干,取180 g粉碎,过50目筛,用40%乙醇(v/v)湿样均匀装入直径为5.5 cm的玻璃层析柱中,柱中浸泡60 min,用相同乙醇溶液洗脱,洗脱液流速700mL/h,收集洗脱液1000 mL,减压浓缩至700 mL;Step (3): Slice the raw Radix Polygoni Multiflori, dry it, take 180 g and crush it, pass it through a 50-mesh sieve, put the wet sample with 40% ethanol (v/v) evenly into a glass chromatography column with a diameter of 5.5 cm, and put it in the column. Soak for 60 min, elute with the same ethanol solution, the flow rate of the eluent is 700mL/h, collect 1000 mL of the eluate, and concentrate it to 700 mL under reduced pressure;

步骤(4):将生姜切片晒干,烘干,取30 g粉碎,过50目筛,用40%乙醇(v/v)湿样均匀装入直径为2.5 cm的玻璃层析柱中,柱中浸泡80 min,再用相同浓度乙醇溶液洗脱,洗脱液流速250 mL/h,收集洗脱液200 mL,减压浓缩100 mL;Step (4): Dried the ginger slices in the sun, dried them, took 30 g and crushed them, passed through a 50-mesh sieve, and evenly loaded the wet sample with 40% ethanol (v/v) into a glass chromatography column with a diameter of 2.5 cm. Soak in water for 80 min, then elute with the same concentration of ethanol solution, the flow rate of eluent is 250 mL/h, collect 200 mL of eluate, and concentrate under reduced pressure to 100 mL;

步骤(5):将步骤(1)的提取液、步骤(2)的提取液、步骤(3)提取液和步骤(4)的提取液充分混合,每隔1.5 小时搅拌一次,一共搅拌5次,再进行沉淀和过滤;Step (5): Fully mix the extract of step (1), the extract of step (2), the extract of step (3) and the extract of step (4), stir once every 1.5 hours, a total of 5 times , and then precipitate and filter;

步骤(6)将步骤(5)滤液与0.03%的防腐剂山莉酸钾充分混合,得本发明的纯天然何首乌洗发液。Step (6) Fully mix the filtrate of step (5) with 0.03% preservative potassium behenate to obtain the pure natural Polygonum multiflorum shampoo of the present invention.

对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。It will be apparent to those skilled in the art that the invention is not limited to the details of the above-described exemplary embodiments, but that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Accordingly, the embodiments should be regarded in all points of view as exemplary and not restrictive, the scope of the invention being defined by the appended claims rather than the foregoing description, and it is therefore intended that the scope of the invention be defined by the appended claims rather than by the foregoing description. All changes within the meaning and range of equivalents of the elements are embraced in the present invention.

Claims (1)

1.一种纯天然何首乌洗发液的制备方法,其特征在于:该方法包括如下步骤:1. a preparation method of pure natural Radix Polygoni Multiflori shampoo, is characterized in that: the method comprises the steps: (1)将油茶饼粕150~200g粉碎,过40~60目筛,用沸水湿样均匀装入直径为5~6 cm的玻璃层析柱中,柱中浸泡60~90 min,再用沸水洗脱,洗脱液流速600~900 mL/h,收集洗脱液900~1200 mL,减压浓缩至600~800 mL;(1) Crush 150-200g of Camellia oleifera cake, pass through a 40-60 mesh sieve, put the wet sample in boiling water evenly into a glass chromatography column with a diameter of 5-6 cm, soak in the column for 60-90 min, and then wash it with boiling water For elution, the flow rate of the eluent is 600-900 mL/h, the eluate is collected at 900-1200 mL, and concentrated under reduced pressure to 600-800 mL; (2)将皂荚150~200g粉碎,过40~60目筛,提取和洗脱方法同步骤(1),收集洗脱液900~1200 mL,减压浓缩至600~800 mL;(2) Crush 150-200 g of acacia, pass through a 40-60 mesh sieve, extract and elute as in step (1), collect 900-1200 mL of the eluate, and concentrate under reduced pressure to 600-800 mL; (3)将何首乌150~200g粉碎,过40~60目筛,用30~50%乙醇溶液湿样均匀装入直径为5~6 cm的玻璃层析柱中,柱中浸泡60~90 min,用相同浓度乙醇溶液洗脱,洗脱液流速600~900 mL/h,收集洗脱液900~1200 mL,减压浓缩至600~800 mL;(3) Crush 150-200 g of Radix Polygoni Multiflori, pass through a 40-60 mesh sieve, and evenly load the wet sample with 30-50% ethanol solution into a glass chromatography column with a diameter of 5-6 cm, soak in the column for 60-90 min, Elute with the same concentration of ethanol solution, the flow rate of the eluent is 600-900 mL/h, collect 900-1200 mL of the eluent, and concentrate under reduced pressure to 600-800 mL; (4)将生姜切片晒干或烘干,取20~50g粉碎,过40~60目筛,用40~60%乙醇湿样均匀装入直径2~3 cm的玻璃层析柱中,柱中浸泡60~90min,再用相同浓度乙醇溶液洗脱,洗脱液流速200~300 mL/h,收集洗脱液100~250 mL,减压浓缩60~150 mL;(4) Sun-dry or dry the ginger slices, take 20-50g and crush them, pass through a 40-60 mesh sieve, and evenly load the wet sample with 40-60% ethanol into a glass chromatography column with a diameter of 2-3 cm. Soak for 60-90 minutes, then elute with the same concentration of ethanol solution, the flow rate of the eluent is 200-300 mL/h, collect 100-250 mL of the eluent, and concentrate under reduced pressure for 60-150 mL; (5)将步骤(1)的提取液、步骤(2)的提取液、步骤(3)提取液和步骤(4)的提取液充分混合,每隔1~2 小时搅拌一次,一共搅拌5次,再进行沉淀和过滤;(5) Fully mix the extract of step (1), the extract of step (2), the extract of step (3) and the extract of step (4), stir once every 1 to 2 hours, and stir 5 times in total , and then precipitate and filter; (6)将步骤(5)滤液与0.01~0.05%的防腐剂山莉酸钾充分混合,得本发明的纯天然何首乌洗发液。(6) Fully mix the filtrate of step (5) with 0.01-0.05% preservative potassium behenate to obtain the pure natural Polygonum multiflorum shampoo of the present invention.
CN201711282438.3A 2017-12-07 2017-12-07 A kind of preparation method of pure natural fleece-flower root shampoo Pending CN107929129A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108524393A (en) * 2018-06-11 2018-09-14 广西科技大学 A kind of ginger shampoo and preparation method thereof
CN108653097A (en) * 2018-07-11 2018-10-16 贵州捷易康植化有限公司 A kind of preparation method of pure natural gleditsia sinensis shampoo
CN111419771A (en) * 2020-05-08 2020-07-17 达州市俊颜企业管理咨询有限公司 Tea bran hair nourishing composition, preparation and hair nourishing method
CN113693983A (en) * 2021-09-09 2021-11-26 湖南科技学院 Oil-tea cake shampoo and preparation method thereof

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108524393A (en) * 2018-06-11 2018-09-14 广西科技大学 A kind of ginger shampoo and preparation method thereof
CN108524393B (en) * 2018-06-11 2021-04-27 广西科技大学 Ginger shampoo and preparation method thereof
CN108653097A (en) * 2018-07-11 2018-10-16 贵州捷易康植化有限公司 A kind of preparation method of pure natural gleditsia sinensis shampoo
CN111419771A (en) * 2020-05-08 2020-07-17 达州市俊颜企业管理咨询有限公司 Tea bran hair nourishing composition, preparation and hair nourishing method
CN113693983A (en) * 2021-09-09 2021-11-26 湖南科技学院 Oil-tea cake shampoo and preparation method thereof

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