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CN107857792A - A kind of extracting method of gleditschiasaponin - Google Patents

A kind of extracting method of gleditschiasaponin Download PDF

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Publication number
CN107857792A
CN107857792A CN201711083423.4A CN201711083423A CN107857792A CN 107857792 A CN107857792 A CN 107857792A CN 201711083423 A CN201711083423 A CN 201711083423A CN 107857792 A CN107857792 A CN 107857792A
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saponins
gleditschiasaponin
extraction
water
magnetization
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梅杰
张许昌
钱军
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Shenzhen Orchid Pavilion Science And Technology Co Ltd
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Shenzhen Orchid Pavilion Science And Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J63/00Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
    • C07J63/008Expansion of ring D by one atom, e.g. D homo steroids
    • 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
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/10Washing or bathing 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

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  • General Health & Medical Sciences (AREA)
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Abstract

A kind of extracting method of gleditschiasaponin.The present invention provides one kind and adopts water as solvent, with reference to ultrasound-assisted extraction technology and magnetic water treatment device, expeditiously to extract the method for the natural surfactant gleditschiasaponin in Chinese honey locust, this method is safe and environment-friendly, it is quick, inexpensive, suitable for commercial Application, and the gleditschiasaponin extract solution obtained may be directly applied in personal care product and household care product without purifying concentration.Wherein the power of ultrasonic wave is 300 500W, and the Ultrasonic Radiation time is 6 10 minutes, and Extracting temperature is 80 90 DEG C, and the weight ratio of Chinese honey locust and water is 1:2~1:4, extract 1~3 hour.

Description

一种皂荚皂甙的提取方法A kind of extraction method of saponin

技术领域technical field

本发明涉及一种皂荚皂甙的提取方法,尤其是使用水作为溶剂提取皂荚皂甙的方法。The invention relates to a method for extracting saponins, in particular to a method for extracting saponins using water as a solvent.

背景技术Background technique

皂荚树(Gleditsia Linn)是豆科植物,苏木亚科,共有约十二种。常见的有如下六种:皂荚树(Gleditsia sinensis Lam)、肥皂荚树(Gymnoclabrs chinensis)、山皂荚树(G.melanacantha)、野皂荚树(Gleditisia heterophylla)、绒毛皂荚树(G.vestita chunex How)、日本皂荚树(Gleditsia.japonica)。其中皂荚树(Gleditsia sinensis Lam)(又称中国皂荚)是我国的特有品种,生长分布区域约占我国国土面积的一半。皂荚树为落叶乔木,树干挺拔,树叶茂盛,生长寿命可达600年,产果期长达200年。Honey locust tree (Gleditsia Linn) is a leguminous plant, and there are about twelve species in the subfamily Hematoxylin. There are six common species: Gleditsia sinensis Lam, Gymnoclabrs chinensis, G. melanacantha, Gleditisia heterophylla, G. vestita chunex How , Japanese honey locust tree (Gleditsia. japonica). Among them, Gleditsia sinensis Lam (also known as Chinese honey locust) is a unique species in my country, and its growth and distribution area accounts for about half of my country's land area. Honey locust tree is a deciduous tree with a tall and straight trunk and lush leaves. Its growth life can reach 600 years and its fruit-producing period can reach 200 years.

皂荚树全身都可以利用。树干木质良好,耐腐蚀耐磨损,是极好的工业木材。皂角刺富含黄酮、皂甙、氨基酸、酚类等药用成分,是中华传统中药材,是治疗乳腺癌、肺癌等多种疾病的配伍中草药。猪牙皂是皂荚树受到外伤时结出的畸形小荚果,具有祛痰开窍和散结消肿的功效,是中国药典收藏的中药材之一。皂荚果包括皂荚种子和皂荚。皂荚种子可以提取出皂荚胶,皂荚胶可以广泛应用于化妆品、石油开采、食品医药、印染纺织、选矿采矿等行业作为增稠剂、稳定剂、粘合剂等。皂荚中含有大量的天然表面活性剂皂荚皂甙,是最古老的表面活性剂之一,早在古代就被人们用来洗涤衣物、毛发、裘皮等。此外,皂荚皂甙还具有杀虫、祛痰、开窍、搜风等功效。The whole body of the honey locust tree can be used. The trunk has good wood, corrosion and wear resistance, and is an excellent industrial wood. Saponin thorn is rich in flavonoids, saponins, amino acids, phenols and other medicinal ingredients. It is a traditional Chinese medicinal material and a compatible Chinese herbal medicine for the treatment of breast cancer, lung cancer and other diseases. Pig tooth soap is a deformed small pod produced by the acacia tree when it is traumatized. It has the effects of eliminating phlegm and resuscitation, dispelling stagnation and reducing swelling. It is one of the traditional Chinese medicines collected in the Chinese Pharmacopoeia. Honey locust fruit includes honey locust seeds and honey locusts. Acacia seeds can extract acacia gum, which can be widely used in cosmetics, petroleum exploration, food and medicine, printing and dyeing textiles, mineral processing and mining and other industries as thickeners, stabilizers, adhesives, etc. Acacia saponin contains a large amount of natural surfactant saponin, which is one of the oldest surfactants and has been used by people to wash clothes, hair, fur, etc. in ancient times. In addition, acacia saponins also have the effects of killing insects, eliminating phlegm, resuscitation, and searching wind.

皂荚树的根系发达而且抗旱节水,是非常理想的生态树种,目前世界各国与中国都在大量种植皂荚树,作为农田、农场防护林、野生动植物保护林,城乡景观林和水土保持林等。但是大量的皂荚资源任其腐烂,没有得到很好的利用,白白浪费了这极其宝贵的天然产物资源。皂荚中富含大量的天然表面活性剂皂荚皂甙,若是将皂荚中的皂荚皂甙提取出来并成功的运用到个人护理及家居护理产品中,这将极大的促进皂荚树的种植及其下游产业链的深层次开发。不仅有益于绿化造林、退耕还林,促进生态经济农业的发展,而且天然优质的植物原料运用于化妆品必将促进化妆品产业的升级换代,造福普通大众。由此可见,皂荚皂甙的工业提取及应用研究,符合现代社会绿色可持续发展的需求。The root system of the acacia tree is developed, and it is drought-resistant and water-saving. It is an ideal ecological tree species. At present, countries all over the world and China are planting acacia trees in large quantities, as farmland, farm shelter forests, wild animal and plant protection forests, urban and rural landscape forests, and soil and water conservation forests. But a large amount of acacia resources are allowed to rot and are not well utilized, wasting this extremely valuable natural product resource in vain. Acacia saponins are rich in a large amount of natural surfactant saponins. If the saponins in acacia are extracted and successfully applied to personal care and home care products, it will greatly promote the planting of acacia trees and its downstream industrial chain in-depth development. Not only is it beneficial to afforestation, returning farmland to forests, and promoting the development of ecological and economic agriculture, but also the application of natural high-quality plant raw materials in cosmetics will definitely promote the upgrading of the cosmetics industry and benefit the general public. It can be seen that the industrial extraction and application research of saponins meet the needs of green and sustainable development in modern society.

皂荚皂甙的分子结构非常复杂,分子结构中既含有亲油基团皂甙元,又包含亲水基团糖和糖醛酸等,皂荚皂甙的分子结构如下式所示。常见的皂甙元为五环三萜类化合物,当R1为H是为齐墩果酸结构,当R1为OH时为刺囊酸结构。皂甙中的糖有葡萄糖、木糖、阿拉伯糖、鼠李糖、半乳糖等,皂甙中的糖醛酸有半乳糖醛酸、葡萄糖醛酸等。The molecular structure of saponins is very complex. The molecular structure contains not only lipophilic group saponin, but also hydrophilic groups such as sugar and uronic acid. The molecular structure of saponins is shown in the following formula. Common saponins are pentacyclic triterpenoids. When R1 is H, it is an oleanolic acid structure, and when R1 is OH, it is a echinocytic acid structure. The sugars in saponins include glucose, xylose, arabinose, rhamnose, galactose, etc., and the uronic acids in saponins include galacturonic acid, glucuronic acid, etc.

皂荚皂甙常用的提取方法有甲醇或乙醇提取法、渗漉法、异丙醇溶解重结晶法、回流提取法、超临界流体萃取法、半仿生提取法、微波辅助萃取法、超高压提取法,等等。但是上述提取方法往往操作繁琐,溶剂使用量大,仪器设备昂贵,不适合大规模工业化操作。Commonly used extraction methods for saponins include methanol or ethanol extraction, percolation, isopropanol dissolution and recrystallization, reflux extraction, supercritical fluid extraction, semi-bionic extraction, microwave-assisted extraction, and ultra-high pressure extraction. and many more. However, the above-mentioned extraction methods are often cumbersome to operate, use a large amount of solvent, and are expensive in equipment, and are not suitable for large-scale industrial operation.

皂荚皂甙的分子量在1600左右,分子中含有较多的羟基、羧基、酯基等极性基团,根据相似相溶原理,皂荚皂甙易溶解于极性溶剂中。目前工业中最常用的极性溶剂有甲醇、乙醇、水,故以上三种溶剂是目前工业中提取皂荚皂甙最适合的溶剂。The molecular weight of saponins is about 1600, and the molecules contain more polar groups such as hydroxyl, carboxyl, and ester groups. According to the principle of similar compatibility, saponins are easily soluble in polar solvents. At present, the most commonly used polar solvents in industry are methanol, ethanol, and water, so the above three solvents are the most suitable solvents for extracting saponins in industry.

李莹桥(山皂荚皂甙的提取工艺及其表面活性剂性能的测定[D].吉林农业大学硕士学位论文,2011)以甲醇为溶剂,对皂荚皂甙的提取方法进行了详尽的研究,结果表明采用75%的甲醇提取1小时,共提取三次,皂荚皂甙的提取率为22.39%。显然该提取方法皂荚皂甙的提取率偏低,77.61%的皂甙仍未提取出来,该提取方案未能充分的利用皂荚资源。再者,甲醇为剧毒化学品,以甲醇为溶剂提取皂荚皂甙,产品中残留的甲醇必将给皂荚皂甙的使用带来安全隐患。Li Yingqiao (The extraction process of saponins and the determination of their surfactant properties [D]. Jilin Agricultural University master's degree thesis, 2011) used methanol as a solvent to study the extraction method of saponins in detail. The results showed that 75 % methanol was extracted for 1 hour and extracted three times in total, and the extraction rate of saponins was 22.39%. Apparently, the extraction rate of saponins in this extraction method is on the low side, and 77.61% of saponins have not been extracted yet. This extraction scheme fails to make full use of saponins resources. Furthermore, methanol is a highly toxic chemical. Using methanol as a solvent to extract saponins, the residual methanol in the product will definitely bring safety hazards to the use of saponins.

张春霞等(天然表面活性剂皂荚皂甙的性能与应用[J].郑州轻工业学院学报,1993,8(2):56-61)采用乙醇为溶剂提取皂荚皂甙,并对其表面活性进行了研究。乙醇属于危险化学品,易燃易爆,而且大量的溶剂消耗以及繁琐的减压蒸馏程序,势必极大的阻碍了皂荚皂甙的工业应用。乙醇提取的皂荚皂甙中会含有较多的脂溶性成分,这些脂溶性会严重的影响皂荚皂甙的泡沫等表面活性剂性能,而且也会加深皂荚皂甙的色泽,不利于皂荚皂甙在个人护理及家居护理用品中的应用。Zhang Chunxia et al. (The performance and application of natural surfactant saponins [J]. Journal of Zhengzhou Institute of Light Industry, 1993, 8 (2): 56-61) used ethanol as a solvent to extract saponins and studied their surface activity. Ethanol is a dangerous chemical, flammable and explosive, and a large amount of solvent consumption and cumbersome vacuum distillation procedures are bound to greatly hinder the industrial application of saponins. Acacia saponin extracted by ethanol will contain more fat-soluble components, which will seriously affect the foam and other surfactant properties of acacia saponin, and will also deepen the color of acacia saponin, which is not conducive to the use of acacia saponin in personal care and household Application in nursing products.

梁静谊等(皂荚皂甙提取工艺研究[J].中国野生植物资源,2003,22(6):58-61)以水为溶剂,对皂荚皂甙的提取工艺进行了正交实验优化研究,实验结果表明,以水为溶剂提取皂荚皂甙的最佳工艺条件为固液比1:10,提取温度45℃,提取时间18小时,提取三次,皂荚皂甙的提取率为90.9%。该工艺的提取时间为54小时(一次提取时间为18小时共提取三次),显然提取时间太过长久。文中采用的皂荚产地为北京,其中皂荚皂甙的含量为32%,按照上述提取工艺则可以推算出该提取液中皂荚皂甙的活性物含量约为1%,如此低的活性物含量显然不适合直接运用于个人护理及家居护理用品工业中。Liang Jingyi et al. (Research on the extraction process of saponins from saponins [J]. China Wild Plant Resources, 2003, 22(6):58-61) used water as solvent to conduct an orthogonal experimental optimization study on the extraction process of saponins from saponins. The experimental results showed that , using water as the solvent to extract saponins, the best process conditions are solid-to-liquid ratio 1:10, extraction temperature 45°C, extraction time 18 hours, extraction three times, the extraction rate of saponins is 90.9%. The extraction time of this process is 54 hours (one extraction time is 18 hours and extracts three times altogether), obviously the extraction time is too long. The place of origin of the saponins used in the paper is Beijing, and the content of saponins is 32%. According to the above extraction process, it can be inferred that the active matter content of saponins in the extract is about 1%. Such a low active matter content is obviously not suitable for direct extraction. Used in personal care and household care products industry.

综上所述,目前皂荚皂甙的提取方法很多,但是往往操作繁琐、溶剂消耗量大、或者根本不适用于大规模工业化生产运用。那么安全、环保、快速、低成本的皂荚皂甙提取方法的建立显得尤为迫切。To sum up, there are many methods for extracting saponins from saponins, but they are often complicated to operate, consume a lot of solvents, or are not suitable for large-scale industrial production at all. So it is particularly urgent to establish a safe, environmentally friendly, fast and low-cost method for extracting saponins from saponins.

发明内容Contents of the invention

本发明采用最丰富廉价的水为溶剂,结合超声波辅助萃取技术和磁化水处理装置,来高效率地提取皂荚中的天然表面活性剂皂荚皂甙,该方法安全、环保、快速、低成本、适于工业应用,获得的皂荚皂甙是优质天然原料,并且获得的皂荚皂甙提取液无需纯化浓缩即可直接应用于个人护理产品和家居护理产品中。The present invention uses the most abundant and cheap water as a solvent, combined with ultrasonic-assisted extraction technology and magnetized water treatment equipment, to efficiently extract the natural surfactant saponins in saponins. The method is safe, environmentally friendly, fast, low-cost, suitable for For industrial applications, the obtained saponin is a high-quality natural raw material, and the obtained saponin extract can be directly applied to personal care products and home care products without purification and concentration.

本发明目的是通过如下技术方案实现的。The object of the present invention is achieved through the following technical solutions.

本发明提供一种皂荚皂甙的提取方法,其使用皂荚作为原料,水作为溶剂,同时使用磁化水处理装置和超声波辅助萃取技术。The invention provides a method for extracting acacia saponin, which uses acacia as a raw material, water as a solvent, and simultaneously uses a magnetized water treatment device and ultrasonic-assisted extraction technology.

磁化水处理技术和超声波辅助萃取技术均为近几十年发展起来的新技术、新科技,本发明将上述两项技术有机的结合起来,运用到萃取皂荚中的皂荚皂甙的方法中,以提高皂荚皂甙的提取率,缩短提取时间,为皂荚皂甙的工业化应用提供可能。Both magnetized water treatment technology and ultrasonic-assisted extraction technology are new technologies and new technologies developed in recent decades. The present invention organically combines the above two technologies and applies them to the method for extracting saponins in saponins to improve The extraction rate of saponins and the shortening of extraction time provide the possibility for the industrial application of saponins.

磁化水处理技术利用磁化水处理装置,请参见附图1,其包括磁化储水室(1)、电机(2)、减速机(3)、传动轴(4)、磁化叶轮(5),所述电机(2)连接所述减速机(3)并设置在所述磁化储水室(1)顶端,所述传动轴(4)连接减速机(3)并设置于磁化储水室(1)内部,所述磁化叶轮(5)连接传动轴(4);The magnetized water treatment technology utilizes a magnetized water treatment device, please refer to accompanying drawing 1, which includes a magnetized water storage chamber (1), a motor (2), a reducer (3), a drive shaft (4), and a magnetized impeller (5). The motor (2) is connected to the reducer (3) and arranged on the top of the magnetized water storage chamber (1), and the transmission shaft (4) is connected to the reducer (3) and arranged on the magnetized water storage chamber (1) Inside, the magnetized impeller (5) is connected to the transmission shaft (4);

优选地,所述磁化储水室(1)下端设置磁化室(12),其中,磁化室(12)内部设置磁铁(6);Preferably, a magnetization chamber (12) is arranged at the lower end of the magnetization water storage chamber (1), wherein a magnet (6) is arranged inside the magnetization chamber (12);

优选地,所述磁化储水室(1)外侧设置夹套(7),夹套(7)一端设置冷水出水口(8),另一端设置冷水进水口(9);Preferably, a jacket (7) is provided outside the magnetized water storage chamber (1), a cold water outlet (8) is arranged at one end of the jacket (7), and a cold water inlet (9) is arranged at the other end;

优选地,所述磁化室(12)内部的磁铁(6)为多个;Preferably, there are multiple magnets (6) inside the magnetization chamber (12);

优选地,所述磁铁(6)为天然磁铁;Preferably, the magnet (6) is a natural magnet;

优选地,所述天然磁铁与所述去离子水的质量比为1:10-20;Preferably, the mass ratio of the natural magnet to the deionized water is 1:10-20;

优选地,所述天然磁铁为Fe3O4;Preferably, the natural magnet is Fe3O4;

优选地,该磁化水处理装置为200L。Preferably, the magnetized water treatment device is 200L.

对于超声波辅助萃取技术来说,超声波的功率和超声波的辐射时间对萃取的效率都有很大的影响。本发明中超声波的功率为300-500W,优选300W;超声波辐射时间为6-10分钟,优选6分钟。For ultrasonic-assisted extraction technology, the power of ultrasonic waves and the radiation time of ultrasonic waves have a great influence on the extraction efficiency. The power of the ultrasonic wave in the present invention is 300-500W, preferably 300W; the ultrasonic radiation time is 6-10 minutes, preferably 6 minutes.

温度对化学反应的速率和化学反应的平衡都有很大的影响。提取的温度较低势必会降低皂荚皂甙在水中的溶解度,提取的速率也会较慢。但是,温度太高可能又会导致皂荚皂甙的部分水解,反而降低提取率。所以皂荚皂甙的提取温度是非常关键的工艺参数。Temperature has a great influence on the rate of chemical reactions and the equilibrium of chemical reactions. The lower extraction temperature will inevitably reduce the solubility of saponins in water, and the extraction rate will be slower. However, if the temperature is too high, it may cause partial hydrolysis of saponin, which reduces the extraction rate. Therefore, the extraction temperature of saponins is a very critical process parameter.

固液比即为皂荚与水的质量比,显然随着水的增加,提取率会相应的提高,但是水的增加会导致最终提取液中皂荚皂甙活性物的浓度降低。目前的个人护理及家居护理行业标准中,洗发水、沐浴露、洗手液、洗衣液、洗洁精的总表面活性剂含量标准最低分别为10%、7%、7%、15%、15%。那么,低含量的皂荚皂甙天然表面活性剂提取液必须浓缩之后才能应用于上述产品中。提取液的浓缩工艺必然会带来能量的消耗和人力成本的增加等不良因素。所以提取工艺中固液比的选择显得十分关键。The solid-to-liquid ratio is the mass ratio of saponins to water. Obviously, with the increase of water, the extraction rate will increase accordingly, but the increase of water will lead to a decrease in the concentration of saponin active substances in the final extract. In the current personal care and home care industry standards, the minimum total surfactant content standards for shampoo, shower gel, hand sanitizer, laundry detergent, and dish soap are 10%, 7%, 7%, 15%, and 15% respectively . Then, the low content saponin natural surfactant extract must be concentrated before it can be used in the above products. The concentration process of the extract will inevitably bring about adverse factors such as energy consumption and increase in labor costs. Therefore, the choice of solid-liquid ratio in the extraction process is very critical.

皂荚皂甙活性成分从皂荚溶解到水溶液中需要穿过皂荚细胞膜、细胞壁等,显然随着时间的延长提取率会相应的提高。但是提取时间太长,一方面由于皂荚皂甙在水溶液中溶解达到饱和,时间延长提取率并不增加,反而是皂荚皂甙部分水解导致提取率降低;另一方面,提取时间的延长会导致工业能耗、人工成本等都会成倍的增加,不利于该项目的工业化。所以,提取时间的选择对皂荚皂甙的提取显得尤为重要。The active ingredients of saponin from saponins need to pass through the cell membrane and cell wall of saponins to be dissolved into the aqueous solution. Obviously, the extraction rate will increase correspondingly with the extension of time. However, the extraction time is too long. On the one hand, because the saponins in the aqueous solution are dissolved and reach saturation, the extraction rate does not increase after a prolonged period of time. On the contrary, the partial hydrolysis of the saponins leads to a decrease in the extraction rate; on the other hand, the prolongation of the extraction time will lead to industrial energy consumption. , labor costs, etc. will increase exponentially, which is not conducive to the industrialization of the project. Therefore, the choice of extraction time is particularly important for the extraction of saponins from saponins.

在本发明中,经实验证实,优选的提取温度为80-90℃,更优选85℃;皂荚与水的重量比为1:2~1:4,更优选1:3;提取1~3小时,更优选3小时。In the present invention, it has been proved by experiments that the preferred extraction temperature is 80-90°C, more preferably 85°C; the weight ratio of acacia to water is 1:2 to 1:4, more preferably 1:3; extraction takes 1 to 3 hours , more preferably 3 hours.

本发明皂荚皂甙的提取方法中可使用各种皂荚,优选中国皂荚(Gleditsiasinensis Lam)。Various saponins can be used in the extraction method of saponins of the present invention, preferably Chinese saponins (Gleditsiasinensis Lam).

本发明进一步提供按照上述本发明方法获得的皂荚皂甙提取液。The present invention further provides the saponin extract obtained according to the above-mentioned method of the present invention.

在本发明另一个实施方案中,本发明提供一种个人护理用品,包含本发明皂荚皂甙提取液,该个人护理用品可以是洗发水、沐浴露、洗手液等。In another embodiment of the present invention, the present invention provides a personal care product comprising the saponins extract of the present invention, and the personal care product may be shampoo, shower gel, hand sanitizer, etc.

在本发明另一个实施方案中,本发明提供一种家居护理用品,包含本发明皂荚皂甙提取液,该个人护理用品可以是洗衣液、洗洁精等。In another embodiment of the present invention, the present invention provides a household care product comprising the saponin extract of the present invention, and the personal care product may be laundry detergent, detergent, etc.

本发明通过简单的水提法得到一种高含量的皂荚皂甙天然表面活性剂。该表面活性剂可以广泛的应用于个人护理用品及家居护理用品中,作为洗发水、沐浴露、洗手液、洗衣液、洗洁精等产品的主表面活性剂或辅助表面活性剂。由于皂荚皂甙天然表面活性剂的亲油基团为三萜类化合物,亲水基团为多糖等成分,从化学结构的角度来说,皂荚皂甙对皮肤的亲和程度必然远远大于合成表面活性剂,对皮肤的刺激性必然远小于合成表面活性剂。由此可知,皂荚皂甙天然表面活性剂也可运用于高端洗护或者婴幼儿洗沐产品中。The invention obtains a high-content saponin natural surfactant through a simple water extraction method. The surfactant can be widely used in personal care products and household care products, as the main surfactant or auxiliary surfactant of shampoo, shower gel, hand sanitizer, laundry detergent, detergent and other products. Since the lipophilic groups of natural surfactants of saponins are triterpenoids, and the hydrophilic groups are polysaccharides and other components, from the perspective of chemical structure, the affinity of saponins to the skin must be far greater than that of synthetic surfactants. The irritation to the skin must be far less than that of synthetic surfactants. It can be seen that saponins natural surfactants can also be used in high-end cleaning products or baby cleaning products.

本发明拟采用最丰富廉价的水为溶剂,结合超声波辅助萃取技术和磁化水处理装置来提取皂荚中的天然表面活性剂皂荚皂甙,在本发明摸索出的工业生产条件,不但安全、环保、快速、成本低,而且皂荚皂甙的提取率很高。如此简单、快速的操作工艺为大规模化运用皂荚资源提供了切实可行的操作方案。The present invention intends to use the most abundant and cheap water as a solvent, combined with ultrasonic-assisted extraction technology and magnetized water treatment equipment to extract the natural surfactant saponin in saponins. The industrial production conditions explored in the present invention are not only safe, environmentally friendly, and fast , low cost, and the extraction rate of saponins is very high. Such a simple and rapid operation process provides a practical operation plan for large-scale utilization of acacia resources.

上述皂荚皂甙提取液中除了含有皂荚皂甙天然表面活性剂之外,还含有少量纤维素、蛋白质、多糖等化学成分。纤维素、蛋白质、多糖等均为个人护理及家居护理产品中允许使用的化学成分,而且上述组分具有增稠、保湿等功效。提取液中共存的纤维素、蛋白质、多糖等杂质无需经过分离提纯。提取溶剂是水,也无需经过减压蒸馏浓缩。因此,上述方法获得的皂荚皂甙提取液可以不用经过提纯分离而直接运用于个人护理及家居护理用品中作为主表面活性剂或者辅助表面活性剂,极大的降低了生产的成本。In addition to containing saponin natural surfactant in the above-mentioned saponin extract, it also contains a small amount of chemical components such as cellulose, protein and polysaccharide. Cellulose, protein, polysaccharides, etc. are all chemical components allowed in personal care and home care products, and the above components have functions such as thickening and moisturizing. Impurities such as cellulose, protein, and polysaccharides coexisting in the extract do not need to be separated and purified. The extraction solvent is water, and it does not need to be concentrated by vacuum distillation. Therefore, the saponin extract obtained by the above method can be directly used in personal care and household care products as the main surfactant or auxiliary surfactant without purification and separation, which greatly reduces the production cost.

附图说明Description of drawings

以下,结合附图来详细说明本发明的实施方案,其中:Below, describe embodiment of the present invention in detail in conjunction with accompanying drawing, wherein:

图1为磁化水处理装置。Figure 1 is a magnetized water treatment device.

图2皂荚皂甙标准品样品的红外光谱图。The infrared spectrogram of Fig. 2 saponins standard sample.

具体实施方式Detailed ways

下面结合具体实施方式对本发明进行进一步的详细描述,给出的实施例仅为了阐明本发明,而不是为了限制本发明的范围。The present invention will be further described in detail below in conjunction with specific embodiments, and the given examples are only for clarifying the present invention, not for limiting the scope of the present invention.

下述实施例中的试验方法,如无特殊说明,均为常规方法,下述实施例中所用的原料、试剂材料等,如无特殊说明,均为市售购买产品。The test methods in the following examples, unless otherwise specified, are conventional methods, and the raw materials, reagent materials, etc. used in the following examples, unless otherwise specified, are commercially available products.

实施例1:皂荚皂甙标准品的制备、含量测定和定性检验Embodiment 1: preparation, content determination and qualitative inspection of saponins standard substance

本实验使用的皂荚来自产地为河南的皂荚树(Gleditsia sinensis Lam),其它化学试剂均为分析纯,国药集团化学试剂公司。The acacia used in this experiment came from Gleditsia sinensis Lam in Henan, and other chemical reagents were of analytical grade, from Sinopharm Chemical Reagent Company.

(1)皂荚皂甙标准品的制备和皂荚皂甙含量的测定(称重法):(1) Preparation of saponin standard substance and determination of saponin content (weighing method):

称取105℃烘干至衡重的皂荚2g(精确到0.0001g),以乙醚为溶剂索氏抽提6小时,脱去皂荚中的脂类成分。以甲醇为溶剂索氏抽提6小时,向甲醇提取液中加入等体积的乙醚收集析出的沉淀,重复操作,直到加入乙醚不再析出沉淀为止。析出的沉淀用水溶解,然后用正丁醇萃取皂甙,重复操作,直到正丁醇相无皂荚皂甙为止,合并正丁醇萃取液,挥干正丁醇,残渣放入已衡重的称量瓶中,105℃烘干至衡重,可得到皂荚皂甙标准品,称重。此法可以测得皂荚中皂荚皂甙的含量。计算公式如下:Weigh 2 g (accurate to 0.0001 g) of honey locust dried at 105°C to a constant weight, and use ether as solvent for Soxhlet extraction for 6 hours to remove the lipid components in the honey locust. Use methanol as solvent for Soxhlet extraction for 6 hours, add an equal volume of diethyl ether to the methanol extract to collect the precipitated precipitate, and repeat the operation until the precipitate is no longer precipitated after adding diethyl ether. Dissolve the precipitated precipitate in water, then extract the saponin with n-butanol, repeat the operation until the n-butanol phase has no saponins, combine the n-butanol extract, evaporate the n-butanol, and put the residue into a weighing bottle In the process, dry at 105°C to constant weight to obtain the standard saponins of saponins, and weigh them. This method can measure the content of saponins in saponins. Calculated as follows:

X—皂荚皂甙百分含量,%;X—the percentage content of saponins of saponins, %;

W1—皂荚的质量,g;W1—mass of acacia, g;

W2—烘干至衡重的称量瓶的质量,g;W2—the mass of the weighing bottle dried to the constant weight, g;

W3—烘干至衡重的试样和称量瓶的质量,g。W3—the mass of the sample and weighing bottle dried to constant weight, g.

经测定,产地为河南的皂荚中皂荚皂甙的含量为29.8%。It has been determined that the content of saponins in the saponins produced in Henan is 29.8%.

(2)皂荚皂甙标准品的定性检验(醋酐-浓硫酸显色法):(2) Qualitative inspection of saponin standard substance (acetic anhydride-concentrated sulfuric acid color method):

实验原理:皂荚皂甙遇浓硫酸先呈黄色,然后慢慢变红,再变成紫色,最后变为蓝色。Experimental principle: Saponins of saponins first turn yellow when they meet concentrated sulfuric acid, then slowly turn red, then turn purple, and finally turn blue.

实验方法:将少量上述获得的皂荚皂甙标准品样品溶于装有醋酐的试管中,然后向试管中滴加浓硫酸-醋酐试剂,观察试管中的颜色变化。Experimental method: Dissolve a small amount of saponin standard sample obtained above in a test tube filled with acetic anhydride, then add concentrated sulfuric acid-acetic anhydride reagent dropwise to the test tube, and observe the color change in the test tube.

实验结果:皂荚皂甙标准品样品在试管中的颜色变化顺序为黄色-红色-紫色-蓝色。Experimental results: the color change order of saponin standard sample in the test tube is yellow-red-purple-blue.

(3)皂荚皂甙标准品的熔点和红外光谱分析:(3) melting point and infrared spectroscopic analysis of saponins standard substance:

对上述获得的皂荚皂甙标准品样品进行熔点、红外光谱、薄层层析和液相色谱分析。Carry out melting point, infrared spectrum, thin-layer chromatography and liquid chromatography analysis to the saponins standard substance sample obtained above.

熔点:测得皂荚皂甙的熔点范围为191~195℃,文献值为192~193℃,基本吻合。Melting point: The measured melting point range of saponins is 191-195°C, and the literature value is 192-193°C, which is basically consistent.

红外光谱分析:KBr压片法。红外光谱图如图2所示。Infrared spectroscopic analysis: KBr tablet method. The infrared spectrogram is shown in Figure 2.

薄层层析:吸附剂采用硅胶G,展开剂采用乙酸乙酯-乙酸-水(8:2:1),以50%的硫酸为显色剂。Thin-layer chromatography: silica gel G was used as the adsorbent, ethyl acetate-acetic acid-water (8:2:1) was used as the developer, and 50% sulfuric acid was used as the developer.

液相色谱:ODS-2 C18反相柱(4.6mm×250mm,5μm),柱温:40℃;流动相:V(乙腈):V(水)=4:1,0.8mL·min-1;紫外检测器,检测波长454nm。Liquid chromatography: ODS-2 C 18 reverse-phase column (4.6mm×250mm, 5μm), column temperature: 40°C; mobile phase: V (acetonitrile): V (water) = 4:1, 0.8 mL·min -1 ; Ultraviolet detector, detection wavelength 454nm.

经过验证,确认提取出来的成分即为皂荚皂甙。After verification, it is confirmed that the extracted ingredients are saponins.

实施例2:皂荚皂甙提取液提取条件筛选Embodiment 2: Extraction condition screening of saponins extract

在本实施例中,参照实施例1的方法,对皂荚皂甙提取液中皂荚皂甙的含量进行测定,并相应计算出皂荚皂甙提取率。In this example, referring to the method in Example 1, the content of saponin in the saponin extract was measured, and the extraction rate of saponin was calculated accordingly.

实施例2-1:皂荚皂甙超声波功率的选择Embodiment 2-1: the selection of saponin ultrasonic power

在200L磁化水处理装置(请参见图1)中,固定皂荚:水的固液比为1:3(50公斤皂荚:150公斤水),设定超声波总辐射时间为6分钟,提取时间为2小时,提取温度为85℃。提取结束后,经过滤获得皂荚皂甙提取液。超声波功率对皂荚皂甙提取率的影响如下表1所示。In the 200L magnetized water treatment device (please refer to Fig. 1), the fixed acacia: the solid-liquid ratio of water is 1:3 (50 kilograms of acacia: 150 kilograms of water), the total ultrasonic radiation time of setting is 6 minutes, and the extraction time is 2 Hours, the extraction temperature was 85°C. After the extraction, the saponin extract was obtained by filtration. The influence of ultrasonic power on the extraction rate of saponin from saponins is shown in Table 1 below.

表1 超声波功率对提取率的影响Table 1 Effect of ultrasonic power on extraction rate

由上表可知,在300W-500W的范围获得了较好的提取率,当超声波的功率在300W时,皂荚皂甙的提取率已经较高,继续增加超声波功率,皂荚皂甙的提取率几乎没有变化。It can be seen from the above table that a good extraction rate is obtained in the range of 300W-500W. When the ultrasonic power is at 300W, the extraction rate of saponins is already high. Continue to increase the ultrasonic power, and the extraction rate of saponins hardly changes.

实施例2-2:超声波辐射时间的选择Example 2-2: Selection of Ultrasonic Radiation Time

在200L磁化水处理装置(请参见图1)中,固定皂荚:水的固液比为1:3(50公斤皂荚:150公斤水),设定超声波的功率为300W,提取时间为2小时,提取温度为85℃。提取结束后,经过滤获得皂荚皂甙提取液。In the 200L magnetized water treatment device (please refer to Fig. 1), fixed acacia: the solid-liquid ratio of water is 1:3 (50 kilograms of acacia: 150 kilograms of water), the power of setting ultrasonic wave is 300W, and extraction time is 2 hours, The extraction temperature was 85°C. After the extraction, the saponin extract was obtained by filtration.

超声波的辐射时间对皂荚皂甙提取率的影响如下表2所示。The impact of the radiation time of ultrasonic waves on the extraction rate of saponin from saponins is shown in Table 2 below.

表2 超声波辐射时间对提取率的影响Table 2 Effect of ultrasonic radiation time on extraction rate

由上表可知,在6-10分钟的范围获得了较好的提取率,当辐射时间在6分钟时,皂荚皂甙的提取率已经较高,继续增加辐射时间,皂荚皂甙提取率几乎没有变化。As can be seen from the above table, a better extraction rate has been obtained in the range of 6-10 minutes. When the radiation time is 6 minutes, the extraction rate of saponin is already high. Continue to increase the radiation time, and the extraction rate of saponin hardly changes.

实施例2-3:提取温度的选择Embodiment 2-3: the selection of extraction temperature

在200L磁化水处理装置(请参见图1)中,固定皂荚:水的固液比为1:3(50公斤皂荚:150公斤水),设定超声波的功率为300W,超声波辐射时间为6分钟,提取时间为2小时。提取结束后,经过滤获得皂荚皂甙提取液。提取温度对皂荚皂甙提取率的影响如下表3所示。In the 200L magnetized water treatment device (please refer to Figure 1), the solid-liquid ratio of fixed acacia: water is 1:3 (50 kg of acacia: 150 kg of water), the power of the ultrasonic wave is set to 300W, and the ultrasonic radiation time is 6 minutes , the extraction time is 2 hours. After the extraction, the saponin extract was obtained by filtration. The influence of extraction temperature on the extraction rate of saponin from saponins is shown in Table 3 below.

表3 提取温度对提取率的影响Table 3 Effect of extraction temperature on extraction rate

由上表可知,提取温度在80~90℃时,皂荚皂甙的提取率较高。温度在85℃以下时,随着温度的升高提取率逐渐升高,温度在85℃以上时,提取率随着温度的升高反而降低。可能是温度大于85℃时,皂荚皂甙开始部分水解导致。It can be seen from the above table that when the extraction temperature is 80-90°C, the extraction rate of saponins is higher. When the temperature was below 85°C, the extraction rate increased gradually with the increase of temperature, and when the temperature was above 85°C, the extraction rate decreased with the increase of temperature. It may be caused by partial hydrolysis of saponin when the temperature is higher than 85°C.

实施例2-4:提取时间的选择Embodiment 2-4: selection of extraction time

在200L磁化水处理装置(请参见图1)中,固定皂荚:水的固液比为1:3(50公斤皂荚:150公斤水),设定超声波的功率为300W,超声波辐射时间为6分钟,提取温度为85℃。提取结束后,经过滤获得皂荚皂甙提取液。提取时间对皂荚皂甙的影响如下表4所示。In the 200L magnetized water treatment device (please refer to Figure 1), the solid-liquid ratio of fixed acacia: water is 1:3 (50 kg of acacia: 150 kg of water), the power of the ultrasonic wave is set to 300W, and the ultrasonic radiation time is 6 minutes , the extraction temperature was 85°C. After the extraction, the saponin extract was obtained by filtration. The impact of extraction time on saponins is shown in Table 4 below.

表4 提取时间对提取率的影响Table 4 Effect of extraction time on extraction rate

由上表可知,提取时间在2~4h时,皂荚皂甙的提取率较高。当提取时间为2小时,皂荚皂甙的提取率即达到最高值。It can be seen from the above table that when the extraction time is 2 to 4 hours, the extraction rate of saponins is relatively high. When the extraction time was 2 hours, the extraction rate of saponins reached the highest value.

实施例2-5:固液比的选择Embodiment 2-5: the selection of solid-liquid ratio

在200L磁化水处理装置(请参见图1)中,设定超声波的功率为300W,超声波辐射时间为6分钟,提取温度为85℃,提取时间为2小时。提取结束后,经过滤获得皂荚皂甙提取液。固液比对皂荚皂甙提取率的影响如下表5所示。In the 200L magnetized water treatment device (please refer to FIG. 1 ), the power of the ultrasonic wave is set to 300W, the ultrasonic radiation time is 6 minutes, the extraction temperature is 85° C., and the extraction time is 2 hours. After the extraction, the saponin extract was obtained by filtration. The influence of solid-liquid ratio on the extraction rate of saponin from saponins is shown in Table 5 below.

表5 固液比对提取率的影响Table 5 Effect of solid-liquid ratio on extraction rate

固液比solid to liquid ratio 1:11:1 1:21:2 1:31:3 1:41:4 1:51:5 提取率/%Extraction rate/% 65.8865.88 77.6577.65 85.3585.35 85.4285.42 85.6185.61

由上表可知,皂荚皂甙的提取率随着水的增加,提取率增加,固液比为1:3~1:5时,皂荚皂甙的提取率较高,当固液比达到1:3以后,皂荚皂甙的提取率随着水比例的增加变化不明显。It can be seen from the above table that the extraction rate of saponins increases with the increase of water. When the solid-liquid ratio is 1:3-1:5, the extraction rate of saponins is higher. When the ratio of solid-liquid reaches 1:3 , the extraction rate of acacia saponin did not change significantly with the increase of water ratio.

实施例2-6:提取条件的正交实验优化Embodiment 2-6: Orthogonal Experimental Optimization of Extraction Conditions

在200L磁化水处理装置(请参见图1)中,设定超声波的功率为300W,超声波辐射时间为6分钟。In the 200L magnetized water treatment device (see FIG. 1 ), the power of the ultrasonic wave is set to 300W, and the ultrasonic radiation time is 6 minutes.

利用正交实验,进一步优化皂荚皂甙的提取工艺条件。选取提取温度(T)、提取时间(t)、固液比(n)为正交试验的因素,评价标准为皂荚皂甙的提取率,因素水平表见下表6,正交试验结果见下表7。Orthogonal experiments were used to further optimize the extraction process conditions of saponins. Selecting extraction temperature (T), extraction time (t), solid-liquid ratio (n) is the factor of orthogonal test, evaluation standard is the extraction rate of saponins, factor level table is shown in the following table 6, and the results of orthogonal test are shown in the following table 7.

表6 因素水平表Table 6 Factor level table

T(提取温度)/℃T(extraction temperature)/℃ t(提取时间)/ht(extraction time)/h n(固液比)n (solid-liquid ratio) 11 8080 11 1:21:2 22 8585 22 1:31:3 33 9090 33 1:41:4

表7 正交试验结果Table 7 Orthogonal test results

在上表中,I为各个因素对应的第一个水平的皂荚皂甙提取率之和,II为各个因素对应的第二个水平的皂荚皂甙提取率之和,III为各个因素对应的第三个水平的皂荚皂甙提取率之和,I/3为各个因素对应的第一个水平的皂荚皂甙提取率的平均值,II/3为各个因素对应的第二个水平的皂荚皂甙提取率的平均值,III/3为各个因素对应的第三个水平的皂荚皂甙提取率的平均值。In the above table, I is the sum of the first level of saponin extraction rate corresponding to each factor, II is the sum of the extraction rate of saponin of the second level corresponding to each factor, and III is the third level of each factor The sum of the saponins extraction rate of each level, I/3 is the average value of the first level saponin extraction rate corresponding to each factor, and II/3 is the average value of the second level saponin extraction rate corresponding to each factor , III/3 is the average value of the saponins extraction rate of the third level corresponding to each factor.

由表7可知,实验序号9对应的皂荚皂甙产率最高,实验序号5对应的皂荚皂甙产率第二,两次实验的条件见下表8。It can be seen from Table 7 that the saponin yield corresponding to experiment number 9 is the highest, and the yield of saponin corresponding to experiment number 5 is the second. The conditions of the two experiments are shown in Table 8 below.

表8 正交试验直观分析表Table 8 Orthogonal test visual analysis table

由极差分析可知,对皂荚皂甙提取率影响最大的因素依次是:提取时间(t)>固液比(n)>提取温度(T)。皂荚皂甙最优提取工艺条件为T2t3n2,即提取温度为85℃、提取时间为3小时,固液比为1:3。From the range analysis, it can be seen that the factors that have the greatest impact on the extraction rate of saponins are: extraction time (t) > solid-liquid ratio (n) > extraction temperature (T). The optimal extraction process conditions for saponins are T 2 t 3 n 2 , that is, the extraction temperature is 85°C, the extraction time is 3 hours, and the solid-liquid ratio is 1:3.

对皂荚皂甙提取的最优工艺条件进行了3次实验验证,结果如下表9所示,皂荚皂甙的平均提取率为86.56%。Three experiments were carried out to verify the optimal process conditions for the extraction of saponins from saponins. The results are shown in Table 9 below. The average extraction rate of saponins from saponins is 86.56%.

表9 验证性试验Table 9 Confirmatory test

实施例3:皂荚皂甙提取液理化指标的分析Embodiment 3: the analysis of physical and chemical index of saponin saponin extract

经测定,由如上实施例7中的实验10-12获得的皂荚皂甙提取液混合物的理化指标如下表10所示。The physical and chemical indicators of the saponins extract mixture obtained from Experiments 10-12 in Example 7 above are shown in Table 10 below.

表10 皂荚皂甙提取液的理化指标*Table 10 Physicochemical indicators of saponins extract*

*测试方法参考《化妆品安全技术规范》(2015版)*The test method refers to "Safety and Technical Specifications for Cosmetics" (2015 edition)

由表10中的测试数据可知,上述皂荚皂甙提取液的各项理化指标均符合《化妆品安全技术规范》(2015版)中对原料的要求。由此可知,该皂荚皂甙提取液可以直接作为化妆品原料添加到化妆品配方中。From the test data in Table 10, it can be seen that the physical and chemical indicators of the above-mentioned saponin extract of saponins all meet the requirements for raw materials in the "Safety and Technical Specifications for Cosmetics" (2015 edition). It can be seen that the saponin extract can be directly added to the cosmetic formula as a cosmetic raw material.

实施例4:本发明皂荚皂甙提取液的应用Embodiment 4: the application of saponin saponin extract of the present invention

实施例4-1:皂荚洗发水的配制Embodiment 4-1: the preparation of soap locust shampoo

称取如下各个原料:本发明皂荚皂甙提取液4000g、EDTA二钠5g、椰油酰胺丙基甜菜碱300g、椰油酰胺DEA 100g、乳化硅油150g、瓜儿胶羟丙基三甲基氯化铵10g、聚季铵盐-10 5g、柠檬酸0.5g、氯化钠75g、卡松4g、香精17.5g、去离子水333g。Take by weighing the following raw materials: saponin saponin extract of the present invention 4000g, disodium EDTA 5g, cocamidopropyl betaine 300g, cocamide DEA 100g, emulsified silicone oil 150g, guar gum hydroxypropyl trimethyl ammonium chloride 10g, polyquaternium-10 5g, citric acid 0.5g, sodium chloride 75g, Cathone 4g, essence 17.5g, deionized water 333g.

将瓜儿胶羟丙基三甲基氯化铵和200g水搅拌混合,得到瓜儿胶羟丙基三甲基氯化铵水溶液。将聚季铵盐-10和133g水搅拌混合,得到聚季铵盐-10水溶液。Guar gum hydroxypropyltrimethylammonium chloride and 200g of water were stirred and mixed to obtain an aqueous solution of guar gum hydroxypropyltrimethylammonium chloride. Stir and mix polyquaternium-10 and 133 g of water to obtain polyquaternium-10 aqueous solution.

将本发明皂荚皂甙提取液加入到搅拌锅中,加热至75℃。加入瓜儿胶羟丙基三甲基氯化铵水溶液、聚季铵盐-10水溶液,搅拌均匀;加入EDTA二钠、椰油酰胺丙基甜菜碱、椰油酰胺DEA,搅拌均匀;降温至45℃,加入乳化硅油、柠檬酸、氯化钠、卡松、香精,搅拌30分钟,然后用200目过滤网过滤,即得。Add the saponins extract of the present invention into a stirring pot and heat to 75°C. Add guar gum hydroxypropyltrimethylammonium chloride aqueous solution, polyquaternium-10 aqueous solution, stir well; add disodium EDTA, cocamidopropyl betaine, cocamide DEA, stir well; cool down to 45 ℃, add emulsified silicone oil, citric acid, sodium chloride, Cathone, and essence, stir for 30 minutes, and then filter with a 200-mesh filter to obtain the product.

实施例4-2:皂荚沐浴露的配制Embodiment 4-2: the preparation of soap locust shower gel

称取如下各个原料:本发明皂荚皂甙提取液2250g、EDTA二钠5g、椰油酰胺丙基甜菜碱300g、椰油酰胺DEA 100g、柠檬酸0.5g、氯化钠100g、卡松4g、香精17.5g、去离子水2223g。Take by weighing the following raw materials: saponin extract of saponins of the present invention 2250g, disodium EDTA 5g, cocamidopropyl betaine 300g, cocamide DEA 100g, citric acid 0.5g, sodium chloride 100g, Kathon 4g, essence 17.5g g, deionized water 2223g.

依次将去离子水、本发明皂荚皂甙提取液、EDTA二钠、椰油酰胺丙基甜菜碱、椰油酰胺DEA、柠檬酸、氯化钠、卡松、香精加入到搅拌锅中,搅拌60分钟,然后用200目过滤网过滤,即得。Add deionized water, saponin extract of saponins of the present invention, disodium EDTA, cocamidopropyl betaine, cocamide DEA, citric acid, sodium chloride, cassonne, and essence into the stirring pot in turn, and stir for 60 minutes , and then filter with a 200-mesh filter, that is.

实施例4-3:皂荚洗手液的配制Embodiment 4-3: the preparation of soap locust hand sanitizer

称取如下各个原料:本发明皂荚皂甙提取液1250g、月桂醇聚醚硫酸酯钠125g、EDTA二钠5g、椰油酰胺丙基甜菜碱300g、椰油酰胺DEA100g、柠檬酸0.5g、氯化钠100g、卡松4g、香精17.5g、去离子水3098g。Take by weighing following each raw material: saponin saponin extract 1250g of the present invention, sodium laureth sulfate 125g, disodium EDTA 5g, cocamidopropyl betaine 300g, cocamide DEA100g, citric acid 0.5g, sodium chloride 100g, Kason 4g, essence 17.5g, deionized water 3098g.

依次将去离子水、本发明皂荚皂甙提取液、月桂醇聚醚硫酸酯钠、EDTA二钠、椰油酰胺丙基甜菜碱、椰油酰胺DEA、柠檬酸、氯化钠、卡松、香精加入到搅拌锅中,搅拌60分钟,然后用200目过滤网过滤,即得。Add deionized water, saponin extract of saponins of the present invention, sodium lauryl ether sulfate, disodium EDTA, cocamidopropyl betaine, cocamide DEA, citric acid, sodium chloride, Cathone, and essence in sequence Put it in a stirring pot, stir for 60 minutes, and then filter it with a 200-mesh filter.

实施例4-4:皂荚洗衣液的配制Embodiment 4-4: the preparation of soap locust laundry detergent

称取如下各个原料:本发明皂荚皂甙提取液500g、十二烷基苯磺酸钠300g、月桂醇聚醚-9 200g、月桂醇聚醚硫酸酯钠300g、柠檬酸钠25g、羟乙基纤维素35g、DMDM乙内酰脲10g、香精7.5g、去离子水3622.5g。Take by weighing the following raw materials: saponin extract of saponins of the present invention 500g, sodium dodecylbenzenesulfonate 300g, laureth-9 200g, sodium laureth sulfate 300g, sodium citrate 25g, hydroxyethyl cellulose Su 35g, DMDM hydantoin 10g, essence 7.5g, deionized water 3622.5g.

依次将去离子水、本发明皂荚皂甙提取液、十二烷基苯磺酸钠、月桂醇聚醚-9、月桂醇聚醚硫酸酯钠、柠檬酸钠、羟乙基纤维素、DMDM乙内酰脲、香精加入到搅拌锅中,搅拌60分钟,然后用200目过滤网过滤,即得。Deionized water, saponin extract of the present invention, sodium dodecylbenzenesulfonate, lauryl ether-9, sodium lauryl ether sulfate, sodium citrate, hydroxyethyl cellulose, DMDM benzine Add the ureide and essence into the stirring pot, stir for 60 minutes, and then filter with a 200-mesh filter to obtain the product.

实施例4-5:皂荚洗洁精的配制Embodiment 4-5: the preparation of soap locust detergent

称取如下各个原料:本发明皂荚皂甙提取液750g、十二烷基苯磺酸钠300g、月桂醇聚醚-9 75g、月桂醇聚醚硫酸酯钠500g、柠檬酸钠25g、氯化钠75g、DMDM乙内酰脲10g、香精7.5g、去离子水3257.5g。Take by weighing the following raw materials: 750g of saponin extract of saponins of the present invention, 300g of sodium dodecylbenzenesulfonate, 75g of laureth-9, 500g of sodium laureth sulfate, 25g of sodium citrate, and 75g of sodium chloride , DMDM hydantoin 10g, essence 7.5g, deionized water 3257.5g.

依次将去离子水、本发明皂荚皂甙提取液、十二烷基苯磺酸钠、月桂醇聚醚-9、月桂醇聚醚硫酸酯钠、柠檬酸钠、氯化钠、DMDM乙内酰脲、香精加入到搅拌锅中,搅拌60分钟,然后用200目过滤网过滤,即得。Deionized water, saponin extract of saponins of the present invention, sodium dodecylbenzenesulfonate, laureth-9, sodium laureth sulfate, sodium citrate, sodium chloride, DMDM hydantoin 1. Add the essence into the stirring pot, stir for 60 minutes, and then filter with a 200-mesh filter to get the product.

Claims (10)

1. a kind of extracting method of gleditschiasaponin, it is characterised in that using Chinese honey locust as raw material, water uses magnetic as solvent Water chemical treatment device and ultrasound-assisted extraction technology.
2. the extracting method of gleditschiasaponin according to claim 1, wherein the magnetic water treatment device used includes magnetization Reservoir chamber (1), motor (2), reductor (3), power transmission shaft (4), magnetization impeller (5), the motor (2) connect the reductor (3) and described magnetization reservoir chamber (1) top is arranged on, power transmission shaft (4) the connection reductor (3) is simultaneously arranged at magnetization reservoir chamber (1) it is internal, magnetization impeller (5) the connection power transmission shaft (4);
Preferably, described magnetization reservoir chamber (1) lower end sets magnetization chamber (12), wherein, magnet is set inside magnetization chamber (12) (6);
Preferably, chuck (7) is set on the outside of the magnetization reservoir chamber (1), and chuck (7) one end sets cold water delivery port (8), another End sets cold water inlet (9);
Preferably, the internal magnet (6) of the magnetization chamber (12) is multiple;
Preferably, the magnet (6) is native magnet;
Preferably, the native magnet and the mass ratio of the deionized water are 1:10-20;
Preferably, the native magnet is Fe3O4;
Preferably, the magnetic water treatment device is 200L.
3. the power of the extracting method of gleditschiasaponin according to claim 1 or 2, wherein ultrasonic wave is 300-500W, surpass The acoustic irradiation time is 6-10 minutes.
4. the power of the extracting method of gleditschiasaponin according to claim 3, wherein ultrasonic wave is 300W, Ultrasonic Radiation Time is 6 minutes.
5. the extracting method of the gleditschiasaponin according to claim any one of 1-4, wherein Extracting temperature are 80-90 DEG C, soap The weight of pod and water ratio is 1:2~1:4, extract 1~3 hour.
6. the extracting method of gleditschiasaponin according to claim 5, wherein Extracting temperature are 85 DEG C, the weight of Chinese honey locust and water Than for 1:3, extract 3 hours.
7. the extracting method of the gleditschiasaponin according to claim any one of 1-6, the Chinese honey locust used is Chinese Chinese honey locust (Gleditsia sinensis Lam)。
8. the gleditschiasaponin extract solution obtained according to any one of claim 1-7 extracting method.
9. a kind of personal-care supplies, the gleditschiasaponin extract solution comprising claim 8, it is preferably shampoo, shower cream, washed Hand liquid.
10. a kind of household care products, the gleditschiasaponin extract solution comprising claim 8, it is preferably liquid detergent, liquid detergent.
CN201711083423.4A 2017-11-07 2017-11-07 A kind of extracting method of gleditschiasaponin Pending CN107857792A (en)

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CN113599323A (en) * 2021-08-18 2021-11-05 广州德谷个人护理用品有限公司 Formula and preparation method of shower gel containing gleditschia horrida saponin
CN115595215A (en) * 2022-09-07 2023-01-13 江苏雪豹日化有限公司(Cn) Environment-friendly oil stain purifying agent and preparation method thereof
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