CN103750563A - Preparation method and radical reduction and harm reduction application of squalene and tea polyphenol composition liquid proliposome - Google Patents
Preparation method and radical reduction and harm reduction application of squalene and tea polyphenol composition liquid proliposome Download PDFInfo
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技术领域 technical field
本发明涉及化学技术领域,更具体地,涉及一种含角鲨烯与茶多酚组合物的液态前体脂质体及其制备方法和在水烟型过滤嘴降基减害方面的应用。 The invention relates to the field of chemical technology, more specifically, to a liquid proliposome containing a composition of squalene and tea polyphenols, a preparation method thereof, and an application in reducing bases and harms of hookah-type filters.
背景技术 Background technique
吸烟产生的数千种化合物以及高浓度的自由基对人体造成的危害引起人们的普遍重视。而自由基对身体作用最强危害最大,其可引起肺病、心脏病和癌症,这些自由基对吸烟者产生严重的伤害。吸烟产生高浓度的自由基,包括寿命相对较长的固相自由基,醌类和半醌类、多环芳烃类自由基以及它们与氧反应产生的活性氧自由基如超氧阴离子(O2 -)、过氧化氢(H2O2)、羟自由基(·OH)、单线态氧(1O2)和脂质过氧化自由基(ROO·)等和存在时间相对较短的气相自由基,烷氧自由基(RO·)、烷基自由基(R·)、氮氧化物自由基等。 Thousands of compounds produced by smoking and the harm caused by high concentration of free radicals to the human body have attracted widespread attention. Free radicals have the strongest effect on the body and are the most harmful. They can cause lung disease, heart disease and cancer. These free radicals can cause serious damage to smokers. Smoking produces high concentrations of free radicals, including relatively long-lived solid-phase free radicals, quinones and semiquinones, polycyclic aromatic hydrocarbons free radicals, and reactive oxygen free radicals produced by their reactions with oxygen such as superoxide anion (O 2 - ), hydrogen peroxide (H 2 O 2 ), hydroxyl radicals (·OH), singlet oxygen ( 1 O 2 ) and lipid peroxidation radicals (ROO·) and gas phase free radicals with a relatively short existence time radicals, alkoxy radicals (RO·), alkyl radicals (R·), nitrogen oxide radicals, etc.
目前在对烟气中自由基清除研究方面并不多,主要从外加天然抗氧化剂、维生素、氨基酸、蛋白质等以及生物酶自由基清除剂和微量元素、天然矿物质来降低烟气中自由基对人体的伤害。还有,我国部分地区有吸水烟的习惯,其是燃烧后的烟通过水烟筒里的水后再吸入嘴里,其不但可以清除溶于水的有害化学物质,还可以清除部分气相自由基,减轻了吸烟对人体的伤害。并且可以减轻由于吸烟引起人体上火的机率。罗福仲(2013)在公开号为CN 203182005 U的实用新型专利公开了一种水烟型过滤嘴,在水中加入表面活性剂和/或加入薄荷、甘草等中草药提取成分,其达到的目的是显著降低焦油、尼古丁含量,不会上火,也不会影响烟草的味道,结构简单、成本低廉;姜志敏(2008)在专利号为ZL200820107184.1的实用新型专利申请中公开了一种水烟过滤嘴,在水烟过滤嘴结构上改进设计。蒋华国(1998)在其实用新型专利申请中公开了一种便携式水烟斗,将水烟斗的结构简单化;黄辉(2005)在公开号为CN200510129846.6的发明专利中公开了一种利用水烟斗对烟卷除焦及综合减害的方法,研究了除焦和综合减害而调制成型的液态制剂。在上述水烟型过滤嘴中,都没有涉及将适宜的抗氧化剂科学加入水烟型烟嘴中,清除烟气中气相自由基的研究。 At present, there are not many researches on the scavenging of free radicals in flue gas, mainly from the addition of natural antioxidants, vitamins, amino acids, proteins, etc., as well as biological enzyme free radical scavengers, trace elements, and natural minerals to reduce free radicals in flue gas human injury. In addition, some areas of our country have the habit of smoking hookah, which means that the burned smoke passes through the water in the hookah and then inhales into the mouth. It can not only remove harmful chemicals dissolved in water, but also remove some gaseous free radicals. Reduced the harm of smoking to the human body. And it can reduce the probability of human body getting angry due to smoking. Luo Fuzhong (2013) disclosed a utility model patent with the publication number CN 203182005 U to disclose a hookah-type filter tip, adding surfactants and/or extracts of Chinese herbal medicines such as mint and licorice into the water, the purpose of which is to significantly reduce tar, Nicotine content, will not get angry, and will not affect the taste of tobacco. improve the design. Jiang Huaguo (1998) disclosed a portable water pipe in his utility model patent application, which simplifies the structure of the water pipe; Huang Hui (2005) disclosed a water pipe using For the method of decoking and comprehensive harm reduction of cigarettes, the liquid preparation formulated for decoking and comprehensive harm reduction is studied. Among the above-mentioned hookah-type filters, there is no research on scientifically adding suitable antioxidants into the hookah-type cigarette holder to remove gas-phase free radicals in the smoke.
角鲨烯是一种脂质不皂化物,为一种多不饱和烯烃(三十碳六烯),最初是从鲨鱼的肝油中发现的,1914年被命名为Squalene,其化学名称为2,6,10,15,19,23-六甲基-2,6,10,14,18,22-二十四碳六烯,属开链三萜,又称鱼肝油萜,参与人体胆固醇合成并能促进新陈代谢,具有提高体内超氧化物歧化酶(SOD)活性、增强机体免疫能力、抗衰老、抗疲劳、抗肿瘤等多种生理功能,是一种无毒性的具有防病治病作用的海洋生物活性物质。角鲨烯在植物中分布很广,但含量不高,多低于植物油中不皂化物的5%,仅少数含量较多,如橄榄油含有角鲨烯150~700mg/100g,米糠油中其含量为332mg/100g。 Squalene is a lipid unsaponifiable substance, a polyunsaturated olefin (tricosahexaene), originally discovered from shark liver oil, named Squalene in 1914, and its chemical name is 2, 6,10,15,19,23-hexamethyl-2,6,10,14,18,22-tetracosahexaene, which is an open-chain triterpene, also known as cod liver oil terpene, participates in the synthesis of cholesterol in the human body and can It promotes metabolism, has many physiological functions such as increasing the activity of superoxide dismutase (SOD) in the body, enhancing the body's immunity, anti-aging, anti-fatigue, anti-tumor, etc. It is a non-toxic marine organism with the effect of preventing and curing diseases active substance. Squalene is widely distributed in plants, but the content is not high, mostly less than 5% of the unsaponifiable matter in vegetable oil, and only a few have more content, such as olive oil containing squalene 150-700mg/100g, rice bran oil containing The content is 332mg/100g.
茶多酚是茶叶中儿茶素类、丙酮类、酚酸类和花色素类化合物的总称。是一种稠环芳香烃,可分为黄烷醇类、羟基-[4]-黄烷醇类、花色苷类、黄酮类、黄酮醇类和酚酸类等。其中以儿茶素最为重要,约占多酚类总量的60%~80%;儿茶素类主要由EGC、DLC、EC、EGCG、GCG、ECG等几种单体组成。茶多酚在茶叶中的含量一般在20~35%。在茶多酚中各组成份中以黄烷醇类为主,黄烷醇类又以儿茶素类物质为主。儿茶素类物质的含量约占茶多酚总量的70%左右。具有很强的消除有害自由基的作用,抗衰老作用,抗辐射作用,对癌细胞的抑制作用,抗菌、杀菌作用,对艾滋病病毒的抑制作用,现有研究证明茶多酚还对烟民有好处,可以清洗肺部尼古丁。 Tea polyphenols are the general term for catechins, acetones, phenolic acids and anthocyanins in tea. It is a fused-ring aromatic hydrocarbon, which can be divided into flavanols, hydroxy-[4]-flavanols, anthocyanins, flavonoids, flavonols and phenolic acids. Among them, catechins are the most important, accounting for about 60% to 80% of the total polyphenols; catechins are mainly composed of several monomers such as EGC, DLC, EC, EGCG, GCG, and ECG. The content of tea polyphenols in tea is generally 20-35%. Among the components of tea polyphenols, flavanols are the main components, and flavanols are mainly catechins. The content of catechins accounts for about 70% of the total amount of tea polyphenols. It has a strong effect of eliminating harmful free radicals, anti-aging effect, anti-radiation effect, inhibitory effect on cancer cells, antibacterial and bactericidal effects, and inhibitory effect on HIV. Existing studies have proved that tea polyphenols are also good for smokers , can clean the lungs of nicotine.
为了克服普通抗氧化剂的缺点,达到可同时清除长寿命的固相自由基和存在时间相对较短的气相自由基的目的,本申请人长期致力于相关研究并获得相关专利。在专利号为ZL201010529711.X的申请中公开了角鲨烯与茶多酚组合物及其在卷烟中的应用,将角鲨烯与茶多酚增效组合物直接添加到烟丝中,获得较好的应用效果。但进一步的研究发现,角鲨烯与茶多酚在空气中易于氧化变质,组合物在应用时不稳定,实际生产不方便。 In order to overcome the shortcomings of common antioxidants and achieve the purpose of simultaneously removing long-lived solid-phase free radicals and relatively short-lived gas-phase free radicals, the applicant has devoted himself to related research for a long time and obtained related patents. In the application with the patent number ZL201010529711.X, the composition of squalene and tea polyphenols and its application in cigarettes are disclosed. The synergistic composition of squalene and tea polyphenols is directly added to shredded tobacco to obtain better application effect. However, further studies have found that squalene and tea polyphenols are prone to oxidative deterioration in the air, and the composition is unstable during application, which is inconvenient for actual production.
脂质体(liposome)是一种人工膜。当两性分子如磷脂和鞘脂分散于水相时,分子的疏水尾部倾向于聚集在一起,避开水相,而亲水头部暴露在水相,形成具有双分子层结构的的封闭囊泡,称为脂质体。按照结构分类,脂质体分为单室脂质体,多室脂质体和液态前体脂质体。液态前体脂质体是一种具有缓释效果的脂质体,由许多非同心室连接构成,粒径在5~50μm,比普通脂质体具有更大的包封体积,尤其适用于水溶性药物的包封。脂质体的应用目前主要是在医药方面。 Liposome is an artificial membrane. When amphiphilic molecules such as phospholipids and sphingolipids are dispersed in the aqueous phase, the hydrophobic tails of the molecules tend to gather together and avoid the aqueous phase, while the hydrophilic heads are exposed to the aqueous phase, forming closed vesicles with a bilayer structure , called liposomes. According to structural classification, liposomes are divided into unilamellar liposomes, multilamellar liposomes and liquid proliposomes. Liquid proliposome is a kind of liposome with sustained release effect, composed of many non-concentric ventricular connections, with a particle size of 5-50 μm, which has a larger encapsulation volume than ordinary liposomes, and is especially suitable for water-soluble Encapsulation of sexual drugs. The application of liposome is mainly in medicine at present.
将这些自由基清除剂加工成液态前体脂质体,并科学置入水烟型烟嘴中清除气相自由基(降基)的研究目前未见报道,更未见基于角鲨烯与茶多酚增效组合物的液态前体脂质体的制备技术和应用报道。 The research of processing these free radical scavengers into liquid proliposomes and scientifically placing them in hookah cigarette holders to scavenge gaseous free radicals (reduced radicals) has not been reported at present, let alone studies based on the enhancement of squalene and tea polyphenols. Preparation technology and application report of liquid proliposomes with effective composition.
发明内容 Contents of the invention
本发明的目的是克服现有液态前体脂质体技术在卷烟方面的应用不足,以及角鲨烯与茶多酚增效组合物在卷烟应用方面的技术不足,提供一种含角鲨烯与茶多酚组合物的液态前体脂质体。 The purpose of the present invention is to overcome the deficiency in the application of existing liquid proliposome technology in cigarettes, and the technical deficiency in the application of squalene and tea polyphenol synergistic composition in cigarettes, and provide a kind of Liquid proliposomes of tea polyphenol compositions.
本发明的另一目的是提供所述液态前体脂质体的制备方法。 Another object of the present invention is to provide a method for preparing the liquid proliposome.
本发明的还一发明目的是提供所述含角鲨烯与茶多酚组合物的液态前体脂质体在水烟型过滤嘴中的应用。 Still another object of the present invention is to provide the application of the liquid proliposome containing squalene and tea polyphenols composition in hookah filter.
本发明的目的通过以下技术方案予以实现: The purpose of the present invention is achieved through the following technical solutions:
提供一种含角鲨烯与茶多酚组合物的液态前体脂质体,所述液态前体脂质体是由以下质量份数的各组分制备得到: A liquid proliposome containing squalene and tea polyphenol composition is provided, and the liquid proliposome is prepared from the following components in parts by mass:
氢化磷脂: 7~10份; Hydrogenated phospholipids: 7 to 10 parts;
稳定剂: 8~12份; Stabilizer: 8 to 12 parts;
表面活性剂: 10~15份; Surfactant: 10-15 parts;
角鲨烯与茶多酚组合物:25~45份; Composition of squalene and tea polyphenols: 25-45 parts;
余量的水; remaining water;
上述各组分质量份数之和为100份; The sum of the mass parts of the above-mentioned components is 100 parts;
优选地,所述含角鲨烯与茶多酚组合物的液态前体脂质体,所述液态前体脂质体是由以下质量份数的各组分制备得到: Preferably, the liquid proliposome containing squalene and tea polyphenol composition is prepared from the following components in parts by mass:
氢化磷脂: 8~9 份; Hydrogenated phospholipids: 8-9 parts;
稳定剂: 9~11份; Stabilizer: 9 to 11 parts;
表面活性剂: 12~14份; Surfactant: 12 to 14 parts;
角鲨烯与茶多酚组合物: 30~35 份; Composition of squalene and tea polyphenols: 30-35 parts;
余量的水; remaining water;
上述各组分质量份数之和为100份。 The sum of the parts by mass of the above-mentioned components is 100 parts.
可采用复乳法以上述各组分制备得到所述含角鲨烯与茶多酚组合物的液态前体脂质体。 The liquid proliposome containing the composition of squalene and tea polyphenol can be prepared by using the above-mentioned components by double emulsion method.
所述的磷脂为卵磷脂、大豆磷脂、氢化大豆磷脂中的一种或多种;采用多种磷脂,各种磷脂的混合比例不做严格限定。 The phospholipids are one or more of lecithin, soybean lecithin, and hydrogenated soybean lecithin; a variety of phospholipids are used, and the mixing ratio of various phospholipids is not strictly limited.
所述的稳定剂优选羟基淀粉,更为优选地,所述羟基淀粉为羟甲基淀粉、羟乙基淀粉或羟丙基淀粉中的一种或多种。采用多种时,混合比例不做严格限定。 The stabilizer is preferably hydroxystarch, more preferably, the hydroxystarch is one or more of hydroxymethyl starch, hydroxyethyl starch or hydroxypropyl starch. When using multiple types, the mixing ratio is not strictly limited.
所述表面活性剂为丙三醇。 The surfactant is glycerol.
所述的角鲨烯与茶多酚组合物中角鲨烯与茶多酚的质量比例为1∶8~8∶1,更优化的比例为:2∶7~7∶2。 The mass ratio of squalene and tea polyphenols in the squalene and tea polyphenols composition is 1:8-8:1, and the more optimal ratio is: 2:7-7:2.
所述的角鲨烯可以是从植物、动物或微生物中提取的抽提物或经纯化后的纯品,可采用市购产品。 The squalene can be an extract extracted from plants, animals or microorganisms or a purified product, and commercially available products can be used.
所述的茶多酚可以是从茶叶中提取的茶多酚抽提物也可以是经纯化后的纯品,可采用市购产品。 The tea polyphenols can be tea polyphenol extracts extracted from tea leaves or purified pure products, and commercially available products can be used.
本发明同时提供了所述含角鲨烯与茶多酚组合物的液态前体脂质体的制备方法,科学配伍原料,精确了工艺条件,克服了角鲨烯与茶多酚在水中溶解度不 The present invention also provides the preparation method of the liquid proliposome containing squalene and tea polyphenols composition, scientifically compatible raw materials, accurate process conditions, and overcomes the incompatibility of squalene and tea polyphenols in water solubility.
高的缺点,成功制备得到含角鲨烯与茶多酚混配增效组合物的液态前体脂质体,可以很好地实现将其应用于水烟型过滤嘴的目的。所述制备方法包括以下步骤: High disadvantages, the successful preparation of liquid proliposomes containing squalene and tea polyphenols mixed synergistic composition can well achieve the purpose of applying it to hookah filters. The preparation method comprises the following steps:
S1.将磷脂和角鲨烯与茶多酚组合物溶于丙三醇中,得混合体系; S1. Dissolving the composition of phospholipids, squalene and tea polyphenols in glycerol to obtain a mixed system;
S2.将S1所得混合体系高速均化使其充分混匀,得均化的混合体系; S2. Homogenize the mixed system obtained in S1 at high speed to make it fully mixed to obtain a homogenized mixed system;
S3.将稳定剂和水混合得到稳定剂的水溶液,往S2所得均化的混合体系中加入稳定剂的水溶液后搅拌均匀,形成稳定的微粒悬浮液即得含角鲨烯与茶多酚组合物的液态前体脂质体。 S3. Mix the stabilizer and water to obtain an aqueous solution of the stabilizer, add the aqueous solution of the stabilizer to the homogenized mixing system obtained in S2 and stir evenly to form a stable particle suspension to obtain the composition containing squalene and tea polyphenols liquid proliposomes.
优选地,S2所述高速均化的工艺条件为:2000 r/min,搅拌45min。 Preferably, the process conditions of the high-speed homogenization described in S2 are: 2000 r/min, stirring for 45min.
本发明提供上述方法制备得到的含角鲨烯与茶多酚组合物的液态前体脂质体。 The invention provides the liquid proliposome containing squalene and tea polyphenols prepared by the above method.
本发明所述含角鲨烯与茶多酚组合物的液态前体脂质体在卷烟中获得很好的应用,具体是应用于水烟型过滤嘴,是将所述液态前体脂质体装入两端为防水防尘透气膜的空心圆柱体中,在卷烟滤嘴棒成型过程中内置于醋酸纤维的卷烟过滤嘴中。 The liquid proliposome containing squalene and tea polyphenol composition of the present invention is very well applied in cigarettes, and is particularly applied to a hookah filter tip, and the liquid proliposome is packed into In a hollow cylinder with waterproof, dustproof and air-permeable membranes at both ends, it is built into a cigarette filter tip of acetate fiber during the molding process of a cigarette filter rod.
优选地应用方法为:将所述液态前体脂质体装入两端为防水防尘透气膜的空心圆柱体中,每粒装入1克所述液态前体脂质体,在卷烟滤嘴棒成型过程中内置于醋酸纤维的卷烟过滤嘴中,每支卷烟过滤嘴内置1粒,得到可降低卷烟危害的卷烟过滤嘴,当消费者吸烟时,烟气通过内置的液态前体脂质体,由于液态前体脂质体表面积大,抗氧化剂与主流烟气充分接触,可有效清除主流烟气中的气相自由基,为解决吸烟与健康的问题提供有力的技术支持。 The preferred application method is: the liquid proliposome is packed into a hollow cylinder with waterproof, dustproof and air-permeable membranes at both ends, and 1 gram of the liquid proliposome is packed into each capsule, and placed in the cigarette filter In the rod forming process, it is built into the acetate fiber cigarette filter. Each cigarette filter is built with 1 capsule, and the cigarette filter that can reduce the harm of cigarettes is obtained. When consumers smoke, the smoke passes through the built-in liquid precursor liposome, due to the liquid The proliposome has a large surface area, and the antioxidant is in full contact with the mainstream smoke, which can effectively remove the gas-phase free radicals in the mainstream smoke, and provide strong technical support for solving the problems of smoking and health.
本发明的有益效果: Beneficial effects of the present invention:
本发明首次将脂质体尤其是液态前体脂质体的技术应用于卷烟中,并成功结合角鲨烯与茶多酚增效组合物,总结出适宜的配伍助剂和配伍比例,简单易行地制备得到含角鲨烯与茶多酚增效组合物的液态前体脂质体,为脂质体的进一步开拓应用提供有力的技术支持,所得液态前体脂质体为高度分散微小液滴,分散度高,比表面积大,可直接应用于水烟型过滤嘴中。 The present invention applies liposome technology, especially liquid proliposome technology, to cigarettes for the first time, and successfully combines squalene and tea polyphenol synergistic composition, sums up suitable compatibility aids and compatibility ratio, simple and easy The liquid proliposomes containing squalene and tea polyphenols synergistic composition were successfully prepared, which provided strong technical support for the further development and application of liposomes. The obtained liquid proliposomes were highly dispersed micro-liquids Drops, high dispersion, large specific surface area, can be directly applied to hookah filter.
本发明将增效组合物成功包埋于液态前体脂质体中,克服了角鲨烯与茶多酚在空气中易于氧化失效的缺点,同时克服角鲨烯与茶多酚增效组合物不溶于水的缺陷,通过对角鲨烯与茶多酚混配增效组合物微胶囊化,达到增加角鲨烯与茶多酚混配增效组合物的稳定性,获得可以应用于卷烟过滤嘴的液态前体脂质体。 The invention successfully embeds the synergistic composition in the liquid proliposome, overcomes the shortcoming that squalene and tea polyphenols are easy to oxidize and fail in air, and simultaneously overcomes the synergistic composition of squalene and tea polyphenols The defect of being insoluble in water, by microencapsulating the compounded synergistic composition of squalene and tea polyphenols, the stability of the compounded synergistic composition of squalene and tea polyphenols can be increased, and it can be applied to cigarette filters liquid proliposomes.
本发明精确限定原料配伍和制备工艺条件,加工得到的液态前体脂质体透气性强,表面积大,适合卷烟过滤嘴的应用需求,可直接应用于水烟型过滤嘴,抗氧化剂可与主流烟气充分接触,达到清除主流烟气中自由基的目的,为解决吸烟与健康的问题提供有力的技术支持。 The invention precisely defines the raw material compatibility and preparation process conditions, and the processed liquid proliposome has strong air permeability and large surface area, which is suitable for the application requirements of cigarette filters, can be directly applied to hookah filters, and the antioxidant can be fully mixed with mainstream smoke. Contact, to achieve the purpose of removing free radicals in mainstream smoke, and provide strong technical support for solving the problems of smoking and health.
具体实施方式 Detailed ways
下面结合具体实施例进一步详细说明本发明。下述实施例中所使用的试验方法如无特殊说明,均为常规方法;所使用的材料、试剂等,如无特殊说明,为可从常规商业途径得到的试剂和材料。 The present invention will be further described in detail below in conjunction with specific examples. The test methods used in the following examples, unless otherwise specified, are conventional methods; the materials, reagents, etc. used, unless otherwise specified, are reagents and materials that can be obtained from conventional commercial channels.
实施例1 Example 1
按照以下质量份数制备各组分:氢化卵磷脂10克(g);角鲨烯(上海信然生物技术有限公司,含量大于96.0%,下述实施例同。但并不因此限定本发明,本领域技术人员可采用其他来源的角鲨烯)5克(g);茶多酚(宁波优捷化工有限公司,含量大于98.0%,下述实施例同。但并不因此限定本发明,本领域技术人员可采用其他来源的茶多酚)20克(g);丙三醇10克(g);羟甲基淀粉8克(g),水47克(g)。 Prepare each component according to the following parts by mass: 10 grams (g) of hydrogenated lecithin; squalene (Shanghai Xinran Biotechnology Co., Ltd., with a content greater than 96.0%, the same as the following examples. But this does not limit the present invention, Those skilled in the art can use other sources of squalene) 5 grams (g); tea polyphenols (Ningbo Youjie Chemical Co., Ltd., content greater than 98.0%, the following examples are the same. But it does not therefore limit the present invention, the present invention Those skilled in the art can use 20 grams (g) of tea polyphenols from other sources; 10 grams (g) of glycerol; 8 grams (g) of hydroxymethyl starch, and 47 grams (g) of water.
制备步骤为: The preparation steps are:
S1.将氢化卵磷脂和角鲨烯与茶多酚组合物溶于丙三醇中,得混合体系; S1. Dissolving the composition of hydrogenated lecithin, squalene and tea polyphenols in glycerol to obtain a mixed system;
S2.将S1所得混合体系高速均化使其充分混匀,得均化的混合体系; S2. Homogenize the mixed system obtained in S1 at high speed to make it fully mixed to obtain a homogenized mixed system;
S3.将稳定剂和水混合得到稳定剂的水溶液,往S2所得均化的混合体系中加入稳定剂的水溶液后搅拌均匀,形成稳定的微粒悬浮液即得含角鲨烯与茶多酚组合物的液态前体脂质体。 S3. Mix the stabilizer and water to obtain an aqueous solution of the stabilizer, add the aqueous solution of the stabilizer to the homogenized mixing system obtained in S2 and stir evenly to form a stable particle suspension to obtain the composition containing squalene and tea polyphenols liquid proliposomes.
实施例2 Example 2
制备步骤同实施例1。称取氢化大豆磷脂10克,10克角鲨烯,15克茶多酚溶于10克丙三醇中,高速均化使其充分混匀,再加入8克羟乙基淀粉溶于47克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 10 grams of hydrogenated soybean lecithin, 10 grams of squalene, 15 grams of tea polyphenols dissolved in 10 grams of glycerol, homogenize at high speed to make it fully mixed, then add 8 grams of hydroxyethyl starch dissolved in 47 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例3 Example 3
制备步骤同实施例1。称取氢化大豆磷脂10克,15克角鲨烯,10克茶多酚溶于10克丙三醇中,高速均化使其充分混匀,再加入8克羟甲基淀粉溶于47克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 10 grams of hydrogenated soybean lecithin, 15 grams of squalene, 10 grams of tea polyphenols dissolved in 10 grams of glycerol, homogenize at high speed to make it fully mixed, then add 8 grams of hydroxymethyl starch dissolved in 47 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例4 Example 4
制备步骤同实施例1。称取氢化大豆磷脂10克,5克角鲨烯,20克茶多酚溶于10克丙三醇中,高速均化使其充分混匀,再加入8克羟丙基淀粉溶于47克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 10 grams of hydrogenated soybean lecithin, 5 grams of squalene, 20 grams of tea polyphenols dissolved in 10 grams of glycerin, homogenize at high speed to make it fully mixed, then add 8 grams of hydroxypropyl starch dissolved in 47 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例5 Example 5
制备步骤同实施例1。称取氢化卵磷脂8克,5克角鲨烯,25克茶多酚溶于12克丙三醇中,高速均化使其充分混匀,再加入10克羟乙基淀粉溶于40克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated lecithin, 5 grams of squalene, and dissolve 25 grams of tea polyphenols in 12 grams of glycerol, homogenize at a high speed to fully mix, then add 10 grams of hydroxyethyl starch and dissolve in 40 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例6 Example 6
制备步骤同实施例1。称取氢化大豆磷脂8克,10克角鲨烯,20克茶多酚溶于12克丙三醇中,高速均化使其充分混匀,再加入10克羟丙基淀粉溶于40克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean lecithin, 10 grams of squalene, 20 grams of tea polyphenols dissolved in 12 grams of glycerin, homogenize at a high speed to fully mix, then add 10 grams of hydroxypropyl starch dissolved in 40 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例7 Example 7
制备步骤同实施例1。称取氢化大豆磷脂8克,15克角鲨烯,15克茶多酚溶于12克丙三醇中,高速均化使其充分混匀,再加入10克羟甲基淀粉溶于40克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean lecithin, 15 grams of squalene, and 15 grams of tea polyphenols dissolved in 12 grams of glycerin, homogenize at a high speed to fully mix, then add 10 grams of hydroxymethyl starch dissolved in 40 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例8 Example 8
制备步骤同实施例1。称取氢化大豆磷脂8克,20克角鲨烯,10克茶多酚溶于12克丙三醇中,高速均化使其充分混匀,再加入10克羟乙基淀粉溶于40克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean phospholipids, 20 grams of squalene, 10 grams of tea polyphenols dissolved in 12 grams of glycerin, homogenize at a high speed to fully mix, then add 10 grams of hydroxyethyl starch dissolved in 40 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例9 Example 9
制备步骤同实施例1。称取氢化大豆磷脂8克,25克角鲨烯,5克茶多酚溶于12克丙三醇中,高速均化使其充分混匀,再加入10克羟丙基淀粉溶于40克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean lecithin, 25 grams of squalene, 5 grams of tea polyphenols dissolved in 12 grams of glycerin, homogenize at high speed to make it fully mixed, then add 10 grams of hydroxypropyl starch dissolved in 40 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例10 Example 10
制备步骤同实施例1。称取氢化大豆磷脂7克,5克角鲨烯,35克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入12克羟丙基淀粉溶于26克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 7 grams of hydrogenated soybean lecithin, 5 grams of squalene, and dissolve 35 grams of tea polyphenols in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 12 grams of hydroxypropyl starch dissolved in 26 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例11 Example 11
制备步骤同实施例1。称取氢化卵磷脂7克,10克角鲨烯,30克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入12克羟乙基淀粉溶于26克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 7 grams of hydrogenated lecithin, 10 grams of squalene, and dissolve 30 grams of tea polyphenols in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 12 grams of hydroxyethyl starch dissolved in 26 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例12 Example 12
制备步骤同实施例1。称取氢化卵磷脂7克,15克角鲨烯,25克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入12克羟甲基淀粉溶于26克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 7 grams of hydrogenated lecithin, 15 grams of squalene, and dissolve 25 grams of tea polyphenols in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 12 grams of hydroxymethyl starch and dissolve in 26 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例13 Example 13
制备步骤同实施例1。称取氢化卵磷脂7克,20克角鲨烯,20克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入12克羟甲基淀粉溶于26克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 7 grams of hydrogenated lecithin, 20 grams of squalene, and 20 grams of tea polyphenols dissolved in 15 grams of glycerin, homogenize at a high speed to fully mix, then add 12 grams of hydroxymethyl starch dissolved in 26 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例14 Example 14
制备步骤同实施例1。称取氢化大豆磷脂7克,30克角鲨烯,10克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入12克羟乙基淀粉溶于26克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 7 grams of hydrogenated soybean lecithin, 30 grams of squalene, 10 grams of tea polyphenols dissolved in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 12 grams of hydroxyethyl starch dissolved in 26 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例15 Example 15
制备步骤同实施例1。称取氢化卵磷脂7克,35克角鲨烯,5克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入12克羟丙基淀粉溶于26克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 7 grams of hydrogenated lecithin, 35 grams of squalene, 5 grams of tea polyphenols dissolved in 15 grams of glycerin, homogenize at a high speed to fully mix, then add 12 grams of hydroxypropyl starch dissolved in 26 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例16 Example 16
制备步骤同实施例1。称取氢化大豆磷脂8克,5克角鲨烯,40克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入10克羟甲基淀粉溶于22克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean lecithin, 5 grams of squalene, 40 grams of tea polyphenols dissolved in 15 grams of glycerin, homogenize at high speed to make it fully mixed, then add 10 grams of hydroxymethyl starch dissolved in 22 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例17 Example 17
制备步骤同实施例1。称取氢化大豆磷脂8克,10克角鲨烯,35克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入10克羟乙基淀粉溶于22克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean phospholipids, 10 grams of squalene, 35 grams of tea polyphenols dissolved in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 10 grams of hydroxyethyl starch dissolved in 22 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例18 Example 18
制备步骤同实施例1。称取氢化大豆磷脂8克,20克角鲨烯,25克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入10克羟丙基淀粉溶于22克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean lecithin, 20 grams of squalene, and 25 grams of tea polyphenols dissolved in 15 grams of glycerin, homogenize at a high speed to fully mix, then add 10 grams of hydroxypropyl starch dissolved in 22 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例19 Example 19
制备步骤同实施例1。称取氢化卵磷脂8克,30克角鲨烯,15克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入10克羟甲基淀粉溶于22克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated lecithin, 30 grams of squalene, and dissolve 15 grams of tea polyphenols in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 10 grams of hydroxymethyl starch and dissolve in 22 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例20 Example 20
制备步骤同实施例1。称取氢化大豆磷脂8克,35克角鲨烯,10克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入10克羟甲基淀粉溶于22克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated soybean phospholipids, 35 grams of squalene, 10 grams of tea polyphenols dissolved in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 10 grams of hydroxymethyl starch dissolved in 22 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
实施例21 Example 21
制备步骤同实施例1。称取氢化卵磷脂8克,40克角鲨烯,5克茶多酚溶于15克丙三醇中,高速均化使其充分混匀,再加入10克羟甲基淀粉溶于22克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。 The preparation steps are the same as in Example 1. Weigh 8 grams of hydrogenated lecithin, 40 grams of squalene, 5 grams of tea polyphenols dissolved in 15 grams of glycerol, homogenize at a high speed to fully mix, then add 10 grams of hydroxymethyl starch dissolved in 22 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained.
将上述实施例1~21制备得到的液态前体脂质体检测结果如下:采用激光散射法检测,实施例1~21制备得到的液态前体脂质体粒径为65~100nm,分布均匀,呈正态性,跨距小。 The detection results of the liquid proliposomes prepared in the above-mentioned Examples 1-21 are as follows: detection by laser light scattering method, the particle size of the liquid proliposomes prepared in Examples 1-21 is 65-100 nm, and the distribution is uniform. It is normal and the span is small.
采用透析法分离方法将溶液中游离的角鲨烯与茶多酚和脂质体分离,分别测定、计算包封率。按照(脂质体中角鲨烯与茶多酚组合物质量/脂质体中角鲨烯与茶多酚组合物总质量)×100%计算包封率。本发明实施例1~21制备得到的液态前体脂质体包封率为88%以上。 The free squalene in the solution was separated from tea polyphenols and liposomes by dialysis separation method, and the encapsulation efficiency was measured and calculated respectively. The encapsulation efficiency was calculated according to (mass of squalene and tea polyphenol composition in liposome/total mass of squalene and tea polyphenol composition in liposome)×100%. The encapsulation efficiency of the liquid proliposomes prepared in Examples 1-21 of the present invention is above 88%.
对比例1 Comparative example 1
制备步骤同实施例1。称取氢化卵磷脂5克,40克角鲨烯,5克茶多酚溶于20克丙三醇中,高速均化使其充分混匀,再加入5克羟甲基淀粉溶于25克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。制备得到的液态前体脂质体粒径为190~370nm,分布不均匀。包封率为57%。 The preparation steps are the same as in Example 1. Weigh 5 grams of hydrogenated lecithin, 40 grams of squalene, 5 grams of tea polyphenols dissolved in 20 grams of glycerol, homogenize at a high speed to fully mix, then add 5 grams of hydroxymethyl starch dissolved in 25 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained. The particle size of the prepared liquid proliposome is 190-370 nm, and the distribution is uneven. The encapsulation efficiency was 57%.
对比例2 Comparative example 2
称取脑磷脂7克,35克角鲨烯,5克茶多酚溶于15克丙二醇中,高速均化使其充分混匀,再加入12克羟丙基甲基纤维素溶于26克水的水溶液,搅拌均匀,形成稳定的微粒悬浮液,即得含有抗氧化剂角鲨烯与茶多酚组合物的液态前体脂质体。制备得到的液态前体脂质体粒径为310~580nm,分布不均匀。包封率为41%。 Weigh 7 grams of cephalin, 35 grams of squalene, and dissolve 5 grams of tea polyphenols in 15 grams of propylene glycol, homogenize at a high speed to fully mix, then add 12 grams of hydroxypropyl methylcellulose dissolved in 26 grams of water The aqueous solution is stirred evenly to form a stable particle suspension, and the liquid proliposome containing the antioxidant squalene and tea polyphenol composition is obtained. The particle size of the prepared liquid proliposome is 310-580 nm, and the distribution is uneven. The encapsulation efficiency was 41%.
实施例22 应用实验 Example 22 Application experiment
将上述实施例1~21的液态前体脂质体装入两端为防水防尘透气膜的空心圆柱体中,每粒装入1克。在卷烟滤嘴棒成型过程中,置于醋酸纤维的卷烟过滤嘴中,每支卷烟过滤嘴内置1粒,得到可降低卷烟气相自由基危害的水烟型过滤嘴。以不含角鲨烯或茶多酚的100%液态前体脂质体为对照。 The liquid proliposomes of the above-mentioned Examples 1-21 are packed into hollow cylinders with waterproof, dustproof and gas-permeable membranes at both ends, and each capsule is filled with 1 gram. During the forming process of the cigarette filter tip, it is placed in the cigarette filter tip of acetate fiber, and one piece is built in each cigarette filter tip to obtain a hookah-type filter tip capable of reducing the damage of free radicals in the gas phase of the cigarette. A 100% liquid proliposome without squalene or tea polyphenols was used as a control.
卷烟烟气中自由基清除效果检测:烟气气相自由基采用自旋捕集剂PBN(2-苯叔丁基硝酮)捕集后检测。 Detection of free radical scavenging effect in cigarette smoke: free radicals in smoke gas phase were captured by spin trapping agent PBN (2-phenyl-tert-butylnitrone) and detected.
采用常规的气相自由基检测方法:采用玻璃器皿收集烟气自由基。加一定浓度的自由基捕捉剂PBN的四氯化碳溶液到收集器中,将收集器连到吸烟机上,以抽吸容量为35.0mL,抽吸时间为2s,抽吸间隔为60s的标准抽吸速率抽吸卷烟。吸烟后定容收集到烟气自由基溶液,而后放入液氮中冷冻。检测体积为200μL。 The conventional gas-phase free radical detection method is adopted: glassware is used to collect smoke free radicals. Add a certain concentration of carbon tetrachloride solution of the free radical scavenger PBN to the collector, connect the collector to the smoking machine, and use a standard smoking with a suction volume of 35.0mL, a suction time of 2s, and a suction interval of 60s. Smoking rate for smoking cigarettes. After smoking, the smoke free radical solution was collected at a constant volume, and then frozen in liquid nitrogen. The assay volume was 200 μL.
通过检测添加不同含量和不同配比的天然抗氧化剂增效组合物液态前体脂质体的过滤嘴的卷烟产自由基的含量,与对照相比,计算组合物对卷烟烟气中气相自由基的清除效果。实验结果见表1: By detecting the content of free radicals produced by cigarettes added with different contents and different ratios of natural antioxidant synergistic composition liquid proliposomes, compared with the control, the effect of the composition on gas phase free radicals in cigarette smoke is calculated. Clear effect. The experimental results are shown in Table 1:
表1 : Table 1 :
实验结论:从上述实施例对卷烟气相自由基清除效果可以看出,当液态前体脂质体中含天然抗氧化剂的量在25~45%左右时,其对气相自由具有较好的清除效果,特别是当角鲨烯与茶多酚的配比在1∶8~8∶1之间,尤其在2∶7~7∶2之间时,组合物对气相自由基清除效果具有明显的增效作用,其清除自由基的能力随着抗氧化剂的量的增加而增强。根据生产实际,本发明用于卷烟过滤嘴中的天然抗氧化剂组合物的液态前体脂质体中含角鲨烯和茶多酚在30~45%左右,角鲨烯和茶多酚的配比在2∶7~7∶2之间其对气相自由基的清除能力增效作用明显。 Experimental conclusion: From the above examples on the scavenging effect of cigarette gas phase free radicals, it can be seen that when the amount of natural antioxidants contained in the liquid proliposome is about 25-45%, it has a better scavenging effect on gas phase free radicals , especially when the proportioning ratio of squalene and tea polyphenols is between 1:8~8:1, especially between 2:7~7:2, the composition has obvious effect on gas phase free radical scavenging The effect is that its ability to scavenge free radicals is enhanced with the increase of the amount of antioxidants. According to actual production, squalene and tea polyphenols are contained in liquid proliposomes of the natural antioxidant composition used in cigarette filters at about 30% to 45%, and the ratio of squalene and tea polyphenols is The synergistic effect on the scavenging ability of gas phase free radicals is obvious between 2:7 and 7:2.
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