[go: up one dir, main page]

CN117338654A - A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof - Google Patents

A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof Download PDF

Info

Publication number
CN117338654A
CN117338654A CN202311224299.4A CN202311224299A CN117338654A CN 117338654 A CN117338654 A CN 117338654A CN 202311224299 A CN202311224299 A CN 202311224299A CN 117338654 A CN117338654 A CN 117338654A
Authority
CN
China
Prior art keywords
gel
salicornia
parts
mosquito
salicornia bigelovii
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN202311224299.4A
Other languages
Chinese (zh)
Inventor
王笃军
许婷婷
朱佳怡
金志锋
朱雨萍
周美琳
张乐萱
余晓红
张春银
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yancheng Institute of Technology
Original Assignee
Yancheng Institute of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yancheng Institute of Technology filed Critical Yancheng Institute of Technology
Priority to CN202311224299.4A priority Critical patent/CN117338654A/en
Publication of CN117338654A publication Critical patent/CN117338654A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • 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
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • 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
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/81Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
    • A61K8/8141Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • A61K8/8147Homopolymers or copolymers of acids; Metal or ammonium salts thereof, e.g. crotonic acid, (meth)acrylic acid; Compositions of derivatives of such polymers
    • 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
    • A61K8/92Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
    • A61K8/922Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P17/00Drugs for dermatological disorders
    • A61P17/04Antipruritics
    • 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
    • A61Q17/02Barrier 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 containing insect repellants
    • 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
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/59Mixtures
    • A61K2800/592Mixtures of compounds complementing their respective functions
    • A61K2800/5922At least two compounds being classified in the same subclass of A61K8/18
    • 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
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

Landscapes

  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Veterinary Medicine (AREA)
  • Public Health (AREA)
  • General Health & Medical Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • Birds (AREA)
  • Epidemiology (AREA)
  • Engineering & Computer Science (AREA)
  • Dermatology (AREA)
  • Chemical & Material Sciences (AREA)
  • Plant Pathology (AREA)
  • Microbiology (AREA)
  • Botany (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Emergency Medicine (AREA)
  • Pest Control & Pesticides (AREA)
  • Mycology (AREA)
  • Biotechnology (AREA)
  • Bioinformatics & Cheminformatics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Nuclear Medicine, Radiotherapy & Molecular Imaging (AREA)
  • Organic Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Cosmetics (AREA)

Abstract

The invention discloses a Salicornia europaea mosquito-repellent itching-relieving gel and a preparation method thereof, wherein the Salicornia europaea mosquito-repellent itching-relieving gel comprises, by weight, 20-25 parts of Salicornia europaea juice, 0.3-0.5 part of wormwood extract, 0.5-0.6 part of peppermint oil, 0.6-0.7 part of carbomer, 4-5 parts of propylene glycol, 4-5 parts of glycerin, 1-2 parts of pH regulator, 1-2 parts of penetration enhancer, 0.1 part of preservative and 18-20 parts of deionized water. The Salicornia bigelovii mosquito-repellent itching-relieving gel has the characteristics of better mosquito-repellent, itching-relieving, detumescence and the like, has the advantages of natural and harmless raw materials, small skin irritation, quick drug absorption, lasting drug effect and the like, and is friendly to sensitive skin people. The product not only improves the high-value utilization of the medicinal and edible halophyte resource Salicornia bigelovii, but also widens the variety of mosquito-repellent itching-relieving products in the market, and has wide market prospect.

Description

一种海蓬子驱蚊止痒凝胶剂及其制备方法A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof

技术领域Technical field

本发明属于日用化工产品领域,具体涉及一种海蓬子驱蚊止痒凝胶剂及其制备方法。The invention belongs to the field of daily chemical products, and specifically relates to a samphire mosquito repellent and antipruritic gel and a preparation method thereof.

背景技术Background technique

海蓬子属藜科(Chenopodiaceae)盐角草属(Salicornia),俗称海芦笋或海豆,该属分布在全世界,数量大约有五十多个种,它生长于盐碱地,可直接用盐水灌溉海蓬子的生命力很强,繁殖能力也很强。海蓬子作为一种食药两用的植物,《中华本草》中有相关记载,它对于血压、头痛、肝阴虚等方面都有很好的效果。海蓬子含有多种活性成分,如黄酮、生物碱、甾体等,作为一种传统的中草药,已用于平肝、降脂降压、活血抗炎、缓解便秘等问题,海蓬子还有减肥的功效。海蓬子还被用于治疗皮肤瘙痒以及皮疹等皮肤疾病。近年来,研究表明海蓬子可以抑制细胞凋亡,其可以使人皮肤纤维细胞不受到叔丁基过氧化氢的氧化。同时,海蓬子提取物能减少人体中黑色素的合成,其可以抑制酪氨酸酶的活性。因此,无论在食品应用领域还是在药用领域海蓬子都存在巨大潜能作用。Salicornia belongs to the genus Salicornia of the family Chenopodiaceae, and is commonly known as sea asparagus or sea beans. This genus is distributed all over the world and has about fifty species. It grows in saline-alkali soil and can be irrigated directly with salt water. Samphire has a strong vitality and reproductive capacity. As a plant with dual uses as food and medicine, samphire is recorded in "Chinese Materia Medica". It has good effects on blood pressure, headaches, liver yin deficiency, etc. Salicornia contains a variety of active ingredients, such as flavonoids, alkaloids, steroids, etc. As a traditional Chinese herbal medicine, it has been used to calm the liver, lower lipids and blood pressure, activate blood circulation and fight inflammation, relieve constipation and other problems. Salicornia also It has the effect of losing weight. Salicornia is also used to treat skin conditions such as itchy skin and rashes. In recent years, studies have shown that Salicornia can inhibit apoptosis and protect human skin fibroblasts from oxidation by tert-butyl hydroperoxide. At the same time, samphire extract can reduce the synthesis of melanin in the human body, which can inhibit the activity of tyrosinase. Therefore, Salicornia has great potential in both food applications and medicinal applications.

凝胶剂是一种粘稠液体或半固态制剂,通过与合适的基质结合而成,具有一定的凝胶性质。凝胶剂成分包括基质、辅料和主药。凝胶剂有许多优点,与软膏剂、霜剂、擦剂等常见的外用制剂不一样,凝胶剂不像在使用软膏剂和霜剂时会涂抹不均匀,导致污染衣物;也不像洗剂和擦剂,挥发性强、易流散。凝胶剂一般质地细腻稳定,流动性适中,可以很方便的涂抹在皮肤上,有较强附着性,人体吸收速度快,不刺激皮肤和粘膜,而且制备工艺简单方便。此外,可以和凝胶剂基质所结合的药物类型较广,包括结晶状态或粉末状的化学药物、中药材粉末或提取物等。A gel is a viscous liquid or semi-solid preparation that is combined with a suitable matrix and has certain gel properties. Gel ingredients include base, excipients and main drug. Gels have many advantages. Unlike common external preparations such as ointments, creams, and liniments, gels do not apply unevenly when using ointments and creams, causing contamination of clothes; Agents and liniments, highly volatile and easy to spread. Gels generally have a fine and stable texture, moderate fluidity, can be easily applied to the skin, have strong adhesion, are quickly absorbed by the human body, do not irritate the skin and mucous membranes, and the preparation process is simple and convenient. In addition, a wide range of drugs can be combined with the gel matrix, including crystalline or powdered chemical drugs, Chinese herbal medicine powders or extracts, etc.

但目前对海蓬子相关驱蚊产品的研究尚未见报道。However, there have been no reports on research on samphire-related mosquito repellent products.

发明内容Contents of the invention

针对现有技术的不足,本发明提供一种海蓬子驱蚊止痒凝胶剂及其制备方法,具有原料天然无害,对皮肤刺激性小,药物吸收快及药效持久等优点。In view of the shortcomings of the existing technology, the present invention provides a samphire mosquito repellent and anti-itching gel and a preparation method thereof, which have the advantages of natural and harmless raw materials, little irritation to the skin, fast drug absorption and long-lasting drug effect.

本发明是通过以下技术方案实现的:The present invention is achieved through the following technical solutions:

一种海蓬子驱蚊止痒凝胶剂,按重量份包括海蓬子汁20~25份、艾草提取物0.3~0.5份、薄荷素油0.5~0.6份、卡波姆0.6~0.7份、丙二醇4~5份、甘油4~5份、pH调节剂1~2份、促渗透剂1~2份、防腐剂0.1份、去离子水18~20份;其中,海蓬子汁、艾草提取物和薄荷素油为凝胶剂原料;卡波姆为凝胶剂基质;丙二醇和甘油为保湿剂。A kind of samphire mosquito repellent and anti-pruritic gel contains, by weight, 20 to 25 parts of samphire juice, 0.3 to 0.5 parts of mugwort extract, 0.5 to 0.6 parts of peppermint oil, and 0.6 to 0.7 parts of carbomer. 4 to 5 parts of propylene glycol, 4 to 5 parts of glycerin, 1 to 2 parts of pH regulator, 1 to 2 parts of penetration enhancer, 0.1 part of preservative, 18 to 20 parts of deionized water; among them, samphire juice, mugwort Extract and peppermint oil are the raw materials of the gel; carbomer is the gel base; propylene glycol and glycerin are the moisturizers.

优选地,所述pH调节剂为三乙醇胺,所述促渗透剂为氮酮,所述防腐剂为苯甲酸钠。Preferably, the pH adjuster is triethanolamine, the penetration enhancer is azone, and the preservative is sodium benzoate.

一种海蓬子驱蚊止痒凝胶剂的制备方法,包括以下步骤:A preparation method of Samphire mosquito repellent and anti-itch gel, including the following steps:

步骤1)原料预处理:采集新鲜海篷子,洗净,晾干水分,备用;取新鲜艾草地上部分,清理,室温晾干后干燥,粉碎后备用;取新鲜薄荷,清理,干燥,切割成短段备用;Step 1) Preprocessing of raw materials: collect fresh seaweed, wash, dry and set aside; take the above-ground part of fresh mugwort, clean it, dry it at room temperature, crush it and set aside; take fresh mint, clean, dry and cut it into short sections for later use;

步骤2)海蓬子汁的制备:取沥干水分的新鲜海蓬子,破碎榨汁,汁液过滤去除残渣,加入维生素C,制得海蓬子汁备用;Step 2) Preparation of samphire juice: take the drained fresh samphire juice, crush it and squeeze the juice, filter the juice to remove the residue, add vitamin C, and prepare samphire juice for later use;

步骤3)艾草提取物的制备:采用超临界CO2流体萃取技术制备,取经步骤1)处理后的艾草均匀填充于萃取反应釜中,利用CO2反复冲洗去除管道中的空气;将液化后的CO2通过高频柱塞泵泵入混合器,调控参数,制得艾草提取物备用;Step 3) Preparation of mugwort extract: Prepared by supercritical CO 2 fluid extraction technology. Take the mugwort treated in step 1) and fill it evenly into the extraction reaction kettle. Use CO 2 to repeatedly flush the air in the pipeline; liquefy it. The final CO 2 is pumped into the mixer through a high-frequency plunger pump, the parameters are adjusted, and the mugwort extract is prepared for later use;

步骤4)薄荷素油的制备:采用蒸煮法制备,取薄荷原料,按照料液比1:8的比例进行提取,保持微沸状态4h以上,制备得到的薄荷素油用无水硫酸钠进行干燥过滤,备用;Step 4) Preparation of peppermint oil: Prepare by cooking method, take mint raw materials, extract according to the ratio of material to liquid ratio 1:8, keep it in a slightly boiling state for more than 4 hours, and dry and filter the prepared peppermint oil with anhydrous sodium sulfate. spare;

步骤5)海蓬子凝胶剂的制备:按重量份称取卡波姆、丙二醇、甘油、三乙醇胺、氮酮、苯甲酸钠和去离子水;将卡波姆均匀的撒在去离子水表面,静置溶胀24h;依次将相应量的丙二醇、甘油、氮酮、苯甲酸钠,以及步骤1)至步骤3)制得的海蓬子汁、艾草提取物与薄荷素油加入凝胶剂基质中,每次加入试剂用混匀器搅拌均匀后再加入下一种试剂,最后缓慢加入蒸馏水,搅拌均匀,制得海蓬子凝胶剂;Step 5) Preparation of samphire gel: Weigh carbomer, propylene glycol, glycerin, triethanolamine, azone, sodium benzoate and deionized water in parts by weight; sprinkle the carbomer evenly on the surface of the deionized water , leave to swell for 24 hours; add corresponding amounts of propylene glycol, glycerin, azone, sodium benzoate, and the samphire juice, mugwort extract and mentha oil prepared in steps 1) to 3) into the gel matrix in sequence , add the reagent each time and stir it evenly with a mixer before adding the next reagent. Finally, slowly add distilled water and stir evenly to prepare the samphire gel;

步骤6)海蓬子凝胶剂的pH值调控:利用三乙醇胺对步骤5)制得的海蓬子凝胶剂的pH值进行调整,搅拌均匀,调至pH值为6-8即可;Step 6) Adjusting the pH value of the samphire gel: Use triethanolamine to adjust the pH value of the samphire gel prepared in step 5), stir evenly, and adjust the pH value to 6-8;

步骤7)将经步骤6)处理的海蓬子凝胶剂进行氢过氧化物凝胶灭菌,制得翠绿色透明凝胶,灌装后即得海蓬子驱蚊止痒凝胶剂成品。Step 7) Sterilize the samphire gel treated in step 6) with hydroperoxide gel to obtain a green transparent gel. After filling, the finished product of samphire repellent and anti-itch gel is obtained .

优选地,步骤2)所述维生素C的添加量为0.5g/kg海蓬子。Preferably, the amount of vitamin C added in step 2) is 0.5g/kg samphire.

优选地,步骤3)所述调控参数的设置如下:控制CO2流量为25L/h,反应釜分离压力I设定为10±0.2MPa,温度为55℃,分离压力II设定为7±0.2MPa,温度为55℃。Preferably, the settings of the control parameters in step 3) are as follows: control the CO 2 flow rate to 25L/h, set the reactor separation pressure I to 10±0.2MPa, set the temperature to 55°C, and set the separation pressure II to 7±0.2 MPa, the temperature is 55℃.

优选地,步骤5)所述加入蒸馏水的量为:按重量份定容至50份。Preferably, the amount of distilled water added in step 5) is: dilute to 50 parts by weight.

优选地,步骤7)所述海蓬子驱蚊止痒凝胶剂成品的重量为50g。Preferably, the weight of the finished samphire mosquito repellent and anti-itch gel in step 7) is 50g.

本发明的有益效果如下:The beneficial effects of the present invention are as follows:

本发明基于对海蓬子、艾草及薄荷药性特点,灵活运用活性成分协同增效的原理探索配方及生产工艺。主要利用药食同源资源——海蓬子的抗菌、消炎、消肿、止痒等特点,艾草的芳香通窍、活络通筋、刺激局部的血液循环作用,结合薄荷解毒透疹、清凉止痒的功效制备驱蚊止痒凝胶剂。本发明的海蓬子驱蚊止痒凝胶剂具有较好的驱蚊、止痒、消肿等特点,具备原料天然无害,对皮肤刺激性小,药物吸收快以及药效持久等优点,且对敏感型皮肤人群友好。该产品不仅提高了药食同源盐生植物资源海蓬子的高值化利用,也拓宽了市场上驱蚊止痒产品的种类,具有广阔的市场前景。The present invention is based on the medicinal properties of Salicornia, mugwort and mint, and flexibly uses the principle of synergy of active ingredients to explore the formula and production process. It mainly uses medicinal and food resources - the antibacterial, anti-inflammatory, detumescent, antipruritic and other characteristics of samphire, the aroma of mugwort, which can stimulate the orifices, activate collaterals and tendons, and stimulate local blood circulation, combined with the detoxifying, rash-relieving, cooling and soothing effects of mint. Efficacy of Itching Prepare mosquito repellent and anti-itch gel. The samphire mosquito repellent and anti-pruritic gel of the present invention has the characteristics of better mosquito repellent, anti-itching, and swelling reduction, and has the advantages of natural and harmless raw materials, little irritation to the skin, fast drug absorption, and long-lasting drug effect. And friendly to people with sensitive skin. This product not only improves the high-value utilization of samphire, a homologous medicinal and edible halophyte resource, but also broadens the types of mosquito repellent and anti-pruritic products on the market, and has broad market prospects.

附图说明Description of drawings

图1为实施例2中芦丁标准曲线;Figure 1 is the rutin standard curve in Example 2;

图2为实施例3中体外透皮实验空白接收液色谱图;Figure 2 is a chromatogram of the blank receiving solution in the in vitro transdermal experiment in Example 3;

图3为实施例3中体外透皮实验第2h接受液的色谱图;Figure 3 is a chromatogram of the receiving solution at the 2nd hour of the in vitro transdermal experiment in Example 3;

图4为实施例3中体外透皮实验经过12h后皮肤中芦丁色谱图。Figure 4 is a chromatogram of rutin in the skin after 12 hours of the in vitro transdermal experiment in Example 3.

具体实施方式Detailed ways

下面结合附图与具体实施例对本发明做进一步详细说明。The present invention will be further described in detail below in conjunction with the accompanying drawings and specific embodiments.

若无特殊说明,以下实施例中所用的技术手段,均为本领域技术人员所熟知的常规手段,未注明具体条件的实验方法,均为本领域常规方法。Unless otherwise specified, the technical means used in the following examples are conventional means well known to those skilled in the art. Experimental methods without specifying specific conditions are all conventional methods in the art.

以下实施例中所用的材料、试剂等,如无特殊说明,均可从商业途径得到。The materials, reagents, etc. used in the following examples can all be obtained from commercial sources unless otherwise specified.

以下实施例中所用实验动物为昆明小鼠,购自北京维通利华公司实验动物技术有限公司。The experimental animals used in the following examples were Kunming mice, purchased from Beijing Vitong Lever Laboratory Animal Technology Co., Ltd.

实施例1Example 1

一种海蓬子驱蚊止痒凝胶剂,配方如下:海蓬子汁20~25g、艾草提取物0.3~0.5g、薄荷素油0.5~0.6g、卡波姆0.6~0.7g、丙二醇4~5g、甘油4~5g、三乙醇胺1~2g、氮酮1~2g、苯甲酸钠0.1g、去离子水18~20g。A kind of samphire mosquito repellent and anti-pruritic gel, the formula is as follows: 20-25g samphire juice, 0.3-0.5g mugwort extract, 0.5-0.6g menthae oil, 0.6-0.7g carbomer, propylene glycol 4 ~5g, glycerin 4~5g, triethanolamine 1~2g, azone 1~2g, sodium benzoate 0.1g, deionized water 18~20g.

一种海蓬子驱蚊止痒凝胶剂的制备方法,具体步骤如下:A method for preparing a samphire mosquito repellent and antipruritic gel. The specific steps are as follows:

(1)原料预处理:采集新鲜的海篷子,洗净泥沙后晾干水分,备用;新鲜艾草地上部分清理掉泥沙等杂质,室温晾干后用真空干燥箱干燥,粉碎后备用;新鲜的薄荷,去除泥沙等杂质后,真空干燥箱进行干燥,切割成5mm短段备用。(1) Raw material pretreatment: Collect fresh seaweed, wash the sediment and dry the water, and set aside; clean the upper part of the fresh mugwort grass to remove sediment and other impurities, dry it at room temperature, dry it in a vacuum drying oven, crush it and set aside ; Fresh mint, after removing sediment and other impurities, dry it in a vacuum drying oven, and cut it into 5mm short sections for later use.

(2)海蓬子活性物质(海蓬子汁)的制备:取沥干水分的新鲜海蓬子用破壁机破碎榨汁,汁液用滤纸进行过滤,去除残渣,加入一定量维生素C用于护色,添加量为0.5g/kg海蓬子,保证产品的翠绿色及透光度。(2) Preparation of the active substance of Salicornia samphire (Samphire samphire juice): Take the drained fresh samphire samphire and crush it with a wall breaker to squeeze the juice. Filter the juice with filter paper to remove the residue and add a certain amount of vitamin C for use. For color protection, the added amount is 0.5g/kg samphire to ensure the green color and light transmittance of the product.

(3)艾草提取物(艾草精油)的制备:采用超临界CO2流体萃取技术制备艾草精油,取适量艾草均匀填充于萃取反应釜中,利用CO2反复冲洗去除管道中的空气。将液化后的CO2通过高频柱塞泵泵入混合器,控制CO2流量为25L/h,反应釜分离压力I设定为10±0.2MPa,温度为55℃,分离压力II设定为7±0.2MPa,温度为55℃,制备艾草精油备用。(3) Preparation of wormwood extract (wormwood essential oil): Use supercritical CO 2 fluid extraction technology to prepare wormwood essential oil, take an appropriate amount of wormwood and evenly fill it in the extraction reaction kettle, and use CO 2 to repeatedly flush to remove the air in the pipeline . Pump the liquefied CO2 into the mixer through a high-frequency plunger pump, control the CO2 flow rate to 25L/h, set the reactor separation pressure I to 10±0.2MPa, set the temperature to 55°C, and set the separation pressure II to 7± 0.2MPa, the temperature is 55℃, prepare mugwort essential oil for later use.

(4)薄荷素油的制备:采用蒸煮法制备薄荷素油,取适量薄荷原料,按照料液比1:8的比例进行提取,保持微沸状态4h以上,制备得到的薄荷素油用无水硫酸钠进行干燥过滤,备用。(4) Preparation of peppermint oil: Use the cooking method to prepare peppermint oil, take an appropriate amount of peppermint raw materials, extract according to the ratio of material to liquid ratio 1:8, keep it in a slightly boiling state for more than 4 hours, and use anhydrous sodium sulfate to prepare the peppermint oil. Dry, filter and set aside.

(5)海蓬子凝胶剂制作工艺:将卡波姆均匀的撒在去离子水表面,静置溶胀24h。依次将相应量的丙二醇、甘油、氮酮、苯甲酸钠、海蓬子活性物质、艾草精油与薄荷素油加入凝胶剂基质中,每次加入试剂用混匀器搅拌均匀后再加入下一种试剂,最后缓慢加入蒸馏水至50g,搅拌均匀,制成海蓬子凝胶剂。(5) Salicornia gel production process: Sprinkle carbomer evenly on the surface of deionized water and let it stand for 24 hours to swell. Add corresponding amounts of propylene glycol, glycerin, azone, sodium benzoate, samphire active substances, mugwort essential oil and mentha oil into the gel matrix in turn. Stir evenly with a mixer each time you add the reagent before adding the next one. reagent, and finally slowly add distilled water to 50g, stir evenly, and prepare a samphire gel.

(6)海蓬子凝胶剂的pH值调控:利用三乙醇胺对海蓬子凝胶剂的pH值进行调整,搅拌均匀,调至pH值为6-8即可。(6) Adjusting the pH value of the samphire gel: Use triethanolamine to adjust the pH value of the samphire gel, stir evenly, and adjust the pH value to 6-8.

(7)将上述制备的海蓬子凝胶剂进行氢过氧化物凝胶灭菌,制得翠绿色透明凝胶,灌装后得到海蓬子驱蚊止痒凝胶剂成品。(7) The samphire gel prepared above is sterilized by hydroperoxide gel to obtain an emerald green transparent gel. After filling, the finished samphire repellent and anti-itch gel product is obtained.

本实施例的凝胶剂配方及制备方法是通过实施例2的相关实验确定的。The gel formula and preparation method of this embodiment were determined through relevant experiments in Example 2.

实施例2正交优选海蓬子驱蚊止痒凝胶剂基质及验证Example 2 Orthogonal selection of samphire mosquito repellent and antipruritic gel matrix and verification

1、凝胶剂基质的筛选1. Screening of gel matrix

选取凝胶常用基质海藻酸钠、卡波姆940、聚乙烯醇、羧甲基纤维素钠作为凝胶基质筛选对象,取各凝胶基质1g分别加40mL蒸馏水中充分溶胀均匀,静置24h得到不同的凝胶基质。对制备得到的凝胶基质进行评价,以样品的成型、色味、黏稠度、均匀度、涂展性、在3000r·min-1离心稳定性为主要标准进行综合评价,结果见表1。Select commonly used gel matrix sodium alginate, carbomer 940, polyvinyl alcohol, and sodium carboxymethyl cellulose as the gel matrix screening objects. Take 1g of each gel matrix and add 40 mL of distilled water to fully swell evenly, and let it stand for 24 hours to obtain the result. Different gel matrices. The prepared gel matrix was evaluated, and a comprehensive evaluation was conducted based on the main criteria of the sample's molding, color, taste, viscosity, uniformity, spreadability, and centrifugal stability at 3000 r·min -1 . The results are shown in Table 1.

表1凝胶剂基质的综合评价Table 1 Comprehensive evaluation of gel matrix

由表1可知,四种凝胶基质都具有良好的稳定性,海藻酸钠的颜色较为浑浊,聚乙烯醇难溶解,卡波姆940和羧甲基纤维素钠较其他两种基质成型较好、无色无味、黏度适中,但羧甲基纤维素钠的均匀度相比于卡波姆940略差。根据四者的比较结果,确定选取卡波姆940为海蓬子驱蚊止痒凝胶剂的基质。As can be seen from Table 1, the four gel matrices all have good stability. The color of sodium alginate is relatively turbid, polyvinyl alcohol is difficult to dissolve, and carbomer 940 and sodium carboxymethylcellulose are better formed than the other two matrices. , colorless and odorless, with moderate viscosity, but the uniformity of sodium carboxymethyl cellulose is slightly worse than that of carbomer 940. Based on the comparison results between the four, it was determined to select carbomer 940 as the base of the samphire mosquito repellent and anti-itch gel.

2、凝胶剂的处方组成和制备方法2. Prescription composition and preparation method of gel

处方组成:海蓬子活性物、艾叶精油、薄荷素油、桑叶提取物、卡波姆940、丙二醇、甘油、三乙醇胺、氮酮、苯甲酸钠、蒸馏水。Prescription composition: Salicornia active ingredients, mugwort essential oil, peppermint oil, mulberry leaf extract, carbomer 940, propylene glycol, glycerin, triethanolamine, azone, sodium benzoate, distilled water.

制备方法:在制备凝胶剂的24h前按处方要求取卡波姆940置于蒸馏水中充分溶胀。在溶胀后的凝胶剂基质中添加丙二醇和甘油来调整其保湿程度,加入适量氮酮提高其渗透性。加入作为原料的海蓬子活性物、艾叶精油、薄荷素油,然后用三乙醇胺调节凝胶剂的酸碱度,使其pH值在6-8之间,最后加入少量的防腐剂苯甲酸钠。加蒸馏水补充至凝胶剂的固定质量,研磨均匀后即可得到海蓬子驱蚊止痒凝胶剂。Preparation method: 24 hours before preparing the gel, take Carbomer 940 according to the prescription and place it in distilled water to fully swell. Add propylene glycol and glycerin to the swollen gel matrix to adjust its moisturizing degree, and add an appropriate amount of azone to improve its permeability. Add the raw materials of samphire actives, mugwort essential oil, and mentha oil, then use triethanolamine to adjust the pH of the gel to a pH value between 6-8, and finally add a small amount of preservative sodium benzoate. Add distilled water to a fixed mass of the gel, and grind it evenly to obtain a samphire repellent and anti-itch gel.

3、凝胶剂基质的单因素考察实验设计3. Single factor investigation experimental design of gel matrix

经过初步实验设定海蓬子驱蚊止痒凝胶剂的固定质量为50g,其中海蓬子活性物作为凝胶剂原料的固定添加量为40%,艾叶精油、薄荷精油作为辅助剂的固定添加量分别为0.6%和0.6%,甘油作为保湿剂的固定添加量为8%,氮酮作为促渗透剂的固定添加量为1%,苯甲酸钠作为防腐剂的固定添加量为0.2%,并对空白凝胶剂中的卡波姆940、丙二醇、三乙醇胺的用量进行筛选考察。After preliminary experiments, the fixed mass of the samphire mosquito repellent and anti-itch gel is set to 50g, in which the fixed amount of samphire active substance as the raw material of the gel is 40%, and the fixed amount of moxa essential oil and peppermint essential oil as auxiliary agents. The addition amounts are 0.6% and 0.6% respectively, the fixed addition amount of glycerol as a moisturizer is 8%, the fixed addition amount of azone as a penetration enhancer is 1%, the fixed addition amount of sodium benzoate as a preservative is 0.2%, and Screen and investigate the dosage of carbomer 940, propylene glycol, and triethanolamine in the blank gel.

4、凝胶剂基质的综合评价方法4. Comprehensive evaluation method of gel matrix

对凝胶剂基质的评价方法有多个衡量指标,本实施例采用综合评分法对凝胶剂基质的外观、黏度、酸碱度、均匀度、油腻程度五个方面进行分析,下面为五个指标的评分标准,综合评分为五个指标分数相加(总分60分)。There are multiple measurement indicators for evaluating the gel matrix. In this example, a comprehensive scoring method is used to analyze the appearance, viscosity, pH, uniformity, and greasiness of the gel matrix. The following are the five indicators. Scoring standard, the comprehensive score is the sum of the five indicator scores (total score 60 points).

外观:颜色透亮(11~15分);颜色稍浑浊(6~10分);颜色浑浊不透亮(0~5分)。Appearance: color is translucent (11-15 points); color is slightly turbid (6-10 points); color is turbid and opaque (0-5 points).

黏度:黏度适中,倾斜后可较慢流动(11~15分);整体略稀或略稠,倾斜后流动速度过快或过慢(6~10分);太稀或太稠,流动快或不流动(0~5分)。Viscosity: Moderate viscosity, it flows slowly after tilting (11-15 minutes); overall slightly thin or thick, but flows too fast or too slow after tilting (6-10 minutes); too thin or too thick, flows too fast or Not flowing (0 to 5 points).

均匀度:没有明显颗粒,涂抹较为细腻(11~15分);涂开后有些许颗粒存在(6~10分);不易涂开,有明显颗粒或太稀(0~5分)。Uniformity: There are no obvious particles, and the application is relatively delicate (11 to 15 points); there are some particles after spreading (6 to 10 points); it is not easy to spread, there are obvious particles or it is too thin (0 to 5 points).

油腻程度:无明显油腻(11~15分);较油腻或较干燥(6~10分);太油或太稀(0~5分)。Degree of greasiness: not obviously greasy (11 to 15 points); greasy or dry (6 to 10 points); too oily or too thin (0 to 5 points).

酸碱度:pH在6-8范围内(+),pH在6-8范围外(-)。pH: pH is within the range of 6-8 (+), pH is outside the range of 6-8 (-).

(1)卡波姆940的添加量筛选(1) Screening of the amount of carbomer 940 added

在原料和其他辅料固定不变的条件下,由于卡波姆940会对凝胶剂的黏度等方面有所影响,如表2所示,依次以卡波姆940的添加量为0.7%、1.0%、1.3%、1.6%、1.9%为变量,筛选出最优添加量。Under the condition that the raw materials and other auxiliary materials are fixed, since Carbopol 940 will have an impact on the viscosity of the gel, as shown in Table 2, the addition amount of Carbopol 940 is 0.7%, 1.0%, etc. %, 1.3%, 1.6%, and 1.9% are variables, and the optimal addition amount is screened out.

表2卡波姆940添加量设计表Table 2 Carbomer 940 addition amount design table

将表2中的五种样品分别从外观、黏度、均匀度、油腻程度、酸碱度五个指标进行考察,综合评分见表3。The five samples in Table 2 were examined from the five indicators of appearance, viscosity, uniformity, greasiness, and pH. The comprehensive scores are shown in Table 3.

表3卡波姆940添加量综合评分结果Table 3 Comprehensive scoring results of carbomer 940 addition amount

由表3可知,卡波姆940的添加量在1.0%~1.3%时,制成的凝胶剂外观良好、黏度较大、均匀度较好、无明显油腻,酸碱度也在人体可接受范围之内。It can be seen from Table 3 that when the addition amount of carbomer 940 is between 1.0% and 1.3%, the gel produced has a good appearance, high viscosity, good uniformity, no obvious greasiness, and the pH is within the acceptable range of the human body. Inside.

(2)丙二醇的用量筛选(2) Screening of propylene glycol dosage

在原料和其他辅料固定不变的条件下,由于丙二醇会对凝胶剂的油腻程度和均匀度等方面有所影响,如表4所示,依次以丙二醇的添加量为3%、6%、9%、12%、15%为变量,筛选出最优添加量。Under the condition that the raw materials and other auxiliary materials are fixed, since propylene glycol will have an impact on the greasiness and uniformity of the gel, as shown in Table 4, the addition amount of propylene glycol is 3%, 6%, 9%, 12%, and 15% are variables, and the optimal addition amount is screened out.

表4丙二醇添加量设计表Table 4 Propylene glycol addition amount design table

将表4中的五种样品分别从外观、黏度、均匀度、油腻程度、酸碱度五个指标进行考察,综合评分见表5。The five samples in Table 4 were examined from the five indicators of appearance, viscosity, uniformity, greasiness, and pH. The comprehensive scores are shown in Table 5.

表5丙二醇添加量综合评分结果Table 5 Comprehensive scoring results of propylene glycol addition amount

由表5可知,丙二醇的添加量在9%~12%时,状态达到最佳,低于9%或高于12%时油腻性会变差,均匀程度也会降低。It can be seen from Table 5 that when the addition amount of propylene glycol is between 9% and 12%, the state is optimal. When it is lower than 9% or higher than 12%, the greasiness will become worse and the uniformity will also decrease.

(3)三乙醇胺的用量筛选(3) Screening of dosage of triethanolamine

在原料和其他辅料固定不变的条件下,由于三乙醇胺会影响凝胶剂的酸碱度,如表6所示,依次以三乙醇胺的添加量为1.2%、1.5%、1.8%、2.1%、2.4%为变量,筛选出最优添加量。Under the condition that the raw materials and other auxiliary materials are fixed, since triethanolamine will affect the pH of the gel, as shown in Table 6, the addition amount of triethanolamine is 1.2%, 1.5%, 1.8%, 2.1%, and 2.4. % is a variable, and the optimal addition amount is screened out.

表6三乙醇胺添加量设计表Table 6 Triethanolamine addition amount design table

将表6中的五种样品分别从外观、黏度、均匀度、油腻程度、酸碱度五个指标进行考察,综合评分见表7。The five samples in Table 6 were examined from the five indicators of appearance, viscosity, uniformity, greasiness, and pH. The comprehensive scores are shown in Table 7.

表7三乙醇胺添加量综合评分结果Table 7 Comprehensive scoring results of triethanolamine addition amount

由表7可知,三乙醇胺的添加量高于1.8%时,酸碱度可达到人体适合标准,但高于2.1%时,凝胶剂的黏度会增加且均匀度会变差,故三乙醇胺的添加量在1.8%~2.1%时,凝胶剂的状态较好。It can be seen from Table 7 that when the added amount of triethanolamine is higher than 1.8%, the pH can reach the standard suitable for the human body. However, when it is higher than 2.1%, the viscosity of the gel will increase and the uniformity will become worse. Therefore, the added amount of triethanolamine At 1.8% to 2.1%, the gel is in better condition.

(4)凝胶剂基质的正交设计(4) Orthogonal design of gel matrix

根据对凝胶剂的卡波姆940、丙二醇、三乙醇胺三个单因素的考察结果进行分析,设计凝胶剂基质的正交实验,以综合评价结果为分析指标,所得的正交实验结果即海蓬子驱蚊止痒凝胶剂的最优工艺配方。正交优化因素与水平见表8,L9(33)正交分析结果如表9所示。Based on the analysis of the results of the three single factors of the gel: carbomer 940, propylene glycol, and triethanolamine, an orthogonal experiment was designed for the gel matrix. The comprehensive evaluation results were used as the analysis index. The obtained orthogonal experiment results are: The optimal technological formula of Salicornia mosquito repellent and anti-itch gel. The orthogonal optimization factors and levels are shown in Table 8, and the L 9 (3 3 ) orthogonal analysis results are shown in Table 9.

表8正交优化因素与水平设计表Table 8 Orthogonal optimization factors and horizontal design table

表9正交实验分析结果Table 9 Orthogonal experiment analysis results

由表9可知,影响海蓬子凝胶剂基质的三个因素程度为A>B>C,即卡波姆940的添加量对海蓬子凝胶剂的影响最显著,其次为丙二醇的添加量,三乙醇胺对海蓬子凝胶剂的影响最小。海蓬子凝胶剂基质的最优方案为A2B1C2,即添加1.3%卡波姆940、9%丙二醇和2.0%三乙醇胺。It can be seen from Table 9 that the degree of the three factors that affect the matrix of Salicornia gelatin is A>B>C, that is, the addition of carbomer 940 has the most significant impact on the Salicornia gelatin, followed by the addition of propylene glycol. Amount, triethanolamine has the least impact on Salicornia gel. The optimal solution for the samphire gel matrix is A 2 B 1 C 2 , that is, adding 1.3% carbomer 940, 9% propylene glycol and 2.0% triethanolamine.

5、验证实验5. Verification experiment

根据正交优选结果,即添加1.3%卡波姆940、9%丙二醇和2.0%三乙醇胺于其他原料和辅料中制备成三批凝胶剂,并从其外观、黏度、均匀度、油腻程度进行感官评价,综合分数均在58~60分之间,比较稳定。测得三批凝胶剂的pH值见表10,均在6~8之间,符合人体可接受的酸碱度指标。According to the results of orthogonal optimization, three batches of gels were prepared by adding 1.3% carbomer 940, 9% propylene glycol and 2.0% triethanolamine to other raw materials and excipients, and the results were evaluated based on their appearance, viscosity, uniformity and greasiness. In sensory evaluation, the comprehensive scores are all between 58 and 60 points, which is relatively stable. The measured pH values of the three batches of gels are shown in Table 10. They are all between 6 and 8, which is in line with the acceptable pH index for the human body.

表10最优处方的酸碱度Table 10 pH of optimal prescription

从这三批凝胶剂中分别取5g置于离心管中,在3000r·min-1的条件下离心20min,观察到样品无明显分层和颜色变化的现象,说明样品的稳定性良好。Take 5g of each of these three batches of gelling agent and place it in a centrifuge tube, and centrifuge it for 20 minutes at 3000r·min -1 . It is observed that there is no obvious layering or color change in the sample, indicating that the stability of the sample is good.

从这三批凝胶剂中分别取5g置于离心管中,在60℃的条件下放置2h,观察到样品无明显分层和颜色变化的现象,说明样品的耐热性良好。Take 5g of each of these three batches of gels and place them in a centrifuge tube and place them at 60°C for 2 hours. No obvious layering or color change was observed in the samples, indicating that the samples have good heat resistance.

从这三批凝胶剂中分别取5g置于离心管中,在-18℃的条件下放置2h,观察到样品无明显分层和颜色变化的现象,说明样品的耐寒性良好。Take 5g of each of these three batches of gels and place them in a centrifuge tube and place them at -18°C for 2 hours. No obvious layering or color change was observed in the samples, indicating that the samples have good cold resistance.

通过上述的验证实验,表明制备海蓬子驱蚊止痒凝胶剂的工艺稳定且具有可行性。Through the above verification experiments, it is shown that the process for preparing the samphire mosquito repellent and anti-itch gel is stable and feasible.

6、方法学考察6. Methodological investigation

(1)芦丁标准品溶液的制备(1) Preparation of rutin standard solution

精确称量5mg的芦丁于50mL的容量瓶中,加入95%的乙醇定容至刻度线,震荡、摇匀,在水浴锅中加热至完全溶解,可得到浓度为0.1mg/mL的芦丁标准品溶液。Accurately weigh 5 mg of rutin into a 50 mL volumetric flask, add 95% ethanol to adjust the volume to the mark, shake and shake well, and heat in a water bath until completely dissolved to obtain rutin with a concentration of 0.1 mg/mL. Standard solution.

(2)供试品溶液的制备(2) Preparation of test solution

取5g的样品于50mL的容量瓶中,加入95%的乙醇定容至刻度线,充分震荡摇匀后取部分置于离心管中,在3000rpm的条件下离心10min后取上清液4mL于10mL的容量瓶中,分别加入0.3mL 5%的NaNO2溶液、0.3mL 10%的Al(NO3)3溶液和4mL 5%的NaOH溶液,震荡摇匀(每加一次溶液都需要静置6min),最后加入95%的乙醇定容至刻度线,震荡摇匀,静置15min后即可得到供试品溶液。Take 5g of the sample into a 50mL volumetric flask, add 95% ethanol to adjust the volume to the mark, shake well and put some part into a centrifuge tube, centrifuge at 3000rpm for 10min, then take 4mL of the supernatant into 10mL In the volumetric flask, add 0.3mL 5% NaNO 2 solution, 0.3mL 10% Al(NO 3 ) 3 solution and 4mL 5% NaOH solution respectively, shake and shake well (each solution needs to stand for 6 minutes) , finally add 95% ethanol to adjust the volume to the mark, shake well, and let it stand for 15 minutes to obtain the test solution.

(3)标准曲线的建立与绘制(3) Establishment and drawing of standard curve

分别取0mL、1.0mL、2.0mL、3.0mL、4.0mL、5.0mL的芦丁标准品溶液于10mL的容量瓶中。分别加入0.3mL 5%的NaNO2溶液、0.3mL 10%的Al(NO3)3溶液和4mL 5%的NaOH溶液,震荡摇匀(每加一次溶液都需要静置6min),最后加入95%的乙醇定容至刻度线,震荡摇匀,静置15min。将加入0mL的芦丁标准品溶液作为空白对照,在510nm用紫外分光光度计对标准品溶液测定吸光度。并以芦丁对照品的吸光度(c)为横坐标,吸光度(A)为纵坐标得到线性回归方程:y=0.012x+0.0076,R2=0.9991。具体结果数据见表11,芦丁标准曲线如图1所示。Take 0 mL, 1.0 mL, 2.0 mL, 3.0 mL, 4.0 mL, and 5.0 mL of rutin standard solution into a 10 mL volumetric flask respectively. Add 0.3mL 5% NaNO 2 solution, 0.3mL 10% Al(NO 3 ) 3 solution and 4mL 5% NaOH solution respectively, shake and shake well (each solution needs to stand for 6 minutes), and finally add 95% Dilute the volume of ethanol to the mark, shake well, and let stand for 15 minutes. Add 0 mL of rutin standard solution as a blank control, and measure the absorbance of the standard solution with a UV spectrophotometer at 510 nm. Taking the absorbance (c) of the rutin reference substance as the abscissa and the absorbance (A) as the ordinate, the linear regression equation is obtained: y=0.012x+0.0076, R 2 =0.9991. The specific result data are shown in Table 11, and the rutin standard curve is shown in Figure 1.

表11芦丁标准曲线吸光值测定Table 11 Determination of absorbance value of rutin standard curve

(4)海蓬子驱蚊止痒凝胶中总黄酮含量的测定(4) Determination of total flavonoid content in Salicornia mosquito repellent and antipruritic gel

取三份样品按供试液的方法制备,测得吸光度后代入芦丁标准曲线得到样品中芦丁浓度,并计算样品中的黄酮总量,结果见表12。Take three samples and prepare them according to the method of the test solution. The absorbance is measured and then added to the rutin standard curve to obtain the rutin concentration in the sample. The total amount of flavonoids in the sample is calculated. The results are shown in Table 12.

表12样品黄酮含量测定Table 12 Determination of flavonoid content of samples

实施例3海蓬子驱蚊止痒凝胶剂稳定性及透皮效果研究Example 3 Study on the Stability and Transdermal Effect of Samphire Mosquito Repellent and Antipruritic Gel

1、海蓬子驱蚊止痒凝胶剂稳定性研究1. Study on the stability of Salicornia mosquito repellent and antipruritic gel

(1)样品的存放稳定性测定(1) Determination of storage stability of samples

取一批样品(实施例1制得的海蓬子驱蚊止痒凝胶剂)制备成供试品溶液在室温、阴凉、避光条件下放置,以不加芦丁标准品溶液空白样品作为对照,在510nm的条件下测定存储0、30、60、120、180d样品吸光度(表13),结果表明样品的吸光度即黄酮含量相对稳定。Take a batch of samples (Samphire mosquito repellent and antipruritic gel prepared in Example 1) to prepare a test solution and place it under room temperature, cool and dark conditions, and use a blank sample without adding rutin standard solution as the test solution. For comparison, the absorbance of the samples stored for 0, 30, 60, 120, and 180 days was measured under the condition of 510 nm (Table 13). The results showed that the absorbance of the samples, that is, the flavonoid content, was relatively stable.

表13样品稳定性实验结果Table 13 Sample stability test results

(2)极端条件下凝胶剂稳定性测定(2) Determination of gel stability under extreme conditions

①耐热性试验:将三批制备好的海蓬子凝胶剂置于水浴锅中,于60℃条件下放置7d,分别于1、3、5、7d取样,考察各项内容,并取平均值记录在表格中,结果见表14。① Heat resistance test: Place the three batches of prepared samphire gel in a water bath and place it at 60°C for 7 days. Take samples at 1, 3, 5, and 7 days respectively to inspect various contents and take samples. The average values are recorded in the table and the results are shown in Table 14.

表14高温实验结果Table 14 High Temperature Experiment Results

②高湿试验:将三批海蓬子凝胶剂于25℃,相对湿度(90±5)%条件下放置7d,分别于1、3、5、7d取样,进行各项检测,并取平均值记录在表格中,结果见15。② High humidity test: Place three batches of Salicornia gel at 25°C and relative humidity (90±5)% for 7 days, take samples at 1, 3, 5, and 7 days respectively, conduct various tests, and take the average The values are recorded in the table and the results are shown in 15.

表15高湿实验结果Table 15 High Humidity Experiment Results

③光照试验:将三批海蓬子凝胶剂置于光照强度为(4500±500)LX的光照培养箱内7d,分别于1、3、5、7d取样,考察各项指标,并取平均值记录在表格中,结果见16。③Light test: Place three batches of Salicornia gel in a light incubator with a light intensity of (4500±500) LX for 7 days, take samples at 1, 3, 5, and 7 days respectively, examine various indicators, and average The values are recorded in the table and the results are shown in 16.

表16光照实验结果Table 16 Lighting experiment results

由表14-16可知,实施例1制得的海蓬子驱蚊止痒凝胶剂,经高温、高湿实验,凝胶剂的各项检测指标无明显变化,光照实验凝胶剂性状有所变化,表明海蓬子凝胶剂对光照敏感,应避免强光长时间直射。实验结果表明高温对海蓬子凝胶剂的稳定性影响较小,在第7d会使凝胶剂的粘度降低;湿度对稳定性影响也较小;光照会导致海蓬子凝胶剂氧化变质,在第5d海蓬子凝胶剂表面颜色变淡,在第7d部分变微黄。It can be seen from Tables 14-16 that the samphire mosquito repellent and antipruritic gel prepared in Example 1 has no significant change in the various detection indicators of the gel after high temperature and high humidity tests, and the properties of the gel in the light test are: The changes indicate that the samphire gel is sensitive to light and long-term direct exposure to strong light should be avoided. Experimental results show that high temperature has little effect on the stability of Salicornia gel, and will reduce the viscosity of the gel on the 7th day; humidity also has little effect on stability; light will cause oxidative deterioration of Salicornia gel , the color of the surface of the samphire gel became lighter on the 5th day, and turned slightly yellow on the 7th day.

2、海蓬子驱蚊止痒凝胶剂透皮研究2. Transdermal research on Samphire's mosquito repellent and antipruritic gel

(1)体外透皮实验(1) In vitro transdermal experiment

在Franz扩散池的接收室中加满30%乙醇生理盐水,将小鼠皮肤固定在扩散池的接收室与供给室之间,角质层朝上,皮肤要与液面恰好接触。接收室的扩散体积为25mL,扩散面积为0.785cm2,在37℃条件下水浴,磁力搅拌器以300r/min的速度搅拌。向供给室加入2g实施例1制得的海蓬子驱蚊止痒凝胶剂,分别于第2、4、6、8、10、12h从接收室中取样1mL,同时每次取完后再补充1mL的30%乙醇生理盐水接收液。将取出的样品用0.22μm微孔滤膜过滤,按照色谱检测条件为:ZORBAX SB-C18(4.6×150mm,5μm),流动相为甲醇-0.4%磷酸(45:55),流速为1.0mL/min,检测波长为370nm,柱温为30℃,分析时间为20min,进样量为10μL。结果如表17、图2-4所示。Fill the receiving chamber of the Franz diffusion cell with 30% ethanol saline, fix the mouse skin between the receiving chamber and the supply chamber of the diffusion cell, with the stratum corneum facing upward, and the skin should be in perfect contact with the liquid surface. The diffusion volume of the receiving chamber is 25 mL, the diffusion area is 0.785 cm 2 , the mixture is in a water bath at 37°C, and the magnetic stirrer is stirred at a speed of 300 r/min. Add 2g of Salicornia mosquito repellent and antipruritic gel prepared in Example 1 to the supply chamber, and sample 1 mL from the receiving chamber at 2, 4, 6, 8, 10, and 12 hours respectively. Add 1 mL of 30% ethanol saline receiving solution. Filter the removed sample with a 0.22μm microporous filter membrane. According to the chromatographic detection conditions: ZORBAX SB-C18 (4.6×150mm, 5μm), the mobile phase is methanol-0.4% phosphoric acid (45:55), and the flow rate is 1.0mL/ min, the detection wavelength is 370nm, the column temperature is 30°C, the analysis time is 20min, and the injection volume is 10μL. The results are shown in Table 17 and Figure 2-4.

(2)结果及讨论(2) Results and discussion

表17体外透皮结果Table 17 In vitro transdermal results

由表17可知,在12h内海蓬子凝胶剂中芦丁的累积量随时间的增加而增加,且在前4h内增加速度比较快,之后缓慢增加。It can be seen from Table 17 that the accumulated amount of rutin in Salicornia gel increases with time within 12 hours, and the increase rate is relatively fast in the first 4 hours, and then increases slowly.

由图2、图3可知,芦丁的保留时间为4.5min。It can be seen from Figure 2 and Figure 3 that the retention time of rutin is 4.5 minutes.

由图4可知,12h后小鼠皮肤中滞留的芦丁含量为34.114μg·cm-2,滞留在皮肤中的芦丁含量较多。It can be seen from Figure 4 that the rutin content retained in the mouse skin after 12 hours was 34.114 μg·cm -2 , and the rutin content retained in the skin was relatively high.

上述实验结果说明,海蓬子驱蚊止痒凝胶剂具有良好的透皮效果,能够在皮下组织维持一定的剂量药物浓度,能够实现止痒消肿的作用。The above experimental results show that the Salicornia mosquito repellent and anti-pruritic gel has good transdermal effect, can maintain a certain drug concentration in the subcutaneous tissue, and can achieve the effect of relieving itching and reducing swelling.

实施例4海蓬子驱蚊止痒凝胶剂驱蚊效果研究Example 4 Research on the Mosquito Repellent Effect of Samphire Mosquito Repellent and Antipruritic Gel

1、材料及方法1. Materials and methods

采用购买的白纹伊蚊为研究对象,饲养条件为:温度28±2℃,相对湿度(70±5)%,光照周期按照光照12h,黑暗环境12h,采用5%的蔗糖溶液作为饲料进行喂养。产品为实施例1制得的海蓬子驱蚊止痒凝胶剂。The purchased Aedes albopictus was used as the research object. The feeding conditions were: temperature 28±2℃, relative humidity (70±5)%, photoperiod of 12h light and 12h dark environment, and 5% sucrose solution as feed. . The product is the samphire mosquito repellent and antipruritic gel prepared in Example 1.

本实施例采用Y型嗅觉仪分析海蓬子驱蚊止痒凝胶剂对白纹伊蚊的引诱力。处理组取不同剂量(0.2、0.4、0.8、1.6g)凝胶剂涂抹在脱脂棉上,并将其放置在Y型嗅觉分析仪一个分支的顶端,同时在另外一个分支顶端用同样量的酒精作为空白对照,每天固定实验时间,早上9点到晚上9点。实验时,控制环境温度为26±1℃,相对湿度(70±5)%,洁净空气作为载气,流速为0.02m3/h。实验前将白纹伊蚊放入实验环境中适应30min,在Y型嗅觉仪的两个分支顶端分别接入两个管子用于通入空气,将30只白纹伊蚊从Y型嗅觉仪直管口放入管中,适应10min,之后开始计时,记录时间为20min,分别记录两个Y分支端中白纹伊蚊的数量,实验重复6次,每三次实验更换一次Y分支的凝胶剂和酒精位置,每次处理完要洗净烘干,以排除管壁位置对蚊子产生的影响。驱避率(%)=[(对照组-处理组)/(对照组+处理组)]×100%。实验结果如表18所示。In this embodiment, a Y-type olfactometer is used to analyze the attractiveness of Salicornia mosquito repellent and antipruritic gel to Aedes albopictus. The treatment group took different doses (0.2, 0.4, 0.8, 1.6g) of gel and smeared it on absorbent cotton, and placed it on the top of one branch of the Y-type olfactory analyzer. At the same time, the same amount of alcohol was used on the top of the other branch. For blank control, the experimental time is fixed every day, from 9 am to 9 pm. During the experiment, the ambient temperature was controlled to be 26±1°C, the relative humidity was (70±5)%, clean air was used as the carrier gas, and the flow rate was 0.02m 3 /h. Before the experiment, Aedes albopictus was put into the experimental environment for 30 minutes to adapt. Two tubes were connected to the tops of the two branches of the Y-type olfactory instrument to introduce air. 30 Aedes albopictus mosquitoes were put directly from the Y-type olfactory instrument. Put the mouth of the tube into the tube and let it adapt for 10 minutes. Then start timing and record the time for 20 minutes. Record the number of Aedes albopictus in the two Y branch ends. The experiment is repeated 6 times. The gel of the Y branch is replaced every three experiments. and alcohol positions, which must be washed and dried after each treatment to eliminate the impact of the position of the tube wall on mosquitoes. Repellency rate (%) = [(control group - treatment group)/(control group + treatment group)] × 100%. The experimental results are shown in Table 18.

2、结果及讨论2. Results and discussion

表18海蓬子驱蚊止痒凝胶剂对白纹伊蚊的驱避效果Table 18 Repellent effect of Samphire repellent and antipruritic gel against Aedes albopictus

如表18所示,实施例1制得的海蓬子驱蚊止痒凝胶剂对白纹伊蚊有较好的驱避效果,随着凝胶剂剂量的增加,驱避效果显著,呈现显著的剂量依赖性。从结果可知,当凝胶剂量为0.2g时,对白纹伊蚊的驱蚊效果已经达到65.71%,当剂量达到1.6g时,驱蚊效果达到92.45%,表明海蓬子驱蚊止痒凝胶剂具有显著的驱蚊效果。该凝胶剂主要成分来自植物提取物,具有对环境安全,对天敌安全,不易产生抗药性以及来源广泛等优点,为市场上驱蚊产品的研发制备提供了新的思路和途径,有着重要的理论和实际意义。As shown in Table 18, the samphire mosquito repellent and antipruritic gel prepared in Example 1 has a good repellent effect on Aedes albopictus. As the dose of the gel increases, the repellent effect is significant, showing a significant dose dependence. It can be seen from the results that when the gel dose is 0.2g, the mosquito repellent effect on Aedes albopictus has reached 65.71%, and when the dose reaches 1.6g, the mosquito repellent effect reaches 92.45%, indicating that the Samphire repellent and anti-itch gel The agent has significant mosquito repellent effect. The main ingredients of this gel come from plant extracts. It has the advantages of being safe for the environment, safe for natural enemies, not prone to drug resistance, and has a wide range of sources. It provides new ideas and ways for the development and preparation of mosquito repellent products on the market, and has important Theoretical and practical implications.

以上实施例仅是本发明的一部分实施例,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,都应当属于本发明的保护范围。The above 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 those skilled in the art without creative efforts should fall within the protection scope of the present invention.

Claims (7)

1. The Salicornia bigelovii mosquito-repellent itching-relieving gel is characterized by comprising, by weight, 20-25 parts of Salicornia bigelovii juice, 0.3-0.5 part of wormwood extract, 0.5-0.6 part of peppermint oil, 0.6-0.7 part of carbomer, 4-5 parts of propylene glycol, 4-5 parts of glycerol, 1-2 parts of pH regulator, 1-2 parts of penetration enhancer, 0.1 part of preservative and 18-20 parts of deionized water; wherein, the Salicornia bigelovii juice, the mugwort extract and the peppermint oil are gel raw materials; carbomers are gel matrices; propylene glycol and glycerin are humectants.
2. The Salicornia mosquito repellent antipruritic gel of claim 1, wherein the pH adjuster is triethanolamine, the penetration enhancer is azone, and the preservative is sodium benzoate.
3. The preparation method of the Salicornia bigelovii mosquito repellent itching relieving gel as claimed in claim 1 or 2, which is characterized by comprising the following steps:
step 1) pretreatment of raw materials: collecting fresh Salicornia bigelovii, cleaning, airing water for standby; collecting fresh aerial parts of mugwort, cleaning, air drying at room temperature, drying, and pulverizing; taking fresh peppermint, cleaning, drying and cutting into short sections for standby;
step 2) preparation of the salicornia juice: taking fresh Salicornia bigelovii that is drained, crushing, squeezing juice, filtering juice to remove residues, and adding vitamin C to obtain Salicornia bigelovii juice for standby;
step 3) preparation of the mugwort extract: by supercritical CO 2 The preparation by fluid extraction technology, the moxa treated in the step 1) is uniformly filled in an extraction reaction kettle, and CO is utilized 2 Repeatedly flushing to remove air in the pipeline; liquefying the CO 2 Pumping into a mixer by a high-frequency plunger pump, regulating parameters, and preparing the wormwood extract for later use; step 4) preparation of peppermint oil: the peppermint oil is prepared by adopting a steaming method, extracting the peppermint raw materials according to the ratio of 1:8, keeping the micro-boiling state for more than 4 hours, and drying the prepared peppermint oil by using anhydrous sodium sulfateFiltering for standby;
step 5) preparation of the Salicornia bigelovii gel: weighing carbomer, propylene glycol, glycerol, triethanolamine, azone, sodium benzoate and deionized water according to parts by weight; uniformly scattering carbomer on the surface of deionized water, standing and swelling for 24 hours; sequentially adding corresponding amounts of propylene glycol, glycerol, azone, sodium benzoate, the Salicornia Herbacea juice, the folium Artemisiae Argyi extract and the peppermint oil prepared in step 1) to step 3) into a gel matrix, adding the next reagent after uniformly stirring the reagents with a mixer each time, and finally slowly adding distilled water and uniformly stirring to prepare the Salicornia Herbacea gel;
step 6) regulating and controlling the pH value of the Salicornia gel: adjusting the pH value of the Salicornia bigelovii gel prepared in the step 5) by using triethanolamine, uniformly stirring, and adjusting the pH value to 6-8;
and 7) performing hydroperoxide gel sterilization on the Salicornia bigelovii gel processed in the step 6) to obtain emerald transparent gel, and filling to obtain the Salicornia bigelovii mosquito-repellent itching-relieving gel finished product.
4. The method for preparing the Salicornia bigelovii mosquito repellent antipruritic gel according to claim 3, wherein the addition amount of the vitamin C in the step 2) is 0.5g/kg of Salicornia bigelovii.
5. The method for preparing the Salicornia bigelovii mosquito repellent antipruritic gel according to claim 3, wherein the setting of the control parameters in step 3) is as follows: controlling CO 2 The flow rate is 25L/h, the separation pressure I of the reaction kettle is set to be 10+/-0.2 MPa, the temperature is 55 ℃, the separation pressure II is set to be 7+/-0.2 MPa, and the temperature is 55 ℃.
6. The method for preparing the Salicornia bigelovii mosquito repellent antipruritic gel according to claim 3, wherein the distilled water is added in the following amount in the step 5): the volume is fixed to 50 parts by weight.
7. The preparation method of the Salicornia bigelovii mosquito-repellent itching-relieving gel according to claim 3, wherein the weight of the Salicornia bigelovii mosquito-repellent itching-relieving gel finished product in the step 7) is 50g.
CN202311224299.4A 2023-09-21 2023-09-21 A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof Pending CN117338654A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202311224299.4A CN117338654A (en) 2023-09-21 2023-09-21 A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202311224299.4A CN117338654A (en) 2023-09-21 2023-09-21 A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof

Publications (1)

Publication Number Publication Date
CN117338654A true CN117338654A (en) 2024-01-05

Family

ID=89370189

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202311224299.4A Pending CN117338654A (en) 2023-09-21 2023-09-21 A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof

Country Status (1)

Country Link
CN (1) CN117338654A (en)

Similar Documents

Publication Publication Date Title
CN113318023B (en) Bougainvillea spectabilis extract and antioxidant blush based on the same
CN105078803A (en) Application of callicarpa plant extract
CN114948824A (en) Whitening and freckle removal composition
CN108703931A (en) A kind of composition and preparation method thereof with moisture-keeping function
CN107789316A (en) A kind of moisturizing antioxidant composition of extract of stem cell containing pot marigold and its application
CN109939193A (en) A kind of composition for treating skin eczema, preparation and preparation method and application
CN102258094B (en) Tea drink containing natural plants or natural plant extracts, and preparation method and application thereof
CN108815060B (en) A kind of fat-reducing ointment and preparation method thereof containing roselle
CN108078868A (en) A kind of antiallergic composition for skin care item
CN116492385B (en) Compound essential oil for repairing skin and pharmaceutical composition containing compound essential oil
CN117338654A (en) A kind of samphire mosquito repellent and antipruritic gel and preparation method thereof
CN107912773A (en) A kind of preparation for being used to alleviate physical fatigue
CN115607608B (en) Compound Chinese prickly ash ointment and preparation method thereof
CN107049866B (en) Antiallergic plant composition and application thereof
CN115869358A (en) A traditional Chinese medicine composition for treating non-alcoholic fatty liver disease and its application
CN114306164A (en) Antibacterial acne-removing cream and preparation method thereof
CN113956921A (en) Artemisia annua essential oil and white tea essential oil with skin sensitivity improving effect, and their composition
CN111728918A (en) A kind of preparation method of wild chrysanthemum facial mask
CN105412191A (en) Arnica long-acting sustained release preparation for treating contusions and preparation method thereof
CN119770406B (en) External repairing anti-wrinkle composition and preparation method thereof
CN115245480B (en) Skin care composition containing plant essence and toner
CN119033894B (en) Preparation process of skin hemorrhoid clearing ointment pharmaceutical composition
CN107865927A (en) A kind of clarification process and method of quality control of the pharmaceutical composition that there are treatment livid ring around eye to act on
CN109394616A (en) A kind of essential oil composition and its application with balance estrogen action
CN112237600B (en) Application of compound rattan pepper gel in the preparation of products for preventing and/or treating frostbite

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination