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CN105602730A - Phoebe zhennan essential oil and preparation method thereof - Google Patents

Phoebe zhennan essential oil and preparation method thereof Download PDF

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CN105602730A
CN105602730A CN201610017934.5A CN201610017934A CN105602730A CN 105602730 A CN105602730 A CN 105602730A CN 201610017934 A CN201610017934 A CN 201610017934A CN 105602730 A CN105602730 A CN 105602730A
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essential oil
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phoebe
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CN105602730B (en
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宁莉萍
丁文
张莉
李福洲
李贤伟
刘应高
李梅
龙夏颖
安荣苗
王天石
时浩
熊燕
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Du Lizhao
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Sichuan Agricultural University
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/54Lauraceae (Laurel family), e.g. cinnamon or sassafras
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/022Refining
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/02Recovery or refining of essential oils from raw materials
    • C11B9/027Recovery of volatiles by distillation or stripping
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/35Extraction with lipophilic solvents, e.g. Hexane or petrol ether
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

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  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
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  • Fats And Perfumes (AREA)

Abstract

本发明公开了一种楠木精油及其制备方法,包括以下步骤:第一步,将楠木预处理,得到楠木预处理料;第二步,将楠木预处理料加入到提取装置;第三步,从提取装置中分离出含有溶剂的精油;第四步,将精油与溶剂分离;第五步,精油脱水;所述第一步中,原料为楠木属、润楠属及其近缘属树种的木材,预处理为将楠木的树皮、树干、树根、树梢、树枝、花、果实等原料自然风干或烘干后粉碎,粉碎后过筛,过筛目数为2~100目。本发明的优点在于:楠木精油具有抗菌消炎,耐腐防虫,可治疗老年慢性支气管炎,局部麻醉,治疗结肠炎,镇咳祛痰,治疗胃病、结膜炎,镇痛,祛风除湿等特殊效果;该制备方法提取率高,绿色安全,操作简单。The invention discloses a nanmu essential oil and a preparation method thereof, comprising the following steps: firstly, pretreating nanmu to obtain a nanmu pretreated material; secondly, adding the nanmu pretreated material to an extraction device; thirdly, The essential oil containing solvent is separated from the extraction device; the fourth step is to separate the essential oil from the solvent; the fifth step is to dehydrate the essential oil; For wood, the pretreatment is to dry naturally or dry the bark, trunk, root, treetop, branch, flower, fruit and other raw materials of Phoebe, and then sieve after crushing. The advantages of the present invention are: Phoebe essential oil has antibacterial and anti-inflammatory properties, anti-corrosion and anti-insect, can treat senile chronic bronchitis, local anesthesia, treat colitis, antitussive and expectorant, treat stomach disease, conjunctivitis, analgesia, expelling wind and dehumidification and other special effects ; The preparation method has a high extraction rate, is green and safe, and is simple to operate.

Description

楠木精油及其制备方法Phoebe essential oil and preparation method thereof

技术领域 technical field

本发明涉及日用化工领域,具体的说是楠木精油及其制备方法。 The invention relates to the field of daily chemical industry, in particular to nanmu essential oil and a preparation method thereof.

背景技术 Background technique

广义的楠木包括楠木属(旧称桢楠属,PhoebeNees)和润楠属(MachilusNees)及其近缘属。楠木木材结构细致、木性稳定、纹理美丽、易加工,是我国古代重要的建筑、家具用料,明清时期为皇家专享。楠木文化底蕴深厚,从宫殿到陵寝,从座椅到床榻,作为中华文化的载体,折射了中国封建社会皇家文化和文人士大夫的审美观,体现了木文化在建筑、家具、艺术品方面的精髓。(楠木香味清雅而悠长,)久居楠木装修的居室雅斋中,与楠木家具为伴,闻着其幽香能起到延年益寿、养生保健的作用。 Phoebe in a broad sense includes Phoebe (formerly known as Zhennan, PhoebeNees) and Runnan (MachilusNees) and their related genera. Phoebe wood has fine structure, stable wood, beautiful texture and easy processing. It is an important building and furniture material in ancient my country. It was exclusively used by the royal family during the Ming and Qing Dynasties. Phoebe has a profound cultural background. From palaces to mausoleums, from seats to beds, as a carrier of Chinese culture, it reflects the royal culture of Chinese feudal society and the aesthetics of literati and officials, and embodies the essence of wood culture in architecture, furniture and artwork. . (The fragrance of nanmu is elegant and long,) Living in the elegant room decorated with nanmu for a long time, accompanied by nanmu furniture, smelling its delicate fragrance can prolong life and maintain health.

近几年楠木被市场快速热推,2013年后升值速度已超过海南黄花梨,目前市价已高过红酸枝等传统高档木材。所谓“盛世玩收藏”,由于楠木耐腐防虫、材性独特、气味幽香、冬天触之不凉夏天触之不热的特点,受到众多消费者的青睐,市场呈现购销两旺的状况。楠木作为贵重木材,除用作家具以外,还是历代重要建筑场所以及木雕用材,明清两代一些重要的宫殿建筑都是使用楠木做栋梁的,但是在现代加工制作过程中大量的加工边角余料及木屑却未被有效利用,而是被焚烧或废弃处理。由于大部分楠木树种是国家二级保护植物不得随意采伐,且楠木的生长速度非常缓慢,因此成材后的楠木价格昂贵。鉴于此,如何寻找到一种能充分发挥楠木木性优点且生产工艺简单操作方便的楠木精油制备方法是目前迫在眉睫的行业热点问题。 In recent years, nanmu has been rapidly promoted by the market. After 2013, the appreciation rate has surpassed that of Hainan huanghuali. At present, the market price is higher than that of traditional high-grade wood such as red rosewood. The so-called "Great Age Play Collection" is favored by many consumers due to its characteristics of anti-corrosion and insect resistance, unique material properties, delicate smell, and cool in winter and cool in summer. The market is booming in both sales and purchases. As a precious wood, Nanmu is not only used as furniture, but also important building sites and woodcarving materials in the past dynasties. Some important palace buildings in Ming and Qing Dynasties used Nanmu as beams, but in the modern processing and production process, a large number of processing corners are left behind. The raw materials and sawdust are not effectively utilized, but are incinerated or discarded. Since most of the nanmu species are national second-class protected plants and cannot be harvested at will, and the growth rate of nanmu is very slow, the price of nanmu after becoming useful is expensive. In view of this, how to find a method for preparing nanmu essential oil that can give full play to the advantages of nanmu wood and has a simple and convenient production process is an urgent industry hot issue.

我国古代将楠木作为一味祛疾除患的良药,古医书记载“足部水肿。削楠木、桐木煮水泡脚,并饮此水少许。每日如此,直至病愈。心胀腹痛,不得吐泻。取楠木削三、四两,加水三升,煮开三次,饮服。耳出脓。用楠木烧存性,研末敷耳内”(《本草纲目》,李时珍);“楠木枝叶味苦温,无毒,主霍乱,煎汁服之,木高大叶如桑,出南方山中。郭注尔雅云,楠,大木,叶如桑也”(《证类本草》,唐慎微);“楠皮汤,治胃冷吐逆正气,右以楠木皮煎汤汁服之”(《小儿卫生总微论方》);“治耳出脓水久不绝方:楠木一分烧灰,花燕脂一分,右二件药细研为散,每取少许,内于耳中”(《太平圣惠方》,北宋官方修书); In ancient China, nanmu was used as a good medicine for blindly dispelling diseases. Ancient medical books recorded "foot edema. Cut nanmu and paulownia wood and boil water to soak feet, and drink a little of this water. Do this every day until the disease is cured. Heart distension and abdominal pain, no vomiting and diarrhea. Take three or four liang of nanmu, add three liters of water, boil for three times, and take it with drink. The pus comes out of the ear. Burn the nanmu for preservation, grind it into powder and apply it to the ear" ("Compendium of Materia Medica", Li Shizhen); "The branches and leaves of nanmu are bitter and warm, Non-toxic, the main cholera, decoct it, the tree is tall and the leaves are like mulberry, and it comes out of the southern mountains. Guo Zhuer Yayun, Nan, big tree, leaves like mulberry" ("Zheng Lei Materia Medica", Tang Shenwei); "Nanpi Decoction , to treat cold stomach and vomiting against righteousness, take it with nanmu bark decoction soup" ("Children's Health General Micro-On Prescription"); Divide, the two medicines on the right are finely ground into powder, take a little of each, and put it in the ear" ("Taiping Shenghui Prescription", official revision book of the Northern Song Dynasty);

“主霍乱。……以楠木枝叶。煎汁服之”;“治霍乱转筋,用楠木皮。煎汤洗之”;“又方,治脚气肿满大效。……又方,樟木三斤,楠木二斤右件药细锉和匀。每度用半斤。以水三斗。煎至二斗。去滓看冷暖。于避风处淋蘸”(《普济方》,朱橚等);综上,楠木入药,内服外用,可治疗胃病、霍乱、霍乱转筋、聤耳出脓水(中耳炎)、脚气等病症。虽然古籍记载了大量楠木应用于医药的经典实例,但是楠木的内含化学物成分及养生药用原理尚未被现代医学证实。 "To control cholera... Take the branches and leaves of nanmu. Decoct it and take it"; Three catties, two catties of nanmu, the right piece of medicine, finely file and evenly. Use half a catty per degree. Use three buckets of water. Fry until two buckets. Remove the water to see whether it is warm or cold. Drench and dip in a sheltered place" ("Puji Fang", Zhu Wei etc.); in summary, Phoebe is used as medicine, taken internally and externally, and can treat diseases such as stomach problems, cholera, cholera tendons, pus from ears (otitis media), beriberi. Although ancient books have recorded a large number of classic examples of Phoebe being used in medicine, the chemical composition and health-preserving medicinal principles of Phoebe have not been confirmed by modern medicine.

目前虽然也有一些关于木材精油及工艺的专利,如水蒸气蒸馏联合超临界CO2萃取制备桧木精油的方法(申请号:CN201210339865.1),桧木精油及其含有桧木精油的香烟(申请号:CN201010044402.3),一种花梨木木屑萃取花梨木精油的生产工艺及其设备(申请号:CN201510187394.0),一种天然辣木保健精油(申请号:CN201510256307.2),但是关于楠木精油及其制备方法的研究论文和专利报道基本处于空白。楠木作为珍贵资源,其加工废弃物未得到有效利用,上述虽提到精油提取的方法,但工艺复杂,效率一般,安全性有待提高,而且不同树种木材结构,成分有所差异,因此上述方法不适用楠木精油的提取。本发明旨在探索高效提取楠木精油的技术,该技术不仅可以充分利用楠木木材的加工边角料和木屑等废弃物,而且可充分发掘树枝、树叶、树皮等物质资源的药用和养生价值,提高楠木种植过程的经济价值,同时也可通过本发明充分利用楠木的养生药用价值。 Although there are also some patents about wood essential oil and technology at present, such as steam distillation combined with supercritical CO2 extraction method for preparing cypress essential oil (application number: CN201210339865.1), cypress essential oil and cigarettes containing cypress essential oil (application number: CN201010044402.3 ), a production process and equipment for extracting rosewood essential oil from rosewood sawdust (application number: CN201510187394.0), a natural health-care essential oil of moringa (application number: CN201510256307.2), but about Phoebe essential oil and its preparation method Research papers and patent reports are basically blank. Phoebe is a precious resource, and its processing waste has not been effectively utilized. Although the above-mentioned method of extracting essential oils is mentioned, the process is complicated, the efficiency is average, and the safety needs to be improved. Moreover, the wood structure and composition of different tree species are different. Therefore, the above-mentioned method does not It is suitable for the extraction of nanmu essential oil. The present invention aims to explore a technology for efficiently extracting nanmu essential oil. This technology can not only make full use of wastes such as processing scraps and sawdust of nanmu wood, but also fully explore the medicinal and health value of material resources such as branches, leaves, bark, etc., and improve The economic value of Phoebe plantation process can also make full use of the health-preserving medicinal value of Phoebe by the present invention simultaneously.

发明内容 Contents of the invention

本发明的目的就在于针对上述问题,提供一种精油提取率高,绿色安全,操作简单的楠木精油提取工艺。 The object of the present invention is to address the above problems and provide a process for extracting nanmu essential oil with high extraction rate, green and safe, and simple operation.

本发明提供了一种楠木精油制备的方法,其主要包括以下步骤: The invention provides a method for preparing nanmu essential oil, which mainly includes the following steps:

第一步,将楠木预处理,得到楠木预处理料; The first step is to pretreat nanmu to obtain nanmu pretreatment material;

第二步,将楠木预处理料和溶剂加入到超声波处理装置; In the second step, the nanmu pretreatment material and solvent are added to the ultrasonic treatment device;

第三步,将超声波处理后的原料转移到提取装置,并从中分离出含有溶剂的精油; In the third step, the raw material after ultrasonic treatment is transferred to the extraction device, and the essential oil containing solvent is separated from it;

第四步,将精油与溶剂分离; The fourth step is to separate the essential oil from the solvent;

第五步,精油脱水; The fifth step, essential oil dehydration;

更进一步的,所述第一步中,原料为楠木属、润楠属及其近缘属树种的木材,预处理为将楠木的树皮、树干、树根、树梢、树枝、花、果实等原料自然风干或烘干后粉碎,粉碎后过筛,过筛目数为4~100目。 Further, in the first step, the raw material is the wood of Phoebe genus, Phoebe genus and its close relative species, and the pretreatment is to prepare the bark, trunk, root, treetop, branch, flower and fruit of Phoebe The raw materials are naturally air-dried or crushed after drying, and then sieved after crushing. The mesh size of the sieve is 4 to 100 mesh.

更进一步的,所述第三步中提取装置为有机溶剂提取装置,或水蒸气提取装置; Furthermore, the extraction device in the third step is an organic solvent extraction device, or a water vapor extraction device;

更进一步的,所述第三步中,分离出含有溶剂的精油采用的方法为减压过滤法、板框过滤法、压滤法,或冷凝回流法; Further, in the third step, the method used to separate the essential oil containing solvent is vacuum filtration, plate and frame filtration, pressure filtration, or condensation reflux;

更进一步的,所述第四步中,精油与溶剂分离的方法为减压蒸馏法,或重力分离法、离心分离法; Further, in the fourth step, the method for separating the essential oil from the solvent is vacuum distillation, gravity separation, or centrifugation;

更进一步的,所述第五步中,精油脱水采用无水硫酸钠脱水,或常压低温干燥法脱水。 Furthermore, in the fifth step, the essential oil is dehydrated by using anhydrous sodium sulfate dehydration, or dehydration by normal pressure and low temperature drying method.

本发明还提供了一种楠木精油制备的方法,其主要包括以下步骤: The present invention also provides a method for preparing nanmu essential oil, which mainly includes the following steps:

第一步,将楠木的树皮、树干、树根、树梢、树枝、花、果实等原料自然风干或烘干后粉碎,粉碎后过筛,得到楠木预处理料。 In the first step, raw materials such as bark, trunk, root, treetop, branch, flower and fruit of Nanmu are naturally air-dried or dried, then crushed, and then sieved after crushing to obtain a pretreated material of Nanmu.

第二步,将楠木预处理料加入到超声波处理装置内,进行超声波处理; In the second step, the nanmu pretreatment material is added into the ultrasonic treatment device for ultrasonic treatment;

第三步,将有机溶剂和楠木料渣采用减压过滤的方法过滤后转移; In the third step, the organic solvent and the nanmu slag are filtered by vacuum filtration and then transferred;

第四步,将过滤后的滤液进行减压蒸馏,得到粗提物; In the fourth step, the filtered filtrate is subjected to vacuum distillation to obtain a crude extract;

第五步,将粗提物过无水硫酸钠除水,或低温干燥除水; The fifth step is to remove water from the crude extract by passing it over anhydrous sodium sulfate, or dry it at low temperature to remove water;

更进一步的,所述第二步中,溶剂为乙醇、乙酸乙酯、丙酮、乙醚中的一种或一种以上;溶剂添加量为10-40ml/g楠木预处理料;浸提时间为3-48h;超声处理时间为10-120min,温度为10-60℃,超声波频率为20-80Hz; Further, in the second step, the solvent is one or more of ethanol, ethyl acetate, acetone, ether; the amount of solvent added is 10-40ml/g nanmu pretreatment material; the extraction time is 3 -48h; Ultrasonic treatment time is 10-120min, temperature is 10-60℃, ultrasonic frequency is 20-80Hz;

更进一步的,所述第三步中,减压过滤的滤孔孔径为0.2-0.8μm; Further, in the third step, the pore diameter of the filter under reduced pressure filtration is 0.2-0.8 μm;

更进一步的,所述第四步中,减压浓缩的压力为0.03-0.1MPa,温度为30-70℃; Furthermore, in the fourth step, the pressure of vacuum concentration is 0.03-0.1MPa, and the temperature is 30-70°C;

更进一步的,所述第五步中,所述无水硫酸钠的用量为0.2-1g/ml粗提物;或采用低温常压方法干燥脱水,得到精油粗提物;干燥的温度为0~5℃,时间为5~100h;。 Furthermore, in the fifth step, the dosage of the anhydrous sodium sulfate is 0.2-1g/ml crude extract; or adopt low temperature and normal pressure method to dry and dehydrate to obtain the crude extract of essential oil; the drying temperature is 0~ 5 ℃, the time is 5 ~ 100h;.

本发明还提供了一种精油制备的方法,其主要包括以下步骤: The present invention also provides a method for preparing essential oil, which mainly includes the following steps:

第一步,将楠木的树皮、树干、树根、树梢、树枝、花、果实等原料自然风干或烘干后粉碎,粉碎后过筛,得到楠木预处理料。 In the first step, raw materials such as bark, trunk, root, treetop, branch, flower and fruit of Nanmu are naturally air-dried or dried, then crushed, and then sieved after crushing to obtain a pretreated material of Nanmu.

第二步,将楠木预处理料加入0-20%的NaCl水溶液,进行超声波处理 In the second step, add nanmu pretreatment material to 0-20% NaCl aqueous solution for ultrasonic treatment

第三步,采用水蒸气提取装置进行提取; The third step is to use a steam extraction device to extract;

第三步,将夹带有提取物的水蒸气采用冷凝回流的方法收集; In the third step, the water vapor entrained with the extract is collected by condensation and reflux;

第四步,采用重力分离法或离心分离法进行分离; The fourth step is to separate by gravity separation or centrifugation;

第五步,将粗提物过无水硫酸钠除水,或常压低温干燥法脱水; The fifth step is to dehydrate the crude extract by perusing anhydrous sodium sulfate, or dehydrating by normal pressure and low temperature drying method;

更进一步的,所述第二步中,将楠木预处理料加入到超声波处理装置内,进行超声波处理;溶剂为0~20%的NaCl水溶液;溶剂添加量为3~10ml/g楠木预处理料;超声处理时间为5~60min,温度为10~60℃,超声波频率为20~80Hz; Further, in the second step, the nanmu pretreatment material is added into the ultrasonic treatment device for ultrasonic treatment; the solvent is 0-20% NaCl aqueous solution; the solvent addition amount is 3-10ml/g nanmu pretreatment material ; Ultrasonic treatment time is 5-60min, temperature is 10-60℃, ultrasonic frequency is 20-80Hz;

更进一步的,所述第三步中,采用水蒸气装置提取,提取时间为5-10h; Furthermore, in the third step, the water vapor device is used for extraction, and the extraction time is 5-10 hours;

更进一步的,所述第四步中,采用重力分离法或离心分离法进行分离,重力分离法静置10-60min,离心分离法转速为1000-4000RPM,时间为1-10min; Furthermore, in the fourth step, gravity separation or centrifugal separation is used for separation, the gravity separation method is left standing for 10-60 minutes, and the speed of centrifugal separation method is 1000-4000 RPM, and the time is 1-10 minutes;

更进一步的,所述第五步中,所述无水硫酸钠的用量为0.2-1g/ml粗提物;或采用低温常压方法干燥脱水,干燥的温度为0~5℃,时间为5~100h。 Further, in the fifth step, the dosage of the anhydrous sodium sulfate is 0.2-1g/ml crude extract; or adopt the method of low temperature and normal pressure to dry and dehydrate, the drying temperature is 0-5°C, and the drying time is 5 ~100h.

本发明还提供了一种楠木精油,其由上述三种方法中的任意一种制备得到的。 The present invention also provides a kind of Phoebe essential oil, which is prepared by any one of the above three methods.

本发明的有益效果在于:根据楠木精油主要成分β-桉叶醇、愈创蓝油烃、d-杜松烯、γ-杜松烯、愈创木醇、沉香螺旋醇、氧化石竹烯、α-古巴烯得知,楠木精油具有抗菌消炎,耐腐防虫,可治疗老年慢性支气管炎,局部麻醉,治疗结肠炎,镇咳祛痰,治疗胃病、结膜炎,镇痛,祛风除湿等特殊效果。 The beneficial effects of the present invention are: according to the main components of Phoebe essential oil β-cineole, guaiazene, d-junipene, γ-junipene, guaiacyl alcohol, agarwood helicol, caryophyllene oxide, α -Cubacene learned that Phoebe essential oil has antibacterial, anti-inflammatory, anti-corrosion and anti-insect properties. It can treat chronic bronchitis in the elderly, local anesthesia, colitis, cough and expectorant, stomach disease, conjunctivitis, analgesia, wind and dampness and other special effects .

具体实施方式 detailed description

下面结合实施例对本发明作进一步说明: The present invention will be further described below in conjunction with embodiment:

实施例1 Example 1

(1)预处理:将桢楠木质部风干,粉碎过筛后粒度为小于10目,浸泡在95%乙醇中36h; (1) Pretreatment: Air-dry the xylem of Phoebe zhennan, crush and sieve to a particle size of less than 10 mesh, soak in 95% ethanol for 36 hours;

(2)超声波处理:取适量步骤(1)处理后的粉料,将其浸入溶剂中,30℃下超声波处理120min; (2) Ultrasonic treatment: take an appropriate amount of powder treated in step (1), immerse it in a solvent, and ultrasonically treat it at 30°C for 120 minutes;

(3)过滤:将步骤2中处理后的溶液进行减压过滤,过滤后的溶液呈透明澄清,无明显杂质; (3) Filtration: the solution treated in step 2 is filtered under reduced pressure, and the filtered solution is transparent and clear without obvious impurities;

(4)减压蒸馏:将步骤3所得液体加入旋转蒸发仪进行减压蒸馏,压力为0.06MPa,温度为40℃,得粗提物; (4) Distillation under reduced pressure: Add the liquid obtained in step 3 into a rotary evaporator to carry out distillation under reduced pressure at a pressure of 0.06 MPa and a temperature of 40° C. to obtain a crude extract;

(5)脱水:将粗产品进行低温、常压干燥脱水,温度为3℃,时间为10h,除水后即为桢楠木质部精油。 (5) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure at a temperature of 3° C. for 10 hours. After dehydration, the xylem essential oil of Phoebe zhennan is obtained.

将所得桢楠木质部精油进行GC-MS分析,其精油中主要为萜类化合物,β-桉叶醇可帮助开发治疗血管疾病的药物,具有健脾燥湿、抗缺氧作用,并能明显促进胃肠运动;愈创蓝油烃具有抗菌消炎、治疗结膜炎作用;d-杜松烯具有镇痛抗菌、抗肿瘤的作用;γ-杜松烯具有祛痰作用;愈创木醇可镇咳平喘;沉香螺旋醇具有安定作用;大根香叶烯广泛用于药物合成的重要中间体;氧化石竹烯可治疗皮肤霉菌病,同时还具有舒肝、镇痛、抗菌消炎、祛风除湿、清热解毒、利尿消肿的功效;β-石竹烯具有一定平喘作用,可治疗老年慢性支气管炎,有局部麻醉、治疗结肠炎、镇咳祛痰等功效,还可驱除蚊虫、抗焦虑和抑郁、镇痛,并具很好的抗溃疡和抗炎作用;α-古巴烯可作为抗菌剂、利尿剂、镇静剂;桉叶醇有镇静作用,γ-桉叶醇、β-桉叶醇和α-桉叶醇均为蜂胶的主要成分,因此该桢楠精油具有良好的安定及镇咳平喘功效,也可开发神经类药物及止咳平喘药物。 The obtained xylem essential oil of Phoebe zhennan was analyzed by GC-MS. The essential oil is mainly terpenoids, and β-cineole can help to develop drugs for treating vascular diseases. Gastrointestinal motility; guaiazene has antibacterial, anti-inflammatory, and conjunctivitis-treating effects; d-juninene has analgesic, antibacterial, and anti-tumor effects; γ-juninene has expectorant effects; Asthma; agarwood helicol has a stabilizing effect; myrcene is widely used as an important intermediate in drug synthesis; caryophyllene oxide can treat skin mycosis, and it also has the functions of soothing the liver, analgesia, antibacterial and anti-inflammatory, expelling wind and dampness, and clearing away heat The effect of detoxification, diuresis and swelling; β-caryophyllene has a certain antiasthmatic effect, can treat chronic bronchitis in the elderly, has local anesthesia, colitis, antitussive and expectorant effects, and can also repel mosquitoes, anti-anxiety and depression, Analgesic, and has very good anti-ulcer and anti-inflammatory effects; α-Cubacene can be used as an antibacterial agent, diuretic, and sedative; Leaf alcohol is the main component of propolis, so the zhennan essential oil has good stability and antitussive and antiasthmatic effects, and can also be used to develop neurological drugs and antitussive and antiasthmatic drugs.

实施例2 Example 2

(1)预处理:将桢楠树皮风干,粉碎过筛后粒度为小于20目,浸泡在95%乙醇中36h; (1) Pretreatment: Air-dry the bark of Phoebe zhennan, crush and sieve to a particle size of less than 20 mesh, soak in 95% ethanol for 36 hours;

(2)超声波处理:取适量步骤(1)处理后的粉料,将其浸入溶剂中,30℃下超声波处理120min; (2) Ultrasonic treatment: take an appropriate amount of powder treated in step (1), immerse it in a solvent, and ultrasonically treat it at 30°C for 120 minutes;

(3)过滤:将步骤2中处理后的溶液进行减压过滤,过滤后的溶液呈透明澄清,无明显杂质; (3) Filtration: the solution treated in step 2 is filtered under reduced pressure, and the filtered solution is transparent and clear without obvious impurities;

(4)减压蒸馏:将步骤3所得液体加入旋转蒸发仪进行减压蒸馏,压力为0.09MPa,温度为50℃,得粗提物; (4) Distillation under reduced pressure: Add the liquid obtained in step 3 into a rotary evaporator for distillation under reduced pressure at a pressure of 0.09 MPa and a temperature of 50° C. to obtain a crude extract;

(5)脱水:将粗产品进行低温、常压干燥脱水,温度为3℃,时间为15h,除水后即为桢楠树皮精油; (5) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure at a temperature of 3°C for 15 hours. After dehydration, it becomes Zhennan bark essential oil;

将所得桢楠树皮精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained zhennan bark essential oil was analyzed by GC-MS, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例3 Example 3

(1)预处理:将桢楠树叶风干,粉碎过筛后粒度为小于10目,浸泡在95%乙醇中36h; (1) Pretreatment: Air-dry the leaves of Phoebe zhennan, crush and sieve to a particle size of less than 10 mesh, soak in 95% ethanol for 36 hours;

(2)超声波处理:取适量步骤(1)处理后的粉料,将其浸入溶剂中,30℃下超声波处理120min; (2) Ultrasonic treatment: take an appropriate amount of powder treated in step (1), immerse it in a solvent, and ultrasonically treat it at 30°C for 120 minutes;

(3)过滤:将步骤2中处理后的溶液进行减压过滤,过滤后的溶液呈透明澄清,无明显杂质; (3) Filtration: the solution treated in step 2 is filtered under reduced pressure, and the filtered solution is transparent and clear without obvious impurities;

(4)减压蒸馏:将步骤3所得液体加入旋转蒸发仪进行减压蒸馏,压力为0.07MPa,温度为40℃,得粗提物; (4) Distillation under reduced pressure: put the liquid obtained in step 3 into a rotary evaporator to carry out distillation under reduced pressure at a pressure of 0.07 MPa and a temperature of 40° C. to obtain a crude extract;

(5)脱水:将粗产品进行低温、常压干燥脱水,温度为5℃,时间为10h,除水后即为桢楠树叶精油; (5) Dehydration: Dry and dehydrate the crude product at low temperature and normal pressure at a temperature of 5°C for 10 hours. After dehydration, it becomes the essential oil of Phoebe zhennan leaves;

将所得桢楠树叶精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained zhennan leaf essential oil was analyzed by GC-MS, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例4 Example 4

(1)预处理:将桢楠树根风干,粉碎过筛后粒度为小于80目,浸泡在95%乙醇中48h; (1) Pretreatment: air-dry the root of Phoebe zhennan, crush and sieve it to a particle size of less than 80 mesh, soak it in 95% ethanol for 48 hours;

(2)超声波处理:取适量步骤(1)处理后的粉料,将其浸入溶剂中,40℃下超声波处理120min; (2) Ultrasonic treatment: take an appropriate amount of powder treated in step (1), immerse it in a solvent, and ultrasonically treat it at 40°C for 120 minutes;

(3)过滤:将步骤2中处理后的溶液进行减压过滤,过滤后的溶液呈透明澄清,无明显杂质; (3) Filtration: the solution treated in step 2 is filtered under reduced pressure, and the filtered solution is transparent and clear without obvious impurities;

(4)减压蒸馏:将步骤3所得液体加入旋转蒸发仪进行减压蒸馏,压力为0.08MPa,温度为40℃,得粗提物; (4) Distillation under reduced pressure: Add the liquid obtained in step 3 into a rotary evaporator to carry out distillation under reduced pressure at a pressure of 0.08 MPa and a temperature of 40° C. to obtain a crude extract;

(5)脱水:将粗产品过无水硫酸钠除水,温度为2℃,时间为40h,除水后即为桢楠树根精油; (5) Dehydration: remove the water from the crude product sodium persulfate anhydrous, the temperature is 2°C, the time is 40h, after the water is removed, it is the essential oil of Zhennan tree root;

将所得桢楠树根精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained essential oil of Phoebe zhennan root was analyzed by GC-MS, and its main components and pharmacology were the same as above, but the proportions of main components were different.

实施例5 Example 5

(1)预处理:将桢楠树枝风干,粉碎过筛后粒度为80目,浸泡在95%乙醇中48h; (1) Pretreatment: Air-dry the zhennan branches, crush and sieve to a particle size of 80 mesh, soak in 95% ethanol for 48 hours;

(2)超声波处理:取适量步骤(1)处理后的粉料,将其浸入溶剂中,40℃下超声波处理120min; (2) Ultrasonic treatment: take an appropriate amount of powder treated in step (1), immerse it in a solvent, and ultrasonically treat it at 40°C for 120 minutes;

(3)过滤:将步骤2中处理后的溶液进行减压过滤,过滤后的溶液呈透明澄清,无明显杂质; (3) Filtration: the solution treated in step 2 is filtered under reduced pressure, and the filtered solution is transparent and clear without obvious impurities;

(4)减压蒸馏:将步骤3所得液体加入旋转蒸发仪进行减压蒸馏,压力为0.09MPa,温度为40℃,得粗提物; (4) Distillation under reduced pressure: add the liquid obtained in step 3 into a rotary evaporator to carry out distillation under reduced pressure at a pressure of 0.09 MPa and a temperature of 40° C. to obtain a crude extract;

(5)脱水:将粗产品过无水硫酸钠除水,温度为2℃,时间为40h,除水后即为桢楠树枝精油; (5) Dehydration: remove the water from the crude product sodium persulfate anhydrous, the temperature is 2°C, the time is 40h, after the water is removed, it is the essential oil of zhennan tree;

将所得桢楠树枝精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained essential oil of Phoebe zhennan was analyzed by GC-MS, and its main components and pharmacology are the same as above, but the proportions of main components are different.

实施例6 Example 6

(1)预处理:将桢楠阴沉料风干,粉碎过筛后粒度为80目; (1) Pretreatment: Air-dry the zhennan cloudy material, crush and sieve, and the particle size is 80 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:10加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:10, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品过无水硫酸钠除水,温度为0℃,时间为40h,除水后即为桢楠树阴沉料精油; (3) Dehydration: remove the water from the crude product sodium peroxysulfate, the temperature is 0°C, the time is 40h, after the water is removed, it is the essential oil of Phoebe zhennan;

将所得桢楠阴沉料精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 GC-MS analysis was carried out on the obtained zhennan cloudy essential oil, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例7 Example 7

(1)预处理:将桢楠树干风干,粉碎过筛后粒度为120目; (1) Pretreatment: Air-dry the trunk of Phoebe zhennan, crush and sieve, and the particle size is 120 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:8加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:8, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品过无水硫酸钠除水,温度为0℃,时间为40h,除水后即为桢楠树干精油; (3) Dehydration: remove the water from the crude product sodium persulfate anhydrous, the temperature is 0°C, the time is 40h, after the water is removed, it is the trunk essential oil of Phoebe zhennan;

将所得桢楠树干进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained Phoebe zhennan trunk was subjected to GC-MS analysis, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例8 Example 8

(1)预处理:将桢楠树枝风干,粉碎过筛后粒度为60目; (1) Pretreatment: Air-dry the zhennan branches, crush and sieve, and the particle size is 60 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:8加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:8, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品过无水硫酸钠除水,温度为0℃,时间为40h,除水后即为桢楠树枝精油; (3) Dehydration: remove the water from the crude product sodium persulfate anhydrous, the temperature is 0°C, the time is 40h, after the water is removed, it is the essential oil of zhennan tree;

将所得桢楠树枝进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained Phoebe zhennan branches were analyzed by GC-MS, and the main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例9 Example 9

(1)预处理:将桢楠树叶风干,粉碎过筛后粒度为4目; (1) Pretreatment: air-dry the leaves of Phoebe zhennan, pulverize and sieve, and the particle size is 4 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:8加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:8, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品过无水硫酸钠除水,温度为0℃,时间为20h,除水后即为桢楠树叶精油; (3) Dehydration: the crude product is dehydrated by sodium peranhydrous sulfate, the temperature is 0°C, and the time is 20 hours. After dehydration, it is the essential oil of zhennan leaves;

将所得桢楠树叶进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained zhennan leaves were analyzed by GC-MS, and the main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例10 Example 10

(1)预处理:将桢楠树皮风干,粉碎过筛后粒度为40目; (1) Pretreatment: Air-dry the bark of Phoebe zhennan, pulverize and sieve, and the particle size is 40 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:8加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:8, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品过无水硫酸钠除水,温度为0℃,时间为40h,除水后即为桢楠树皮精油; (3) Dehydration: the crude product sodium peranhydrous sulfate is dehydrated, the temperature is 0° C., and the time is 40 hours. After dehydration, it is Zhennan bark essential oil;

将所得桢楠树皮进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained zhennan bark was analyzed by GC-MS, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例11 Example 11

(1)预处理:将细叶楠树干风干,粉碎过筛后粒度为80目; (1) pretreatment: air-drying the trunk of Phoebe chinensis, pulverizing and sieving, the particle size is 80 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:8加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:8, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品过无水硫酸钠除水,温度为2℃,时间为30h,除水后即为细叶楠树干精油。 (3) Dehydration: remove the water from the crude product with peranhydrous sodium sulfate at a temperature of 2° C. for 30 hours.

将所得细叶楠树干精油进行GC-MS分析,其精油中主要成分为单萜类和倍半萜类化合物,β-elemene是温莪术中抗肿瘤作用的主要物质基础,具有抗瘤谱广泛,疗效确切,毒副作用轻微,能明显提高肿瘤患者生存质量等突出优点;β-caryophyllene有抗菌、局麻、抗炎、驱蚊虫、抗焦虑、抗抑、止咳郁等作用;γ-cadinene具有祛痰的作用;guaiol具有镇咳、祛痰,治疗支气管炎作用;α-cadinol有强烈的杀螨活性;β-eudesmol可协助开发治疗血管疾病的药物,具有健脾燥湿、抗缺氧作用,并能明显促进胃肠运动。萜类化合物是自然界分布广泛、种类最多的一类植物天然产物,具有重要的生理学和社会学功能,已广泛应用于工农业生产、医药卫生、香料等领域中,是中药具有临床疗效的重要有效成分。因此该细叶楠精油有一定药用养生价值,主要为镇咳、祛痰、抗菌、消炎的作用。 GC-MS analysis was performed on the obtained essential oil of Phoebe chinensis trunk, and the main components of the essential oil were monoterpenes and sesquiterpenoids. It has the advantages of definite curative effect, mild side effects, and can significantly improve the quality of life of tumor patients; β-caryophyllene has antibacterial, local anesthesia, anti-inflammatory, mosquito repellent, anti-anxiety, anti-inhibitory, and cough-relieving effects; γ-cadinene has expectorant Guaiol has antitussive, expectorant, and bronchitis treatment effects; α-cadinol has a strong acaricidal activity; β-eudesmol can assist in the development of drugs for the treatment of vascular diseases, has the effects of invigorating the spleen, drying dampness, and resisting hypoxia. Can significantly promote gastrointestinal motility. Terpenoids are the most widely distributed and most diverse plant natural products in nature. They have important physiological and sociological functions and have been widely used in industrial and agricultural production, medicine and hygiene, spices and other fields. Element. Therefore, the essential oil of Phoebe chinensis has a certain medicinal value for health preservation, mainly for antitussive, expectorant, antibacterial, and anti-inflammatory effects.

实施例12 Example 12

(1)预处理:将细叶楠树叶风干,粉碎过筛后粒度为10目; (1) Pretreatment: air-dry the leaves of Phoebe chinensis, pulverize and sieve, and the particle size is 10 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:10加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:10, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度为2℃,时间为30h,除水后即为细叶楠树叶精油; (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure, the temperature is 2°C, and the time is 30 hours. After dehydration, it is the essential oil of Phoebe chinensis leaves;

将所得细叶楠树叶精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 GC-MS analysis was carried out to the essential oil of the leaves of Phoebe chinensis, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例13 Example 13

(1)预处理:将细叶楠树枝风干,粉碎过筛后粒度为60目; (1) pretreatment: air-dry the branches of Phoebe chinensis, pulverize and sieve, and the particle size is 60 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:12加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:12, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度为0℃,时间为40h,除水后即为细叶楠树枝精油; (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure, the temperature is 0°C, and the time is 40 hours. After dehydration, it is the essential oil of Phoebe twigs;

将所得细叶楠树枝精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained Phoebe twig essential oil was analyzed by GC-MS, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例14 Example 14

(1)预处理:将细叶楠树皮风干,粉碎过筛后粒度为80目; (1) Pretreatment: air-dry the bark of Phoebe chinensis, crush and sieve, and the particle size is 80 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:10加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:10, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度为0℃,时间为40h,除水后即为细叶楠树皮精油; (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure, the temperature is 0°C, and the time is 40h. After dehydration, it is the bark essential oil of Phoebe chinensis;

将所得细叶楠树皮精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 The obtained Phoebe bark essential oil was analyzed by GC-MS, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例15 Example 15

(1)预处理:将细叶楠树根风干,粉碎过筛后粒度为100目; (1) pretreatment: air-dry the roots of Phoebe chinensis, pulverize and sieve, and the particle size is 100 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:12加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:12, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度为3℃,时间为40h,除水后即为细叶楠树根精油; (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure at a temperature of 3° C. for 40 hours. After dehydration, it becomes the root essential oil of Phoebe chinensis;

将所得细叶楠树根精油进行GC-MS分析,其主要成分及药理同上,主要成分比例不同。 GC-MS analysis was carried out to the essential oil of the obtained Phoebe chinensis root, and its main components and pharmacology were the same as above, but the proportions of the main components were different.

实施例16 Example 16

(1)预处理:将闽楠树干风干,粉碎过筛后粒度为100目; (1) Pretreatment: Air-dry the trunk of Phoebe nannesis, pulverize and sieve, and the particle size is 100 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:10加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:10, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度3℃,时间为40h,除水后即为闽楠树干精油。 (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure at a temperature of 3° C. for 40 hours. After dehydration, it becomes the essential oil of Phoebe basilica.

实施例17 Example 17

(1)预处理:将闽楠木质部风干,粉碎过筛后粒度为100目; (1) Pretreatment: Air-dry the xylem of Phoebe nangifolia, crush and sieve, and the particle size is 100 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:10加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:10, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度为2℃,时间为30h,除水后即为闽楠木质部精油。 (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure at 2° C. for 30 hours. After dehydration, it becomes Phoebe xylem essential oil.

实施例18 Example 18

(1)预处理:将紫楠树干风干,粉碎过筛后粒度为80目; (1) pretreatment: air-drying the trunk of Zinan, pulverized and sieved, and the particle size is 80 mesh;

(2)水蒸气蒸馏:将步骤(1)预处理后的粉料按照料液比为1:8加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the pretreated powder in step (1) according to the solid-liquid ratio of 1:8, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度为0℃,时间为40h,除水后即为紫楠树干精油。 (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure at a temperature of 0° C. for 40 hours. After dehydration, it becomes the essential oil of Phoebe chinensis.

实施例19 Example 19

(1)预处理:将紫楠果实风干,粉碎过筛后粒度为60目; (1) Pretreatment: Air-dry the fruit of Zinan, pulverize and sieve, and the particle size is 60 mesh;

(2)水蒸气蒸馏:向步骤1中过筛的紫楠果实粉按照料液比为1:10加入10%的NaCl水溶液,用水蒸气提取装置进行提取,提取时间为6h,得粗产品; (2) Steam distillation: add 10% NaCl aqueous solution to the cinnamon fruit powder sieved in step 1 according to the ratio of material to liquid of 1:10, and extract with a steam extraction device for 6 hours to obtain a crude product;

(3)脱水:将粗产品进行低温、常压干燥脱水,温度为5℃,时间为30h,除水后即为紫楠果实精油。 (3) Dehydration: The crude product is dried and dehydrated at low temperature and normal pressure at a temperature of 5° C. for 30 hours. After dehydration, it becomes the essential oil of nannus fruit.

以上显示和描述了本发明的基本原理和主要特征及本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。 The basic principles and main features of the present invention and the advantages of the present invention have been shown and described above. Those skilled in the industry should understand that the present invention is not limited by the above-mentioned embodiments. What are described in the above-mentioned embodiments and the description only illustrate the principle of the present invention. Without departing from the spirit and scope of the present invention, the present invention will also have Variations and improvements are possible, which fall within the scope of the claimed invention. The protection scope of the present invention is defined by the appended claims and their equivalents.

Claims (4)

1.一种楠木精油制备的方法,其特征在于,包括以下步骤:1. a method for preparing Phoebe essential oil, is characterized in that, comprises the following steps: 第一步,将楠木预处理,得到楠木预处理料;The first step is to pretreat nanmu to obtain nanmu pretreatment material; 第二步,将楠木预处理料和溶剂加入到超声波处理装置;In the second step, the nanmu pretreatment material and solvent are added to the ultrasonic treatment device; 第三步,将超声波处理后的原料转移到提取装置,并从中分离出含有溶剂的精油;In the third step, the raw material after ultrasonic treatment is transferred to the extraction device, and the essential oil containing solvent is separated from it; 第四步,将精油与溶剂分离;The fourth step is to separate the essential oil from the solvent; 第五步,精油脱水;The fifth step, essential oil dehydration; 所述第一步中,原料为楠木属、润楠属及其近缘属树种的木材,预处理为将楠木的树皮、树干、树根、树梢、树枝、花、果实等原料自然风干或烘干后粉碎,粉碎后过筛,过筛目数为2~100目;In the first step, the raw material is wood of Phoebe genus, Phoebe genus and its close relative species, and the pretreatment is to dry the bark, trunk, roots, treetops, branches, flowers, fruits and other raw materials of Phoebe chinensis naturally Or dried and pulverized, then sieved after pulverized, with a sieve mesh of 2 to 100 mesh; 所述第三步中提取装置为有机溶剂提取装置,或水蒸气提取装置;The extraction device in the third step is an organic solvent extraction device, or a water vapor extraction device; 所述第三步中,分离出含有溶剂的精油采用的方法为减压过滤法、板框过滤法、压滤法或冷凝回流法;In the third step, the method used to separate the essential oil containing solvent is vacuum filtration, plate and frame filtration, pressure filtration or condensation reflux; 所述第四步中,精油与溶剂分离的方法为减压蒸馏法、重力分离法、离心分离法;In the fourth step, the method for separating the essential oil from the solvent is vacuum distillation, gravity separation, centrifugal separation; 所述第五步中,精油脱水采用无水硫酸钠脱水,或常压低温干燥法脱水。In the fifth step, the essential oil is dehydrated by anhydrous sodium sulfate, or dehydrated by normal pressure and low temperature drying. 2.如权利要求1所述的一种楠木精油的制备方法,其特征在于:2. the preparation method of a kind of Phoebe essential oil as claimed in claim 1, is characterized in that: 所述第二步中,将楠木预处理料加入到超声波处理装置内,进行超声波处理;溶剂为乙醇、乙酸乙酯、丙酮、乙醚中的一种或一种以上;溶剂添加量为10-40ml/g楠木预处理料;浸提时间为3~48h;超声处理时间为10~120min,温度为10~60℃,超声波频率为20~80Hz;In the second step, the nanmu pretreatment material is added into the ultrasonic treatment device for ultrasonic treatment; the solvent is one or more of ethanol, ethyl acetate, acetone, ether; the solvent addition amount is 10-40ml /g nanmu pretreatment material; the extraction time is 3-48h; the ultrasonic treatment time is 10-120min, the temperature is 10-60°C, and the ultrasonic frequency is 20-80Hz; 所述第三步中,将有机溶剂和楠木料渣采用减压过滤的方法过滤后转移;减压过滤的滤孔孔径为0.2~0.8μm;In the third step, the organic solvent and Phoebe wood residue are filtered by vacuum filtration and then transferred; the filter pore diameter of vacuum filtration is 0.2-0.8 μm; 所述第四步中,将过滤后的滤液进行减压蒸馏,得到粗提物;减压浓缩的压力为0.03~0.1MPa,温度为30-70℃;In the fourth step, the filtered filtrate is subjected to vacuum distillation to obtain a crude extract; the pressure of vacuum concentration is 0.03-0.1MPa, and the temperature is 30-70°C; 所述第五步,将粗提物过无水硫酸钠除水;所述无水硫酸钠的用量为0.2~1g/ml粗提物;或采用低温常压方法干燥脱水,干燥的温度为0~5℃,时间为5~100h;。In the fifth step, the crude extract is dehydrated by anhydrous sodium sulfate; the dosage of the anhydrous sodium sulfate is 0.2-1g/ml crude extract; ~5℃, the time is 5~100h; 3.如权利要求1所述的一种楠木精油的制备方法,其特征在于:3. the preparation method of a kind of Phoebe essential oil as claimed in claim 1, is characterized in that: 所述第二步中,将楠木预处理料加入到超声波处理装置内,进行超声波处理;溶剂为0~20%的NaCl水溶液;溶剂添加量为3~10ml/g楠木预处理料;超声处理时间为5~60min,温度为10~60℃,超声波频率为20~80Hz;In the second step, the nanmu pretreatment material is added into the ultrasonic treatment device for ultrasonic treatment; the solvent is 0 to 20% NaCl aqueous solution; the solvent addition amount is 3 to 10ml/g nanmu pretreatment material; the ultrasonic treatment time 5~60min, temperature 10~60℃, ultrasonic frequency 20~80Hz; 所述第三步中,采用水蒸气提取装置进行提取;提取时间为5~10h;In the third step, extraction is performed using a steam extraction device; the extraction time is 5 to 10 hours; 所述第三步中,将夹带有提取物的水蒸气采用冷凝回流的方法收集;In the third step, the water vapor entrained with the extract is collected by condensation and reflux; 所述第四步中,采用重力分离法或离心分离法进行分离,重力分离法静置10-60min,离心分离法转速为1000-4000RPM,时间为1-10min;In the fourth step, adopt gravity separation method or centrifugal separation method to separate, gravity separation method stands still for 10-60min, centrifugal separation method speed is 1000-4000RPM, time is 1-10min; 所述第五步中,将粗提物过无水硫酸钠除水;所述无水硫酸钠的用量为0.2~1g/ml粗提物;或采用低温常压方法干燥脱水,干燥的温度为0~5℃,时间为5~100h。In the fifth step, the crude extract is dehydrated by anhydrous sodium sulfate; the dosage of the anhydrous sodium sulfate is 0.2-1g/ml crude extract; 0~5℃, the time is 5~100h. 4.一种楠木精油,其特征在于:可由权利要求1、2、3所述三种方法中任意一种方法制备得到。4. A nanmu essential oil is characterized in that: it can be prepared by any one of the three methods described in claim 1, 2, and 3.
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CN106290656A (en) * 2016-09-27 2017-01-04 四川农业大学 The method that finger printing differentiates hardwood nanmu is set up based on GC MS technology
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CN114958483A (en) * 2022-04-08 2022-08-30 四川农业大学 Quality-improving and efficiency-increasing method for Photinia sericea essential oil and compound essential oil containing Photinia sericea essential oil
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