CN103194312A - Method for extracting essential oil from cypress leaves - Google Patents
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- CN103194312A CN103194312A CN2013101175263A CN201310117526A CN103194312A CN 103194312 A CN103194312 A CN 103194312A CN 2013101175263 A CN2013101175263 A CN 2013101175263A CN 201310117526 A CN201310117526 A CN 201310117526A CN 103194312 A CN103194312 A CN 103194312A
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Abstract
The invention discloses a method for extracting essential oil from cypress leaves. The method comprises the following steps of (1) collecting materials; (2) preprocessing the materials; (3), extracting; (4) condensing and recovering; (5) drying and removing moisture; and (6) bottling to store. By adopting the method, a common domestic micro-wave oven is taken as a micro-wave radiation source; a negative pressure extraction technology is added; the fresh leaves are taken as raw materials; complicated raw material treatment is not needed; any solvent is not added; and the micro-wave is absorbed by the moisture of the material and the material is heated and extracted, so as to achieve the negative pressure distillation and extraction effects of the micro-wave. Compared with the traditional steam distillation method, the method has the advantages that consumption of energy is greatly reduced; the extraction time is shortened; the extraction yield is improved; and waste liquid outflow is avoided. The yield of the essential oil of the cypress leaves extracted by the method can be up to be over 0.5% while the time is just 3-5 minutes; no environmental pollution is generated; and the method is an efficient, energy-saving and environment-friendly extraction mode.
Description
Technical field
The invention belongs to technical field of chemistry, relate to a kind of method of from CedarLeaves, extracting volatile oil.
Background technology
All contain volatile oil mostly in the leaf of Cupressaceae (Cupressaceae) plant.Wherein the most common, resourceful Cupressaceae plant mainly contains arbor-vitae and Chinese juniper.Arbor-vitae (Platycladus orientalis) is the Platycladus plant, claims Japan cypress, arborvitae again, and is wide at Chinese distributed pole, North gets the Inner Mongol, Jilin, reaches Guangdong and the north, Guangxi in the south, and the artificial culture scope spreads all over the country, and resource is very abundant.The Leafy twigs of Oriental Arborvitae delicate fragrance heart of feeling well, bitter and puckery flavor, little suffering.Volatile oil is the main active ingredient of Leafy twigs of Oriental Arborvitae, and its main component is α-Pai Xi, can be widely used in the allotment of reodorant, air freshener and daily cosmetics etc.Traditional Chinese medicine thinks that white cedar leaf oil has cooling blood for hemostasis, growing and blacking hair, removing heat from the lung to relieve cough effect, is used for the treatment of hemorrhage, rheumatic arthralgia, hypertension clinically, coughs and breathe heavily etc.Nearly 70 kinds of Sabina plant, wherein Chinese juniper (Sabina chinensis) extensively is distributed in the Northern Hemisphere.Chinese juniper volatile oil is a kind of miscellany of complexity, and its main component is α-ocimene, is beta-pinene and α-Pai Xi secondly.The Twig and leaf of Przewalsk Juniper essential oil has been widely used as makeup, perfumed soap, sterilizing agent, insect repellent agent, can treat leprosy, typhoid fever, heart, kidney, tuberculosis etc. in addition, has the wide development prospect.
At present, the extracting method of Cupressaceae plant volatile oil mainly contains steam distillation, supercritical CO
2Fluid extraction method, solvent-extraction process, solid-phase microextraction method etc.Traditional steam distillation is to obtain the modal extracting method of volatile oil from scented plants, yet, steam distillation causes the loss of volatile matter easily, extraction efficiency is low, the extraction time is long, and high temperature and water can make some lower boiling small molecule component degradeds and chemical transformation takes place, and are unfavorable for the extraction of determination system of thermal unstable material.Supercritical CO
2Though fluid extraction is much improved in extraction efficiency, required equipment is complicated, and the solvent range of choice is narrow, high pressure container and high-pressure pump, and it is big to set up extensive extraction production line difficulty, the cost height.The power consumption of chemical solvents extraction process is big, and consumptive material is many, length consuming time, and extraction efficiency is low, and the industrial pollution amount is big.The solid-phase microextraction method is a kind of extractive technique of simple and fast, is fit to extraction small molecules and the lower material of boiling point, but is not suitable for for the extraction of macromolecular substance or Ester, and be subjected to the influence of extraction conditions easily, can not get circulation ratio preferably.
Microwave refers to the hertzian wave of frequency between 300MHz～300GHz, and the microwave frequency that is applied to industry and family expenses at present is mainly 915MHz and 2450MHz.Microwave-assisted extraction technique claims microwave-assisted to extract (Microwave-assisted Extraction again, hereinafter to be referred as MAE), it is development in recent years Chinese medicine extracts active ingredients technology rapidly, compare with traditional active ingredient of Chinese herbs extractive technique, have easy, rapidly and efficiently, advantage such as strong, the less energy consumption of selectivity and environmental pollution be little.Microwave has fluctuation, high frequency characteristics and thermal property or non-thermal property (biological effect), thereby characteristics such as the MAE technology has rapidly and efficiently, homogeneous heating, selectivity is strong, biological effect (non-thermal effect) is big.Compare with traditional extractive technique, the advantage that the MAE technology is the most outstanding is that solvent load is few, consuming time less, the property selected is strong, is conducive to extract heat-labile active substance in the Chinese medicine; Can extract a plurality of samples simultaneously, the extraction efficiency height, energy consumption is low, equipment is simple, processing ease, safety, the low pollution.Patent of the present invention provides a kind of method of extracting volatile oil from CedarLeaves on the basis that microwave-assisted extracts, the present invention is subsidized by State Administration of Forestry's forestry public welfare industry special project " Qinling Mountains woods medicine conservation of resources and evaluation and exploration technology research thereof ".
Summary of the invention
The objective of the invention is to overcome the defective that above-mentioned technology exists, a kind of method of extracting volatile oil from CedarLeaves is provided, be a kind of microwave extracting, negative pressure extracting, water distilling apparatus to be combined, do not adding the novel method of extracting Twig of Mourning Cypress volatile oil under the condition of any solvent, its concrete technical scheme is:
A kind of method of extracting volatile oil from CedarLeaves may further comprise the steps:
(1) feedstock capture: gather fresh CedarLeaves (mainly referring to arbor-vitae and Chinese juniper), Best Times is between annual May～October;
(2) raw materials pretreatment: with step (1) gather fresh CedarLeaves, pulverize immediately, adopt common Universalpulverizer to pulverize, grinding particle size is at 0.3mm～0.45mm;
(3) extract: the fresh CedarLeaves crushed material that takes by weighing 180g～220g, pack in the 1000mL distilling flask, be placed on microwave negative pressure extraction device, adjust power to 1600～1800W, frequency 2450MHz, continuous gamma radiation distillation 3.5～5min, and carry out decompress filter simultaneously, pressure-controlling is at 0.045～0.098Mpa, adjust according to the suction filtration situation, all enter condenser system with volatile oil and be as the criterion, till volatile oil content no longer increases in the volatile oil collector, about 3～5min consuming time;
(4) condensation is reclaimed: after microwave distillation and decompress filter, volatile oil enters prolong, and through the water condensation system, volatile oil flows in the returnable bottle;
(5) drying dewaters: by being filled with the glass column of anhydrous sodium sulphate, a small amount of absorbent cotton is spread in the bottom, gets final product with volatile oil;
(6) bottling is preserved: preserve with the sealing of band plug dark glass bottle.
Compared with prior art, beneficial effect of the present invention is:
The present invention with the microwave oven of normal domestic use as microwave radiation source; Increased the negative pressure extraction process; And be raw material with the fresh leaf, need not to carry out complicated raw material and handle; Do not add any solvent, utilize material self moisture absorption microwave to make volatile oil effusion CedarLeaves, and then reach the effect of distillation extraction.Compare with traditional wet distillation, this method has greatly reduced the consumption of energy, has shortened extraction time, has improved the extraction yield, has avoided the waste liquid outflow.The yield of utilizing present method to extract Twig of Mourning Cypress volatile oil can reach more than 0.5%, and the time has only 3～5min, and can not cause environmental pollution, is a kind of efficient, energy-saving and environmental protection type extraction mode.
Description of drawings
Fig. 1 is microwave negative pressure extraction schematic representation of apparatus of the present invention.
Embodiment
Below in conjunction with the drawings and specific embodiments technical scheme of the present invention is done explanation in further detail.
A kind of method of extracting volatile oil from CedarLeaves may further comprise the steps:
(1) feedstock capture: gather fresh CedarLeaves, mainly refer to arbor-vitae and Chinese juniper, Best Times is between annual May～October;
(2) raw materials pretreatment: with step (1) gather fresh CedarLeaves, pulverize immediately, adopt common Universalpulverizer to pulverize, grinding particle size is at 0.3mm～0.45mm;
(3) extract: the fresh CedarLeaves crushed material that takes by weighing 180g～220g, pack in the 1000mL distilling flask, as shown in Figure 1, be placed on microwave negative pressure extraction device, adjust power to 1600～1800W, frequency 2450MHz, continuous gamma radiation distillation 3.5～5min, and carry out decompress filter simultaneously, pressure-controlling is adjusted according to the suction filtration situation at 0.045～0.098Mpa, all entering condenser system with volatile oil is as the criterion, till volatile oil content no longer increases in the volatile oil collector, about 3～5min consuming time;
(4) condensation is reclaimed: after microwave distillation and decompress filter, volatile oil enters prolong, and through the water condensation system, volatile oil flows in the returnable bottle;
(5) drying dewaters: by being filled with the glass column of anhydrous sodium sulphate, a small amount of absorbent cotton is spread in the bottom, gets final product with volatile oil;
(6) bottling is preserved: preserve with the sealing of band plug dark glass bottle.
As shown in Figure 1, microwave negative pressure extraction device comprises three parts: (1) microwave distillation part, and by normal domestic use microwave oven repacking (peak power 1800W, frequency 2450MHz).Be made up of microwave distillation device 1 and distilling flask 2, microwave distillation device operating panel face 3 mainly comprises power switch 4, power regulating switch 5, selection of time switch 6, weight system selector switch 7 and fires mode system selector switch 8; (2) negative pressure equipment that partly adopts of negative pressure extracting is that SHB type circulation ability of swimming is used vacuum pump, rate of air sucked in required 10L/min more; Power 180W; Final vacuum 0.098Mpa, a standard atmospheric pressure, 6～25 ℃ of circulating water temperatures; (3) condensation recovery part is the ortho-water condenser, is made up of prolong 9, recovery tube 10, recovery tube switch 11, receiving flask 12.
Earlier fresh CedarLeaves crushed material is packed in the distilling flask 2, the distilling flask 2 that material will be housed again is placed in the microwave distillation device 1, by synoptic diagram 1 distilling flask 2, recovery tube 10, prolong 9, negative pressure equipment is coupled together.Close recovery tube switch 11, open the power switch 4 on the microwave distillation device operating panel 3, adjust power to 1600～1800W, frequency 2450MHz, continuous gamma radiation distillation 3.5～5min, and open vacuum pump switch 13 simultaneously and carry out the negative pressure extracting, pressure-controlling is at 0.045～0.098Mpa, adjust according to the extracting situation, all enter condenser system with volatile oil and be as the criterion, all enter recovery tube 10 up to volatile oil.Open recovery tube switch 11, volatile oil is recovered in the receiving flask 12.
The above; only be the preferable embodiment of the present invention; protection scope of the present invention is not limited thereto; anyly be familiar with those skilled in the art in the technical scope that the present invention discloses, the simple change of the technical scheme that can obtain apparently or equivalence are replaced and are all fallen within the scope of protection of the present invention.
Claims (1)
1. a method of extracting volatile oil from CedarLeaves is characterized in that, may further comprise the steps:
(1) feedstock capture: gather fresh CedarLeaves, Best Times is between annual May～October;
(2) raw materials pretreatment: with step (1) gather fresh pine needle, pulverize immediately, adopt common Universalpulverizer to pulverize, grinding particle size is at 0.3mm～0.45mm;
(3) extract: the fresh CedarLeaves crushed material that takes by weighing 180g～220g, pack in the 1000mL distilling flask, be placed on microwave negative pressure extraction device, adjust power to 1600～1800W, frequency 2450MHz, continuous gamma radiation distillation 3.5～5min, and carry out decompress filter simultaneously, pressure-controlling is at 0.045～0.098Mpa, till volatile oil content no longer increases in the volatile oil collector;
(4) condensation is reclaimed: after microwave distillation and decompress filter, volatile oil enters prolong, flows in the returnable bottle through condensation volatile oil;
(5) drying dewaters: by being filled with the glass column of anhydrous sodium sulphate, a small amount of absorbent cotton is spread in the bottom with volatile oil;
(6) bottling is preserved: preserve with the sealing of band plug dark glass bottle.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103695181A (en) * | 2013-12-31 | 2014-04-02 | 湖南省百里香天然生物制品开发有限公司 | Preparation method of elsholtziae extract |
| CN103725420A (en) * | 2013-12-20 | 2014-04-16 | 江南大学 | Method and device for extracting nigella plant seed volatile oil and application of volatile oil |
| CN104120035A (en) * | 2014-06-15 | 2014-10-29 | 南京林业大学 | Improved method for extracting volatile oil by steam distillation |
| CN105779126A (en) * | 2016-03-15 | 2016-07-20 | 吉林烟草工业有限责任公司 | Chinese arborvitae twig and leaf absolute oil as well as preparation method and application thereof |
| CN108619906A (en) * | 2018-05-31 | 2018-10-09 | 李兵峰 | Environmentally friendly finishing eliminating smell agent and preparation method thereof |
| CN112961729A (en) * | 2021-03-24 | 2021-06-15 | 西北农林科技大学 | Method for optimizing extraction of peony hydrolat under negative pressure distillation condition |
| CN113845978A (en) * | 2021-11-03 | 2021-12-28 | 上海木汗实业有限公司 | Volatile liquid of hinoki extract and processing method thereof |
| CN114507569A (en) * | 2022-02-28 | 2022-05-17 | 德格宗萨藏医药有限公司 | Extraction process of essential oil of Tibetan cedar at high altitude |
| CN114874854A (en) * | 2022-06-08 | 2022-08-09 | 福建农林大学 | Extraction method of Fujian cypress leaf essential oil |
| WO2023172962A1 (en) * | 2022-03-09 | 2023-09-14 | Hart John F | Microwave extraction of essential oils |
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Cited By (14)
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| CN103725420A (en) * | 2013-12-20 | 2014-04-16 | 江南大学 | Method and device for extracting nigella plant seed volatile oil and application of volatile oil |
| CN103725420B (en) * | 2013-12-20 | 2016-07-13 | 江南大学 | A kind of extract the method for Nigella damascena L. platymiscium Volatile Oil from Seed, device and application |
| CN103695181A (en) * | 2013-12-31 | 2014-04-02 | 湖南省百里香天然生物制品开发有限公司 | Preparation method of elsholtziae extract |
| CN103695181B (en) * | 2013-12-31 | 2015-01-21 | 湖南省百里香天然生物制品开发有限公司 | Preparation method of elsholtziae extract |
| CN104120035A (en) * | 2014-06-15 | 2014-10-29 | 南京林业大学 | Improved method for extracting volatile oil by steam distillation |
| CN105779126A (en) * | 2016-03-15 | 2016-07-20 | 吉林烟草工业有限责任公司 | Chinese arborvitae twig and leaf absolute oil as well as preparation method and application thereof |
| CN108619906A (en) * | 2018-05-31 | 2018-10-09 | 李兵峰 | Environmentally friendly finishing eliminating smell agent and preparation method thereof |
| CN108619906B (en) * | 2018-05-31 | 2021-04-06 | 杭州康嘻环保科技有限公司 | Environment-friendly deodorant for decoration and preparation method thereof |
| CN112961729A (en) * | 2021-03-24 | 2021-06-15 | 西北农林科技大学 | Method for optimizing extraction of peony hydrolat under negative pressure distillation condition |
| CN112961729B (en) * | 2021-03-24 | 2023-10-13 | 西北农林科技大学 | Method for extracting peony hydrosol under optimized negative pressure distillation condition |
| CN113845978A (en) * | 2021-11-03 | 2021-12-28 | 上海木汗实业有限公司 | Volatile liquid of hinoki extract and processing method thereof |
| CN114507569A (en) * | 2022-02-28 | 2022-05-17 | 德格宗萨藏医药有限公司 | Extraction process of essential oil of Tibetan cedar at high altitude |
| WO2023172962A1 (en) * | 2022-03-09 | 2023-09-14 | Hart John F | Microwave extraction of essential oils |
| CN114874854A (en) * | 2022-06-08 | 2022-08-09 | 福建农林大学 | Extraction method of Fujian cypress leaf essential oil |
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Application publication date: 20130710 |