CN1935965B - Refined volatile oil and its preparing method - Google Patents
Refined volatile oil and its preparing method Download PDFInfo
- Publication number
- CN1935965B CN1935965B CN2005100151229A CN200510015122A CN1935965B CN 1935965 B CN1935965 B CN 1935965B CN 2005100151229 A CN2005100151229 A CN 2005100151229A CN 200510015122 A CN200510015122 A CN 200510015122A CN 1935965 B CN1935965 B CN 1935965B
- Authority
- CN
- China
- Prior art keywords
- volatile oil
- reverse osmosis
- osmosis membrane
- film
- oil reservoir
- 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.)
- Expired - Fee Related
Links
- 239000000341 volatile oil Substances 0.000 title claims abstract description 43
- 238000000034 method Methods 0.000 title abstract description 21
- 239000012528 membrane Substances 0.000 claims abstract description 43
- 238000001223 reverse osmosis Methods 0.000 claims abstract description 42
- 239000000463 material Substances 0.000 claims abstract description 29
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 10
- 229920002647 polyamide Polymers 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000004821 distillation Methods 0.000 claims description 4
- 238000005516 engineering process Methods 0.000 abstract description 11
- 239000000284 extract Substances 0.000 abstract description 10
- 229920006395 saturated elastomer Polymers 0.000 abstract description 9
- 229920002678 cellulose Polymers 0.000 abstract description 8
- 239000001913 cellulose Substances 0.000 abstract description 8
- 229920002492 poly(sulfone) Polymers 0.000 abstract description 7
- 239000004695 Polyether sulfone Substances 0.000 abstract description 6
- 229920006393 polyether sulfone Polymers 0.000 abstract description 6
- 239000007864 aqueous solution Substances 0.000 abstract description 4
- -1 polyphenylene formamide Polymers 0.000 abstract description 3
- 229920002379 silicone rubber Polymers 0.000 abstract description 3
- 239000012141 concentrate Substances 0.000 abstract description 2
- 239000012467 final product Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000003390 Chinese drug Substances 0.000 abstract 2
- 238000007670 refining Methods 0.000 abstract 2
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 abstract 1
- 239000004952 Polyamide Substances 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 229910052731 fluorine Inorganic materials 0.000 abstract 1
- 239000011737 fluorine Substances 0.000 abstract 1
- 125000000623 heterocyclic group Chemical group 0.000 abstract 1
- 229920002521 macromolecule Polymers 0.000 abstract 1
- 239000004945 silicone rubber Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 37
- 239000000243 solution Substances 0.000 description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 238000000605 extraction Methods 0.000 description 10
- 238000001256 steam distillation Methods 0.000 description 10
- 239000000126 substance Substances 0.000 description 7
- 150000001408 amides Chemical class 0.000 description 6
- 125000001153 fluoro group Chemical group F* 0.000 description 6
- 229920000592 inorganic polymer Polymers 0.000 description 6
- 229920000642 polymer Polymers 0.000 description 6
- 241000196324 Embryophyta Species 0.000 description 5
- 239000003814 drug Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 4
- 241000112528 Ligusticum striatum Species 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- 244000138993 panchioli Species 0.000 description 3
- 229920006389 polyphenyl polymer Polymers 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 239000002023 wood Substances 0.000 description 3
- 240000004510 Agastache rugosa Species 0.000 description 2
- KXDAEFPNCMNJSK-UHFFFAOYSA-N Benzamide Chemical compound NC(=O)C1=CC=CC=C1 KXDAEFPNCMNJSK-UHFFFAOYSA-N 0.000 description 2
- OEYQBKYISMRWQB-UHFFFAOYSA-N Santal Chemical compound C=1C(OC)=CC(O)=C(C2=O)C=1OC=C2C1=CC=C(O)C(O)=C1 OEYQBKYISMRWQB-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000000287 crude extract Substances 0.000 description 2
- 239000012153 distilled water Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000019634 flavors Nutrition 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Natural products C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 229920000098 polyolefin Polymers 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 241000758795 Aristolochiaceae Species 0.000 description 1
- 240000006891 Artemisia vulgaris Species 0.000 description 1
- 235000008671 Calycanthus floridus Nutrition 0.000 description 1
- 244000025311 Calycanthus occidentalis Species 0.000 description 1
- 235000008670 Calycanthus occidentalis Nutrition 0.000 description 1
- 244000080208 Canella winterana Species 0.000 description 1
- 235000008499 Canella winterana Nutrition 0.000 description 1
- 241000522254 Cassia Species 0.000 description 1
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000035851 Chrysanthemum leucanthemum Species 0.000 description 1
- 235000008495 Chrysanthemum leucanthemum Nutrition 0.000 description 1
- 235000000604 Chrysanthemum parthenium Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- 241000125183 Crithmum maritimum Species 0.000 description 1
- 244000301850 Cupressus sempervirens Species 0.000 description 1
- 229920000858 Cyclodextrin Polymers 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- 239000001116 FEMA 4028 Substances 0.000 description 1
- 241000628997 Flos Species 0.000 description 1
- 240000006927 Foeniculum vulgare Species 0.000 description 1
- 235000002782 Foeniculum vulgare var dulce Nutrition 0.000 description 1
- 241000576429 Forsythia suspensa Species 0.000 description 1
- 240000007232 Illicium verum Species 0.000 description 1
- 235000008227 Illicium verum Nutrition 0.000 description 1
- 240000008415 Lactuca sativa Species 0.000 description 1
- 235000004520 Lindera benzoin Nutrition 0.000 description 1
- 235000008262 Lindera benzoin var. benzoin Nutrition 0.000 description 1
- 244000167230 Lonicera japonica Species 0.000 description 1
- 235000017617 Lonicera japonica Nutrition 0.000 description 1
- 241000218378 Magnolia Species 0.000 description 1
- 244000246386 Mentha pulegium Species 0.000 description 1
- 235000016257 Mentha pulegium Nutrition 0.000 description 1
- 235000004357 Mentha x piperita Nutrition 0.000 description 1
- 241000219926 Myrtaceae Species 0.000 description 1
- 235000019082 Osmanthus Nutrition 0.000 description 1
- 241000333181 Osmanthus Species 0.000 description 1
- 235000004347 Perilla Nutrition 0.000 description 1
- 244000124853 Perilla frutescens Species 0.000 description 1
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 1
- 241000018646 Pinus brutia Species 0.000 description 1
- 235000011613 Pinus brutia Nutrition 0.000 description 1
- 241000758706 Piperaceae Species 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- 241001093501 Rutaceae Species 0.000 description 1
- 244000223014 Syzygium aromaticum Species 0.000 description 1
- 235000016639 Syzygium aromaticum Nutrition 0.000 description 1
- 241000792902 Valerianaceae Species 0.000 description 1
- 240000001519 Verbena officinalis Species 0.000 description 1
- 235000018718 Verbena officinalis Nutrition 0.000 description 1
- 241000234314 Zingiber Species 0.000 description 1
- 244000273928 Zingiber officinale Species 0.000 description 1
- 235000006886 Zingiber officinale Nutrition 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 description 1
- 235000011175 beta-cyclodextrine Nutrition 0.000 description 1
- 229960004853 betadex Drugs 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000010612 desalination reaction Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000008384 feverfew Nutrition 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 235000008397 ginger Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000001050 hortel pimenta Nutrition 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 235000012045 salad Nutrition 0.000 description 1
- 239000007901 soft capsule Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses refining volatile oil made by reverse osmosis membrane technique for the volatile oil containing saturated aqueous solution. The reverse osmosis membrane can be selected from the following: cellulose, polyamide, polyphenylene formamide, aroma heterocycle, polysulfone, polyethersulfone, polgolefin, silicone rubber, fluorine containing macromolecule. The pressure in the filmis 5-80kg/m2 in concentration process. Vacuum degree out the film is 0- -0.1MPa. The temperature is 5-80 degree centigrade. Liquid flow rate is 10-100L/h. The preparing method of the Chinese drug concentrate includes the following steps: extracting the volatile oil by Chinese drug to gain rough extracted liquid; collecting the rough extracted liquid and cooling; concentrating the distillate by reverse osmosis membrane to gain the refining volatile oil which can be directly added acceptable auxiliary materials to form preparation, also can produce the final product by preparation technology after mixing it with other medicinal materials extract in the composing recipe.
Description
Technical field
The present invention relates to a kind of refined volatile oil, especially through volatile oil of reverse osmosis membrane technology enrichment and preparation method thereof.
Background technology
Volatile oil is the effective constituents in the Chinese medicine, extensively distribute in vegitabilia, China wild with cultivation the fragrance that contains volatile oil and medicinal plant have hundreds of more than, have various pharmacologically active and purposes widely.。Feverfew is as chrysanthemum, wormwood artemisia, rhizoma atractylodis; Rutaceae such as rue, dalbergia wood, Medcinal Evodia Fruit etc.; Samphire such as sweet fennel, Ligusticum wallichii, radix bupleuri Radix Angelicae Sinensis etc.; Labiate such as wrinkled giant hyssop, purple perilla etc., canella such as the root of three-nerved spicebush, Chinese cassia tree etc.; Magnoliacea plant such as star anise, the bark of official magnolia etc.; And the many medicines in the Aristolochiaceae, Valerianaceae, Zingiber, piperaceae, Myrtaceae, horsewhip section all are rich in volatile oil, and the certain plants of sections such as pine, cypress, sweet-scented osmanthus, santal rose also contains abundant volatile oil in addition.Volatile oil contents also has minority content to reach more than 10% generally below 1% in the plant, contains volatile oil as cloves and reaches 14%.
In the prior art, volatile oil adopts the wet distillation mode to extract more, behind the distillate standing demix, isolates oil reservoir, with water layer discarded.But this traditional method can be wasted the volatile oil component that is contained in a large number in the saturated aqua aromatica solution, and these volatile oil components are because in a large amount of water, existing technical conditions can't effectively be separated with equipment, so finally discard, causes waste.In addition, the volatile oil component of part Chinese medicine is water-soluble, does not form the oily water separation layer, also can't separate.More than two kinds of situations, adopt traditional molecule rectificating method still can not obtain good effect.So how effectively utilizing the aromatic saturated aqueous solution to obtain more volatile oil component becomes an interior difficult problem of pharmacy field.
The reverse osmosis membrane beneficiation technologies is meant the promotion by means of outside energy or chemical potential difference, selective osmosis by specific film, realization to the solute in the mixture separate with solvent, classification, purification or spissated technology, because himself many advantages, its Application Areas develop into chemical industry, food, the paper industry separation of some organic and inorganics and concentrate from early stage desalination.Its process is a process efficiently normally, do not undergo phase transition in the membrane sepn process, heating or refrigerative energy consumption are very low, usually carry out at normal temperatures, be particularly suitable for separation, the classification and concentrated of heat-sensitive substance, help keeping biological activity, the physical and chemical stability of product, can significantly reduce loss of active ingredients.In addition, the movement-less part of the equipment that is adopted own, install simple, easy to operate, be easy to automatization and easy to maintenance; Processing power can in very large range change, and efficient, equipment unit price, working cost then change not quite.And with respect to general concentration technique, the product quality that reverse osmosis membrane technology is produced is excellent more.Therefore, reverse osmosis membrane technology has significant advantage with respect to existing concentration technique, can replace chemical industry operation unit such as distillation extraction in the pharmaceutical technology, evaporation, absorption.
Adopt reverse osmosis technology enrichment volatile oil, provide possibility, do not appear in the newspapers so far for effectively obtaining volatile oil component.
Summary of the invention
One of purpose of the present invention is according to the deficiencies in the prior art, and a kind of refined volatile oil is provided, the refined volatile oil that especially saturated aqua aromatica obtains through the rich utmost point of reverse osmosis membrane technology.
Another object of the present invention provides the preparation method of this refined volatile oil.
The present invention is implemented by following technical scheme.
Refined volatile oil of the present invention is characterized in that, is that the saturated aqueous solution that contains this volatile oil makes through the reverse osmosis membrane technology enrichment.
Wherein, described volatile oil saturated aqueous solution is meant the saturated aqua aromatica solution that water-fast volatile oil component obtains after the steam distillation method is extracted, separated; Saturated aqua aromatica solution after the volatile oil component that dissolves each other with water is water-soluble, or the saturated aqua aromatica solution that adopts additive method to obtain.
Described reverse osmosis membrane to be selected from but the material that is not limited to following kind make: Mierocrystalline cellulose, polymeric amide, polyphenyl methane amide, aromatic heterocycle, polysulfones, polyether sulfone, polyolefins, silicon rubber, fluoro containing polymers, inorganic polymer, pottery; Preferably make: Mierocrystalline cellulose, polymeric amide, polysulfones, polyethersulfone, fluoro containing polymers, inorganic polymer, pottery with the material of following kind; The best is made with the material of following kind: polymeric amide, polysulfones, fluoro containing polymers, inorganic polymer.
Film internal pressure scope is 5～80kg/m in the described enrichment process
2, preferred 10～60kg/m
2, more preferably 10～40kg/m
2, the best is 10～30kg/m
2
The outer vacuum ranges of described film is 0～-0.1mpa, preferred-0.02～-0.1mpa, more preferably-0.04～-0.1mpa, the best is-0.080～-0.1mpa.
Described enrichment process temperature range is: 5～80 ℃, preferred 10～60 ℃, more preferably 10～50 ℃, the best is 20～35 ℃.
Described enrichment process flow rate of liquid is: 10～100L/h, and preferred 20～80L/h, more preferably 30～60L/h, the best is 40～50L/h.
Refined volatile oil of the present invention can directly add acceptable accessories and make preparation, also can be the extract of single in the compound or a few flavor medicines, after mixing with the extract of other medicinal materials in the prescription, makes final product through preparation process again.
The preparation method of refined volatile oil of the present invention may further comprise the steps:
1, Chinese medicinal materials extracts volatile oil, gets crude extract;
2, collect crude extract, put cold;
3, distillate is concentrated through reverse osmosis membrane, get refined volatile oil.
Wherein the extraction described in the step 1 refers to conventional essential oil extraction method, as steam distillation, and supercritical CO
2Fluid extraction method etc.
Enrichment process film internal pressure scope described in the step 3 is 5～80kg/m
2, preferred 10～60kg/m
2, more preferably 10～40kg/m
2, the best is 10～30kg/m
2The outer vacuum ranges of film is 0～-0.1mpa, preferred-0.02～-0.1mpa, more preferably-0.04～-0.1mpa, the best is-0.08～-0.1mpa; Described enrichment process temperature range is: 5～80 ℃, preferred 10～80 ℃, the best is 20～80 ℃; Described enrichment process flow rate of liquid is: 10～100L/h, and preferred 20～80L/h, more preferably 30～60L/h, the best is 40～50L/h.
Reverse osmosis membrane described in the step 3 to be selected from but the material that is not limited to following kind make: Mierocrystalline cellulose, polymeric amide, polyphenyl methane amide, aromatic heterocycle, polysulfones, polyether sulfone, polyolefins, silicon rubber, fluoro containing polymers, inorganic polymer, pottery; Preferably make: Mierocrystalline cellulose, polymeric amide, polysulfones, polyethersulfone, fluoro containing polymers, inorganic polymer, pottery with the material of following kind; The best is made with the material of following kind: polymeric amide, polysulfones, fluoro containing polymers, inorganic polymer.
In preparation refined volatile oil of the present invention, the gained dialyzate can be directly used in utilization, or alternative distilled water.
The present invention has following beneficial effect:
1. effective enrichment volatile oil reduces the loss again of volatile component in the vapor enrichment process;
2. reduce the loss of heat-sensitive substance in the volatile oil;
3. mould material does not have absorption to effective constituent;
4. efficient, quick, can simplify production technique, shorten the production cycle;
5. energy efficient;
6. dialyzate can be directly used in and drink, or alternative distilled water.
Embodiment
Variation test and specific embodiment below by Chinese medicine active constituent content before and after the reverse osmosis membrane processing further specify the present invention, but are not construed as limiting the invention.
Embodiment 1
Radix bupleuri medicinal material 100kg adds 8 times of water gaging wet distillations, collects effluent liquid 95kg, puts and is chilled to room temperature.Last reverse osmosis membrane separation device adopts polyamide-based 2m
2Reverse osmosis membrane, film internal pressure 12-25kg/m
2, the outer vacuum tightness of film is-0.1mpa 25 ℃ of temperature, flow velocity 40L/h, acquisition refined volatile oil 0.5kg.
Effluent liquid and refined volatile oil are measured, be the results are shown in Table 1.
Concentration contrast before and after the table 1 Radix Bupleuri volatile oil membrane sepn
The result shows that reverse osmosis membrane does not have absorption substantially.
Embodiment 2
Dalbergia wood medicinal material 100kg adds 6 times of water gaging steam distillations, collects effluent liquid 50kg, separates oil reservoir 1L, puts and is chilled to room temperature.Reverse osmosis membrane separation device on the effluent liquid behind the separation oil reservoir adopts aluminum oxide, zirconium white polymkeric substance 2m
2Reverse osmosis membrane, film internal pressure 10-30kg/m
2, the outer vacuum tightness-0.1mpa of film, 80 ℃ of temperature, flow velocity 35L/h gets oil reservoir 0.25L.
Embodiment 3
Radix Angelicae Sinensis medicinal material 80kg adds 6 times of water gaging steam distillations, collects effluent liquid 80kg, separates oil reservoir 1.5L, puts and is chilled to room temperature.Reverse osmosis membrane separation device on the effluent liquid behind the separation oil reservoir adopts polyether sulfone 2m
2Reverse osmosis membrane, film internal pressure 30-50kg/m
2, the outer vacuum tightness 0mpa of film, 30 ℃ of temperature, flow velocity 35L/h gets oil reservoir 0.8L.
Embodiment 4
Ligusticum wallichii medicinal material 80kg adds 5 times of water gaging steam distillations, collects effluent liquid 60kg, separates oil reservoir 1.2L, puts and is chilled to room temperature.Reverse osmosis membrane separation device on the effluent liquid behind the separation oil reservoir adopts cellulose family 4m
2Reverse osmosis membrane, film internal pressure 50-70kg/m
2, 45 ℃ of the outer vacuum tightnesss of film-0.08mpa temperature, flow velocity 40L/h obtains oil reservoir 0.4L.
Embodiment 5
The bright medicinal material 100kg of rhizoma atractylodis adds 5 times of water gaging steam distillations, collects effluent liquid 50kg, separates oil reservoir 4.5L, puts and is chilled to room temperature.Reverse osmosis membrane separation device on the effluent liquid behind the separation oil reservoir adopts polyamide-based 4m
2Reverse osmosis membrane, film internal pressure 60-80kg/m
2, the outer vacuum tightness 0mpa of film, 25 ℃ of temperature, flow velocity 40L/h obtains oil reservoir 1.8L.
Embodiment 6
Fresh ginger medicinal material 100kg adds 6 times of water gaging steam distillations, collects effluent liquid 60kg, separates oil reservoir 2.1L, puts and is chilled to room temperature.Reverse osmosis membrane separation device on the effluent liquid behind the separation oil reservoir adopts polyphenyl benzamide type 6m
2Reverse osmosis membrane, film internal pressure 10-30kg/m
2, the outer vacuum tightness-0.04mpa of film, 40 ℃ of temperature, flow velocity 65L/h obtains oil reservoir 1.8L.
Embodiment 7
Windproof medicinal material 100kg adds 6 times of water gaging steam distillations, collects effluent liquid 60kg, separates oil reservoir 1.6L, puts and is chilled to room temperature.Reverse osmosis membrane separation device on the effluent liquid behind the separation oil reservoir adopts ceramic 2m
2Reverse osmosis membrane, film internal pressure 10-25kg/m
2, the outer vacuum tightness 0mpa of film, 40 ℃ of temperature, flow velocity 50L/h obtains oil reservoir 0.6L.
Embodiment 8
Take by weighing dalbergia wood medicinal material 50kg in extraction tank, regulating extraction temperature is 20 ℃, and pressure is 35Mpa, extracts 6h, CO
2Flow is a 6L/kg medicinal material hour, supercutical fluid CO
2Extract extracting solution 20kg, separate oil reservoir 1.2L.Reverse osmosis membrane separation device on the extracting solution behind the separation oil reservoir adopts polyamide-based 6m2 reverse osmosis membrane, film internal pressure 10-30kg/m
2, the outer vacuum tightness-0.06mpa of film, 35 ℃ of temperature, flow velocity 55L/h obtains oil reservoir 0.6L.
Embodiment 9
Take by weighing Radix Angelicae Sinensis medicinal material 60kg, Ligusticum wallichii medicinal material 40kg is in extraction tank, and regulating extraction temperature is 35 ℃, and pressure is 30Mpa, extracts 5h, CO
2Flow is a 5L/kg medicinal material hour, supercutical fluid CO
2Extract extracting solution 38kg, separate oil reservoir 1.4L, put and be chilled to room temperature.Reverse osmosis membrane separation device on the extracting solution behind the separation oil reservoir adopts polyamide-based 6m
2Reverse osmosis membrane, film internal pressure 30-40kg/m
2, the outer vacuum tightness 0mpa of film, 25 ℃ of temperature, flow velocity 65L/h obtains oil reservoir 0.7L.
Embodiment 10
Wrinkled Gianthyssop Herb medicinal material 40kg adds 6 times of water gaging steam distillations, collects effluent liquid 60kg, separates oil reservoir 1.0L, puts and is chilled to room temperature; Reverse osmosis membrane separation device on the extracting solution behind the separation oil reservoir adopts polyamide-based 6m
2Reverse osmosis membrane, film internal pressure 10-30kg/m
2, the outer vacuum tightness 0mpa of film, 25 ℃ of temperature, flow velocity 50L/h obtains oil reservoir 0.6L, merges oil reservoir, and the adding beta-cyclodextrin is an amount of, and inclusion is standby; Japanese Honeysuckle 30kg, capsule of weeping forsythia 6kg soak half an hour, decoct 2 times, and each 1.5 hours, filter, merging filtrate is put and is chilled to room temperature.Last film enrichment plant adopts cellulose family 6m
2Reverse osmosis membrane, film internal pressure 20-35kg/m
2, the outer vacuum tightness 0.02mpa of film, 25 ℃ of temperature, flow velocity 60L/h is concentrated into density 1.20～1.25 (40 ℃), stirs down, it is an amount of slowly to add ethanol, makes to contain alcohol amount and reach 75%, fully stirs, left standstill 12 hours, it is an amount of that leaching supernatant liquor, residue add 75% ethanol, stirs evenly, left standstill 12 hours, filter, merge ethanol liquid, reclaim ethanol to there not being the alcohol flavor, and be concentrated into the clear cream that relative density is 1.30～1.32 (60～65 ℃), drying under reduced pressure mixes right amount of auxiliary materials such as adding dextrin, adds volatile oil clathrate compound, make particle 10000g, promptly.
Embodiment 11
Take by weighing Flos Chrysanthemi medicinal material 40kg in extraction tank, regulating extraction temperature is 30 ℃, and pressure is 20Mpa, extracts 5h, CO
2Flow is a 5L/kg medicinal material hour, supercutical fluid CO
2Extract extracting solution 15kg, separate oil reservoir 0.8L, put and be chilled to room temperature.Reverse osmosis membrane separation device on the extracting solution behind the separation oil reservoir adopts cellulose family 2m
2Reverse osmosis membrane, film internal pressure 20-40kg/m
2, the outer vacuum tightness-0.08mpa of film, 45 ℃ of temperature, flow velocity 35L/h obtains oil reservoir 0.3L.
Embodiment 12
Peppermint medicinal material 100kg adds 6 times of water gaging steam distillations, collects effluent liquid 50kg, separates oil reservoir 1.2L, puts and is chilled to room temperature.Reverse osmosis membrane separation device on the effluent liquid behind the separation oil reservoir adopts polyamide-based 2m
2Reverse osmosis membrane, film external pressure 10-30kg/m
2, the outer vacuum tightness 0mpa of film, 20 ℃ of temperature, flow velocity 40L/h obtains oil reservoir 0.4L, merges oil reservoir, and the adding salad oil is an amount of, makes soft capsule 10000g, promptly.
Claims (1)
1. the preparation method of a radix bupleuri refined volatile oil is characterized in that, step is: get radix bupleuri medicinal material 100kg, add 8 times of water gaging wet distillations; Collect effluent liquid 95kg, put and be chilled to room temperature; Last reverse osmosis membrane separation device adopts polyamide-based 2m
2Reverse osmosis membrane, film internal pressure 12-25kg/m
2, the outer vacuum tightness of film is-0.1mpa 25 ℃ of temperature, flow velocity 40L/h, acquisition refined volatile oil 0.5kg.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005100151229A CN1935965B (en) | 2005-09-20 | 2005-09-20 | Refined volatile oil and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005100151229A CN1935965B (en) | 2005-09-20 | 2005-09-20 | Refined volatile oil and its preparing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1935965A CN1935965A (en) | 2007-03-28 |
| CN1935965B true CN1935965B (en) | 2010-12-15 |
Family
ID=37953709
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2005100151229A Expired - Fee Related CN1935965B (en) | 2005-09-20 | 2005-09-20 | Refined volatile oil and its preparing method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1935965B (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102703208B (en) * | 2012-05-21 | 2013-06-26 | 管天球 | Tea oil special for children |
| TW201429969A (en) * | 2012-12-20 | 2014-08-01 | Merck Sharp & Dohme | Substituted imidazopyridines as HDM2 inhibitors |
| CN104946395A (en) * | 2015-05-25 | 2015-09-30 | 江苏耐雀生物工程技术有限公司 | Method for extracting lemongrass essential oil |
| CN105106257B (en) * | 2015-08-13 | 2019-04-30 | 南京中医药大学 | A method of extracting bupleurum Chinense volatile oil |
| CN106906047B (en) * | 2017-03-14 | 2020-10-02 | 浙江大学 | Method for adsorbing and extracting water-soluble essential oil from flower aqueous solution |
-
2005
- 2005-09-20 CN CN2005100151229A patent/CN1935965B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 刘培建等.柴胡挥发油提取条件的研究.《河南中医药学刊》.2002,第17卷(第2期), * |
| 王如治等.药剂学.《药剂学》.人民卫生出版社,2000,(第3版),282-283. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1935965A (en) | 2007-03-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103666766B (en) | Method for extracting rose essential oil, rose water and rose aqueous extract from fresh rose flower | |
| CN102021106B (en) | Traditional Chinese medicine health wine and production technology thereof | |
| CN101708063B (en) | Method for concentrating extraction liquid in production of tobacco sheet by papermaking process | |
| CN1935965B (en) | Refined volatile oil and its preparing method | |
| CN102504957A (en) | Method for preparing essential oils | |
| CN102031199A (en) | Method for extracting rose essential oil from fresh rose flowers | |
| CN101564407B (en) | Process for refining isatis root extract by applying membrane separation technique | |
| CN101402900A (en) | Method for extracting rhodamine toner oil and line products from brackish water rose | |
| CN104845406A (en) | Plant dye with functions of health care and color fixation | |
| CN103468409A (en) | Method for extracting Xinyang maojian tea extractum by utilizing subcritical technology | |
| CN108865438A (en) | A kind of cigarette preparation method of Radix Angelicae Sinensis fragrance and the application in cigarette | |
| CN109082357A (en) | The brewage process of health care soft-taste white spirit | |
| CN103655655A (en) | Method for separating active ingredients from medicinal material by membrane technology | |
| CN103655649A (en) | Production technology for concentrating raw material extract of traditional Chinese medicine preparation of anti-inflammation and cholagogic tablet | |
| CN104710831A (en) | Extraction method of odorless perillaldehyde with high stability | |
| CN104189087A (en) | Method for extracting total flavonoid functional substance from folium mori | |
| CN101244092A (en) | Technique for producing instantly mixed concentration medicine liqueur and packing method | |
| CN101301330A (en) | Codonopsis pilosula pollen capsules and preparation thereof | |
| CN1935162A (en) | Chinese medicine concentrate andits preparing method | |
| CN106306203A (en) | Production method of Fu tea concentrated beverage | |
| CN100409856C (en) | Glossy ganoderma extractum preparing process | |
| CN101633616B (en) | Preparation method and medicinal application of tanshinol | |
| CN105343130B (en) | A method of hair propolis is isolated and purified as wasp glue using membrane separation technique | |
| CN102552400A (en) | Concentration process of traditional Chinese medicine liquid extract | |
| CN105907478A (en) | Preparation method of composite herb spice |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C56 | Change in the name or address of the patentee |
Owner name: TASLY PHARMACEUTICAL GROUP CO., LTD. Free format text: FORMER NAME: TIANJIN TASLY PHARM. CO., LTD. |
|
| CP01 | Change in the name or title of a patent holder |
Address after: 300402, No. 1, Liaohe East Road, Beichen Science Park, Beichen District, Tianjin Patentee after: Tasly Pharmaceutical Group Co., Ltd. Address before: 300402, No. 1, Liaohe East Road, Beichen Science Park, Beichen District, Tianjin Patentee before: Tianjin Tianshili Pharmaceutical Co., Ltd. |
|
| CP01 | Change in the name or title of a patent holder | ||
| CP01 | Change in the name or title of a patent holder |
Address after: 300402, No. 1, Liaohe East Road, Beichen Science Park, Beichen District, Tianjin Patentee after: Tasly Pharmaceutical Group Limited by Share Ltd Address before: 300402, No. 1, Liaohe East Road, Beichen Science Park, Beichen District, Tianjin Patentee before: Tasly Pharmaceutical Group Co., Ltd. |
|
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20101215 Termination date: 20190920 |