CN106174381A - A kind of spice volatile oil and preparation method thereof - Google Patents
A kind of spice volatile oil and preparation method thereof Download PDFInfo
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- CN106174381A CN106174381A CN201610580767.5A CN201610580767A CN106174381A CN 106174381 A CN106174381 A CN 106174381A CN 201610580767 A CN201610580767 A CN 201610580767A CN 106174381 A CN106174381 A CN 106174381A
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- 235000013599 spices Nutrition 0.000 title claims abstract description 77
- 239000000341 volatile oil Substances 0.000 title claims abstract description 72
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- 239000003921 oil Substances 0.000 claims abstract description 43
- 239000000843 powder Substances 0.000 claims abstract description 33
- 238000004821 distillation Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 11
- 238000010298 pulverizing process Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 7
- 235000005747 Carum carvi Nutrition 0.000 claims description 5
- 240000000467 Carum carvi Species 0.000 claims description 5
- 241000628997 Flos Species 0.000 claims description 5
- 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 claims description 5
- 235000007265 Myrrhis odorata Nutrition 0.000 claims description 4
- 240000004760 Pimpinella anisum Species 0.000 claims description 4
- 235000012550 Pimpinella anisum Nutrition 0.000 claims description 4
- 229940101006 anhydrous sodium sulfite Drugs 0.000 claims description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 4
- 238000000605 extraction Methods 0.000 abstract description 10
- 230000006378 damage Effects 0.000 abstract description 3
- 230000000052 comparative effect Effects 0.000 description 14
- 235000007129 Cuminum cyminum Nutrition 0.000 description 12
- 241000510672 Cuminum Species 0.000 description 10
- 238000001256 steam distillation Methods 0.000 description 9
- 239000000203 mixture Substances 0.000 description 8
- 235000013305 food Nutrition 0.000 description 7
- 150000001875 compounds Chemical class 0.000 description 5
- WTWBUQJHJGUZCY-UHFFFAOYSA-N cuminaldehyde Chemical compound CC(C)C1=CC=C(C=O)C=C1 WTWBUQJHJGUZCY-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000000796 flavoring agent Substances 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- YKFLAYDHMOASIY-UHFFFAOYSA-N γ-terpinene Chemical compound CC(C)C1=CCC(C)=CC1 YKFLAYDHMOASIY-UHFFFAOYSA-N 0.000 description 4
- HJCUCLCJVVFBTD-UHFFFAOYSA-N [Na].[Na].S(O)(O)(=O)=O Chemical compound [Na].[Na].S(O)(O)(=O)=O HJCUCLCJVVFBTD-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 235000019634 flavors Nutrition 0.000 description 3
- 239000003205 fragrance Substances 0.000 description 3
- 238000001819 mass spectrum Methods 0.000 description 3
- HQRWWHIETAKIMO-UHFFFAOYSA-N 1-phenylbutan-1-ol Chemical compound CCCC(O)C1=CC=CC=C1 HQRWWHIETAKIMO-UHFFFAOYSA-N 0.000 description 2
- RAHRTJHAYXOITA-UHFFFAOYSA-N 7,7-dimethylbicyclo[4.1.0]hept-4-ene-4-carbaldehyde Chemical compound C1CC(C=O)=CC2C(C)(C)C21 RAHRTJHAYXOITA-UHFFFAOYSA-N 0.000 description 2
- 244000304337 Cuminum cyminum Species 0.000 description 2
- 229930006722 beta-pinene Natural products 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 238000010411 cooking Methods 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000002304 perfume Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000002137 ultrasound extraction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- WTARULDDTDQWMU-UHFFFAOYSA-N β-pinene Chemical compound C1C2C(C)(C)C1CCC2=C WTARULDDTDQWMU-UHFFFAOYSA-N 0.000 description 2
- 206010000087 Abdominal pain upper Diseases 0.000 description 1
- 241000208173 Apiaceae Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 208000019255 Menstrual disease Diseases 0.000 description 1
- 244000046052 Phaseolus vulgaris Species 0.000 description 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- 230000001154 acute effect Effects 0.000 description 1
- 230000003260 anti-sepsis Effects 0.000 description 1
- 230000002421 anti-septic effect Effects 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000001413 cellular effect Effects 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000007791 dehumidification Methods 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 201000006549 dyspepsia Diseases 0.000 description 1
- 230000005670 electromagnetic radiation Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000013355 food flavoring agent Nutrition 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 230000003834 intracellular effect Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- -1 mucosubstance Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000001717 pathogenic effect Effects 0.000 description 1
- 238000005502 peroxidation Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- PANBYUAFMMOFOV-UHFFFAOYSA-N sodium;sulfuric acid Chemical compound [Na].OS(O)(=O)=O PANBYUAFMMOFOV-UHFFFAOYSA-N 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 208000011580 syndromic disease Diseases 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Landscapes
- Fats And Perfumes (AREA)
- Seasonings (AREA)
Abstract
The invention discloses the preparation method of a kind of spice volatile oil, including: S1: spice is carried out pulverizing and obtains spice powder, again described spice powder is put in seal pressure tank, and it is passed through water vapour in described seal pressure tank, after making the vapour pressure in described seal pressure tank reach predetermined critical and balance the scheduled time, instantaneous pressure release is to vacuum state；S2: the described spice powder after step S1 processes is added thermal distillation, collects quintessence oil steam and condenses, obtaining the aqueous quintessence oil of spice；S3: carry out aqueous for described spice quintessence oil separating, be dried, filter, obtain spice volatile oil.The invention also discloses the spice volatile oil prepared by above-mentioned preparation method.The preparation method of the spice volatile oil that the present invention provides is simple to operate, energy-conserving and environment-protective, and extraction time significantly shortens, and quintessence oil yield improves, and avoids destruction spice.
Description
Technical field
The present invention relates to food industrial technical field, particularly relate to a kind of spice volatile oil and preparation method thereof.
Background technology
Spice is to utilize the seed of plant, alabastrum, base of leaf, alabastrum, root block etc., or its extract, has zest fragrant
Taste, gives food with local flavor, appetite stimulator, the effect helping digest and absorbing.Spice contains volatile oil (quintessence oil), pungent becomes
Point and the composition such as organic acid, fiber, starch grain, resin, mucosubstance, colloid, its major part fragrance is from the quintessence oil after distillation.
Spice is widely used in cooking food and food industry, acts primarily as the effects such as perfumery, seasoning, toning.Wherein Fructus Cumini Cymini (is learned
Name: Cuminum cyminum L.), have another name called: cumin, Cuminum cyminum L, be then referred to as Fructus Foeniculi in South Sinkiang.Belong to Umbellales, Umbelliferae
Annual or biennial herb, Herb (in addition to fruit) Glabrous.Fructus Cumini Cymini be distributed mainly on India, Iran, Tu Er its, angstrom
And, China and Central Asia, Fructus Cumini Cymini is the king of flavoring agent, suitable meat cooking, it is also possible to use as spice.Fructus Cumini Cymini also has
The effect of certain anti-lipid peroxidation, has antisepsis to food, can be used for food antiseptic.The fruit of Fructus Cumini Cymini can enter
Medicine, have refreshment promote blood circulation, the effect such as pathogenic fire reducing suppressing the hyperactive liver, can dispelling cold and dehumidification, appetizing of regulating the flow of vital energy, wind-expelling pain-stopping.To dyspepsia, cold syndrome of the stomach pain
Bitterly, suffer from a deficiency of the kidney just frequency, menoxenia the most effective in cure.
The extracting mode of aromatic condiment essential oil is numerous at present, and common includes vapor distillation, extraction, supercritical CO2
Extraction, subcritical abstraction, ultrasonic extraction etc..Wherein due to steam distillation, to have equipment simple, simple to operate, easily real
The advantage such as now, most widely used in the extraction of essential oil of spice；But employing steam distillation, temperature is too high is easily destroyed perfume (or spice)
Expect, the time is longer, quintessence oil yield is on the low side；The shortcoming of other common methods is: extraction impurity is too much, and fragrance is impure；
Supercritical CO2Extraction equipment cost is high, is difficult to bear for small business；Subcritical abstraction easily extracts waxiness etc.,
Use inconvenience；Ultrasonic extraction needs to use organic solvent, and same impurity is too much.
Summary of the invention
For solving above-mentioned technical problem, it is an object of the invention to provide a kind of simple to operate, spice of energy-conserving and environment-protective
The preparation method of volatile oil, extraction time significantly shortens, and quintessence oil yield improves, and avoids destruction spice.
For reaching above-mentioned purpose, the present invention by the following technical solutions:
The invention discloses the preparation method of a kind of spice volatile oil, comprise the following steps:
S1: spice is carried out pulverizing and obtains spice powder, more described spice powder is put in seal pressure tank,
And it being passed through water vapour in described seal pressure tank so that the vapour pressure in described seal pressure tank reaches predetermined critical and puts down
After the weighing apparatus scheduled time, instantaneous pressure release is to vacuum state；
S2: the described spice powder after step S1 processes is added thermal distillation, collects quintessence oil steam and condenses, obtaining
The aqueous quintessence oil of spice；
S3: carry out aqueous for described spice quintessence oil separating, be dried, filter, obtain spice volatile oil.
Preferably, step S2 specifically includes: use far infrared to the described spice powder after step S1 processes
Carry out adding thermal distillation.
Preferably, the temperature using far infrared to carry out adding thermal distillation is 105～115 DEG C, and the time is 10～30min.
Preferably, the separating step in step S3 particularly as follows: by aqueous for described spice quintessence oil rotating speed be 3000～
Centrifugation 3～5min under 6000rpm；Drying steps is particularly as follows: add in the aqueous quintessence oil of described spice through separating
Anhydrous sodium sulfite, is placed in hermetically drying 8～24h in the environment of 0～10 DEG C.
Preferably, step S1 specifically includes: it is fragrant pungent described in 80～120 purposes for spice carrying out pulverizing and obtains granularity
Material powder.
Preferably, the temperature of the described water vapour being passed through in described seal pressure tank in step S1 is 100～160 DEG C,
The predetermined critical of vapour pressure is 0.2～0.6MPa, and the scheduled time of equilibrium step is 0.5～6min.
Preferably, in step S1, vacuum state after instantaneous pressure release is 1～10KPa.
Preferably, step S1 also includes: will be passed through water vapour in described seal pressure tank so that described seal pressure tank
In vapour pressure reach predetermined critical and balance the scheduled time after, the step of instantaneous pressure release to vacuum state repeats at least one
Secondary, preferably it is repeated twice.
Preferably, described spice is Fructus Cumini Cymini, Pericarpium Zanthoxyli, anise, Fructus Foeniculi, Cortex Cinnamomi, Rhizoma Zingiberis Recens, caraway, Sha Jiang, Fructus Foeniculi, bean
Cool, Fructus Piperis, Rhizoma Curcumae Longae or Flos Caryophylli.
The invention also discloses a kind of spice volatile oil prepared by above-mentioned preparation method.
Compared with prior art, the beneficial effects of the present invention is: the preparation method of the spice volatile oil of the present invention,
Whole process belongs to nonsolvent extraction process, not only has the equipment identical with tradition steam distillation simple, simple to operate, easy
The advantages such as realization, and spice powder is placed in by the present invention in the environment of high temperature, high pressure, cell is moistened by superheated vapour
Swollen, hole is full of steam, when moment releases high pressure, the superheated liquid in spice cell hole gasifies rapidly, and volume is anxious
Acute expansion and make cell " explosion ", temperature is reduced to room temperature or lower also with moment, and intracellular quintessence oil dissolution, with water vapour
Form microemulsion, it is to avoid thermal degradation process generation, thus avoid thermo-labile component quilt in prepared spice volatile oil
Decompose and destroy；And simultaneously gained essential oil content exceeds more than 20% than steam distillation, the composition of quintessence oil is more rich and quintessence oil
Characteristic component content is higher, and extraction time significantly shortens, and efficiency is improved and energy-conserving and environment-protective；Prepared by this preparation method
Spice volatile oil can be applicable to food or medicinal applications.
In further scheme, the spice powder crossed through steam treatment is used Far-infrared Heating distillation, profit
Pass principle by electromagnetic radiation heat, conduct heat in direct mode and reach the purpose of heat drying object, thus avoid heating medium body
The energy loss caused, infrared ray has the features such as generation is easy, controllability is good simultaneously, and water is that good infrared heat transfer is situated between
Matter so that this preparation method have heating rapidly, drying time is short, the productivity improves, product quality is improved and device space joint
The advantages such as province.
In further scheme, the preparation method of the spice volatile oil of the present invention can be common to essential oil content
Of a relatively high spice, as Fructus Cumini Cymini, Pericarpium Zanthoxyli, anise, Fructus Foeniculi, Cortex Cinnamomi, Rhizoma Zingiberis Recens, caraway, Sha Jiang, Fructus Foeniculi, Fructus Amomi Rotundus, Fructus Piperis,
Rhizoma Curcumae Longae, Flos Caryophylli etc., applied widely.
Detailed description of the invention
Below in conjunction with preferred embodiment the invention will be further described.
The preferred embodiments of the present invention disclose the preparation method of a kind of spice volatile oil, comprise the following steps:
S1: spice is carried out pulverizing and obtains spice powder, more described spice powder is put in seal pressure tank,
And it being passed through water vapour in described seal pressure tank so that the vapour pressure in described seal pressure tank reaches predetermined critical and puts down
After the weighing apparatus scheduled time, instantaneous pressure release is to vacuum state；
S2: the described spice powder after step S1 processes is added thermal distillation, collects quintessence oil steam and condenses, obtaining
The aqueous quintessence oil of spice；
S3: carry out aqueous for described spice quintessence oil separating, be dried, filter, obtain spice volatile oil.
In a further embodiment, step S2 specifically includes: use far infrared to the institute after step S1 processes
State spice powder to carry out adding thermal distillation.
In a further embodiment, the temperature using far infrared to carry out adding thermal distillation is 105～115 DEG C, and the time is 10
～30min.
In a further embodiment, the separating step in step S3 is particularly as follows: turning aqueous for described spice quintessence oil
Speed is centrifugation 3～5min under 3000～6000rpm；Drying steps particularly as follows: to through separation described spice aqueous
Quintessence oil adds anhydrous sodium sulfite, is placed in hermetically drying 8～24h in the environment of 0～10 DEG C；The anhydrous sodium sulphuric acid wherein added
Sodium can be 1～5% of the quality through the aqueous quintessence oil of described spice separated.
In a further embodiment, step S1 specifically includes: spice carrying out pulverizing and obtains granularity is 80～120
Spice powder described in purpose.
In a further embodiment, the temperature of the described water vapour being passed through in described seal pressure tank in step S1 is
100～160 DEG C, the predetermined critical of vapour pressure is 0.2～0.6MPa, and the scheduled time of equilibrium step is 0.5～6min.
In a further embodiment, in step S1, vacuum state after instantaneous pressure release is 1～10KPa.
In a further embodiment, step S1 also includes: will be passed through water vapour in described seal pressure tank so that institute
State after the vapour pressure in seal pressure tank reaches predetermined critical and balance the scheduled time, the step of instantaneous pressure release to vacuum state
It is repeated at least once more, is preferably repeated twice.
In a further embodiment, described spice be Fructus Cumini Cymini, Pericarpium Zanthoxyli, anise, Fructus Foeniculi, Cortex Cinnamomi, Rhizoma Zingiberis Recens, caraway,
Sha Jiang, Fructus Foeniculi, Fructus Amomi Rotundus, Fructus Piperis, Rhizoma Curcumae Longae or Flos Caryophylli.
The preferred embodiments of the present invention also disclose a kind of spice volatile oil prepared by above-mentioned preparation method.
Following preparation method to the spice volatile oil in the preferred embodiment of the present invention in conjunction with specific embodiments make into
One step illustrates, and the comparative example combining employing tradition vapor distillation method prepares spice volatile oil and makees with reference to comparing.
Comparative example: prepare Fructus Cumini Cymini volatile oil A
Cumin powder is broken to the Fructus Cumini Cymini powder of 80～120 mesh, Fructus Cumini Cymini powder 10 times of deionized waters of addition are carried out steam
Distillation 5h, collects the quintessence oil steam produced and condenses, and condensed fluid, for centrifugation 3min under 6000rpm, is isolated oil reservoir, added
Entering appropriate anhydrous sodium sulfite, be placed in hermetically drying 8h in 4 DEG C of environment, filter to obtain Fructus Cumini Cymini volatile oil A, slightly yellow, yield is
2.7%.
Embodiment 1: prepare Fructus Cumini Cymini volatile oil B
Cumin powder is broken in the cumin powder last input seal pressure tank of 100 mesh, is passed through in seal pressure tank simultaneously
Temperature is the water vapour of 105 DEG C so that in still, vapour pressure reaches 0.2MPa back balance 3min, and instantaneous pressure release is to 6KPa vacuum shape
State, be repeated 2 times be passed through in seal pressure tank water vapour and after balance instantaneous pressure release to vacuum state；
Fructus Cumini Cymini powder after processing utilizes far infrared to carry out adding thermal distillation 15min at 110 DEG C, collects the quintessence oil produced
Steam also condenses, and obtains the aqueous quintessence oil of Fructus Cumini Cymini；
By aqueous for Fructus Cumini Cymini quintessence oil for centrifugation 5min under 4000rpm, isolate oil reservoir, add appropriate anhydrous sodium sulphuric acid
Sodium, is placed in hermetically drying 8h in 4 DEG C of environment, filters to obtain Fructus Cumini Cymini volatile oil B, clear, colorless, and yield is 3.5%.
Embodiment 2: prepare Fructus Cumini Cymini volatile oil C
Cumin powder is broken in the cumin powder last input seal pressure tank of 120 mesh, is passed through in seal pressure tank simultaneously
Temperature is the water vapour of 120 DEG C so that in still, vapour pressure reaches 0.1MPa back balance 5min, and instantaneous pressure release is to 5KPa vacuum shape
State, be repeated 2 times be passed through in seal pressure tank water vapour and after balance instantaneous pressure release to vacuum state；
Fructus Cumini Cymini powder after processing utilizes far infrared to carry out adding thermal distillation 30min at 112 DEG C, collects the quintessence oil produced
Steam also condenses, and obtains the aqueous quintessence oil of Fructus Cumini Cymini；
By aqueous for Fructus Cumini Cymini quintessence oil for centrifugation 3min under 4500rpm, isolate oil reservoir, add appropriate anhydrous sodium sulphuric acid
Sodium, is placed in hermetically drying 12h in 6 DEG C of environment, filters to obtain Fructus Cumini Cymini volatile oil C, clear, colorless, and yield is 3.6%.
Embodiment 3: prepare Fructus Cumini Cymini volatile oil D
Cumin powder is broken in the cumin powder last input seal pressure tank of 90 mesh, in seal pressure tank, is passed through temperature simultaneously
Degree is the water vapour of 150 DEG C so that in still, vapour pressure reaches 0.5MPa back balance 1min, instantaneous pressure release to 8KPa vacuum state,
Be repeated 2 times be passed through in seal pressure tank water vapour and after balance instantaneous pressure release to vacuum state；
Fructus Cumini Cymini powder after processing utilizes far infrared to carry out adding thermal distillation 30min at 110 DEG C, collects the quintessence oil produced
Steam also condenses, and obtains the aqueous quintessence oil of Fructus Cumini Cymini；
By aqueous for Fructus Cumini Cymini quintessence oil for centrifugation 3min under 5500rpm, isolate oil reservoir, add appropriate anhydrous sodium sulphuric acid
Sodium, is placed in hermetically drying 10h in 2 DEG C of environment, filters to obtain Fructus Cumini Cymini volatile oil D, clear, colorless, and yield is 3.8%.
The Fructus Cumini Cymini volatile oil gold that the following preparation method to comparative example and embodiment 1 prepares carries out GC gas chromatogram-MS
Mass spectrum relative analysis.
The volatility of the Fructus Cumini Cymini volatile oil B that the Fructus Cumini Cymini volatile oil A preparing comparative example and embodiment 1 prepare and partly waving
The property sent out composition is detected by gas chromatography-mass spectrum.The condition of gas chromatogram is: chromatographic column: Agilent 19091S-105
(50.0m×0.2mm×0.33μm)；Temperature programming: initial temperature 50 DEG C, 2 DEG C/min temperature programming to 150 DEG C, 4 DEG C/min journey
Sequence is warming up to 270 DEG C, retains 10min；Injector temperature: 250 DEG C；Carrier gas is helium (mass component)；Carrier gas flux: constant
1.0mL/min；Split ratio: 40:1, sample size: 0.6uL；Use area normalization standard measure.
Being detected by above-mentioned gas chromatography-mass spectrum, detection obtains Fructus Cumini Cymini volatile oil A and the embodiment 1 that comparative example prepares
The chemical composition of the Fructus Cumini Cymini volatile oil B prepared and retention time and mass fractions relative thereof are as shown in Table 1 and Table 2.
The component analysis of the Fructus Cumini Cymini volatile oil A that table 1 comparative example prepares
The component analysis of the Fructus Cumini Cymini volatile oil B that table 2 embodiment 1 prepares
From the GC-MS analysis result of Tables 1 and 2 it can be seen that comparative example uses the steam distillation of routine prepare
Fructus Cumini Cymini volatile oil A in the compound that identifies be 90 kinds；And embodiment 1 uses the present invention preparation method prepare diligent
So volatile oil B identifies 102 kinds of compounds, the compound many 12 identified in the steam distillation more conventional than comparative example
Kind, therefore the composition of Fructus Cumini Cymini volatile oil using the preparation method of the present invention to prepare is more rich, i.e. the preparation method system of the present invention
The Fructus Cumini Cymini volatile oil fragrance obtained is abundanter.Wherein cumal is the characteristic flavor compounds of Fructus Cumini Cymini, the Fructus Cumini Cymini that comparative example prepares
The main compound content balance such as table 3 of the Fructus Cumini Cymini volatile oil B that volatile oil A and embodiment 1 prepare.
Table 3 comparative example compares with the characteristic component of the Fructus Cumini Cymini volatile oil that embodiment 1 prepares
| Component target | Comparative example | Embodiment 1 |
| Nopinene | 7.000% | 9.759% |
| Foxlene | 4.177% | 3.681% |
| γ-terpinene | 9.924% | 13.048% |
| Cumal | 26.838% | 30.01% |
| 2-carene-10-aldehyde | 0.693% | 13.958% |
| 1-phenylbutanol | 44.000% | 21.082% |
Nopinene in the Fructus Cumini Cymini volatile oil B that embodiment 1 prepares as can be seen from Table 3, γ-terpinene, cumin
Aldehyde, 2-carene-10-aldehyde are above the Fructus Cumini Cymini volatile oil A that comparative example steam distillation prepares, wherein Foxlene conduct
A kind of terpenes, contributes little, meanwhile, although 1-phenylbutanol content is the highest in steam distillation to the characteristic perfume of Fructus Cumini Cymini
In the inventive method, but the characteristic component in this composition not cumin essential oil, little to the contribution of cumin essential oil local flavor.Therefore, right
Ratio extraction ratio and chemical composition, the yield of the Fructus Cumini Cymini volatile oil that the preparation method of the present invention prepares is higher, and quality is the most excellent.
In sum, the preparation method of comparative example and each embodiment is compared it can be seen that use comparative example to prepare
Fructus Cumini Cymini volatile oil be slightly yellow, and the preparation method of the present invention prepare Fructus Cumini Cymini volatile oil clear, colorless, quality is more preferably；
The preparation method time of the preferred embodiment of the present invention significantly shortens, and quintessence oil yield improves more than 20%, and composition is abundanter, quintessence oil
The content of characteristic component is higher, and energy-conserving and environment-protective, and owing to the preferred embodiment of the present invention uses instantaneous decompression to carry out breaking cellular wall,
And employing Far-infrared Heating, distillation time is short, it is to avoid in volatile oil, thermo-labile component is decomposed destruction.
The Fructus Cumini Cymini volatile oil of the preferred embodiment of the present invention can be applicable to the most of a relatively high other of essential oil content
Spice, as prepared by the preparation method of above preferred embodiment: Pericarpium Zanthoxyli volatile oil, anistree volatile oil, Fructus Foeniculi
Volatile oil, Cortex Cinnamomi volatile oil, Rhizoma Zingiberis Recens volatile oil, caraway volatile oil, husky Rhizoma Zingiberis Recens volatile oil, Fructus Foeniculi volatile oil,
Fructus Amomi Rotundus volatile oil, Fructus Piperis volatile oil, Rhizoma Curcumae Longae volatile oil, Flos Caryophylli volatile oil etc..
Above content is to combine concrete preferred implementation further description made for the present invention, it is impossible to assert
Being embodied as of the present invention is confined to these explanations.For those skilled in the art, do not taking off
On the premise of present inventive concept, it is also possible to make some equivalents and substitute or obvious modification, and performance or purposes are identical, all answer
When being considered as belonging to protection scope of the present invention.
Claims (10)
1. the preparation method of a spice volatile oil, it is characterised in that comprise the following steps:
S1: spice is carried out pulverizing and obtains spice powder, more described spice powder is put in seal pressure tank, and to
Described seal pressure tank is passed through water vapour so that the vapour pressure in described seal pressure tank reaches predetermined critical and balances pre-
After fixing time, instantaneous pressure release is to vacuum state；
S2: the described spice powder after step S1 processes is added thermal distillation, collects quintessence oil steam and condenses, and obtains fragrant pungent
Expect aqueous quintessence oil；
S3: carry out aqueous for described spice quintessence oil separating, be dried, filter, obtain spice volatile oil.
Preparation method the most according to claim 1, it is characterised in that specifically include in step S2: use far infrared to warp
Cross the described spice powder after step S1 processes to carry out adding thermal distillation.
Preparation method the most according to claim 2, it is characterised in that the temperature using far infrared to carry out adding thermal distillation is
105～115 DEG C, the time is 10～30min.
Preparation method the most according to claim 1, it is characterised in that separating step in step S3 is particularly as follows: by described
The aqueous quintessence oil of spice centrifugation 3～5min under rotating speed is 3000～6000rpm；Drying steps is particularly as follows: to through undue
From the aqueous quintessence oil of described spice in add anhydrous sodium sulfite, be placed in hermetically drying 8～24h in the environment of 0～10 DEG C.
Preparation method the most according to claim 1, it is characterised in that specifically include in step S1: spice is carried out powder
The broken granularity that obtains is spice powder described in 80～120 purposes.
Preparation method the most according to claim 1, it is characterised in that be passed through in described seal pressure tank in step S1
The temperature of described water vapour is 100～160 DEG C, and the predetermined critical of vapour pressure is 0.2～0.6MPa, the pre-timing of equilibrium step
Between be 0.5～6min.
Preparation method the most according to claim 1, it is characterised in that in step S1, the vacuum state after instantaneous pressure release is 1
～10KPa.
8. according to the preparation method described in any one of claim 1 to 7, it is characterised in that step S1 also includes: will be to described close
Seal pressure tank is passed through water vapour so that the vapour pressure in described seal pressure tank reaches predetermined critical and balances the scheduled time
After, the step of instantaneous pressure release to vacuum state is repeated at least once more, and is preferably repeated twice.
9. according to the preparation method described in any one of claim 1 to 7, it is characterised in that described spice be Fructus Cumini Cymini, Pericarpium Zanthoxyli,
Anise, Fructus Foeniculi, Cortex Cinnamomi, Rhizoma Zingiberis Recens, caraway, Sha Jiang, Fructus Foeniculi, Fructus Amomi Rotundus, Fructus Piperis, Rhizoma Curcumae Longae or Flos Caryophylli.
10. the spice volatile oil prepared according to the preparation method described in any one of claim 1 to 9.
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