CN105273842A - Preparation method of rose perfume - Google Patents
Preparation method of rose perfume Download PDFInfo
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- CN105273842A CN105273842A CN201510787299.4A CN201510787299A CN105273842A CN 105273842 A CN105273842 A CN 105273842A CN 201510787299 A CN201510787299 A CN 201510787299A CN 105273842 A CN105273842 A CN 105273842A
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Abstract
The invention relates to a preparation method of rose perfume. Firstly, fresh roses are frozen and dried in vacuum and then are smashed into 40-60 mesh fine particles, and then the raw materials are extracted through a supercritical carbon dioxide extraction method in different stages; in the first stage, extraction pressure intensity is 8-14 MPa, and extraction time is 60-70 s; in the second stage, extraction pressure intensity is 15-21 MPa, and extraction time is 50-60 s; in the third stage, extraction pressure intensity is 22-28 MPa, and extraction time is 40-50 s; in the fourth stage, extraction pressure intensity is 28-34 MPa, and extraction time is 30-40 s; finally, the rose perfume is obtained through membrane passing and decompression concentration. The preparation method is simple, the content of aroma substances of the rose perfume is high, aroma is pure and natural, stability is good, and the perfume has the vivid aroma characteristic of natural roses and can be widely used for perfuming daily chemicals, tobacco and other products.
Description
Technical field
The present invention relates to a kind of preparation method of Rose spices, belong to spices preparing technical field.
Background technology
Rose aroma overflows, and enjoys people to like, is a kind of perfume material of important fragrance of a flower style, the essential oil prepared by Rose give off a strong fragrance by, someone is referred to as " liquid golden ", is widely used in the fields such as food, makeup and essence and flavoring agent, has great using value and economic worth.
The production of current China Rose spices mainly adopts traditional steam distillation, organic solvent extraction, and because technique is backward and technical qualification are poor, product yield is low, unstable product quality, and the Rose utilization of resources is extremely insufficient.
Summary of the invention
The object of the invention is, in order to solve the complicated and fragrance problem that alcohol is not positive of existing Rose spices complex steps in extraction and preparation process, to provide a kind of preparation method simply, the preparation method of the Rose spices of step easy handling.
The present invention adopts following technical scheme: a kind of preparation method of Rose spices, comprises the steps:
(1) raw materials pretreatment: carry out microwave vacuum freeze drying for raw material with new fresh-rose, the water content making raw material is 5.5 ~ 7.5%, completes drying, is then crushed into 40 ~ 60 object fine particles;
(2) supercritical extraction: the Rose raw material after pulverizing is loaded in the extraction kettle of supercritical extracting equipment, carry out supercritical carbon dioxide extraction, the temperature of extraction kettle is 35 ~ 50 DEG C, the flow of carbonic acid gas is 17 ~ 23 liters/min, after supercritical carbon dioxide extraction terminates, in the separating still of supercritical extracting equipment, take out rose extracting thing, the temperature of separating still is 53 ~ 58 DEG C, and the pressure of separating still is 5.0 ~ 5.5Mpa;
(3) dissolving of supercritical extract: be separated the rose extracting thing obtained with anhydrous alcohol solution, the mass ratio of dehydrated alcohol and rose extracting thing is 490 ~ 510:4.7 ~ 5.4, at room temperature slowly stirring makes rose extracting thing fully dissolve in ethanol, obtains rose extracting thing solution;
(4) film is crossed: rose extracting thing solution step (3) obtained carries out membrane filtration, the macromole wax in removing rose extracting thing solution;
(5) filtered liquid concentrates: the rose extracting thing solution by membrane filtration is carried out concentrating under reduced pressure on the rotary evaporator, bath temperature is 40 ~ 50 DEG C, vacuum tightness is 0.090 ~ 0.098Mpa, and the enriched material obtained is drop into raw materials quality 25 ~ 32 ‰, namely obtains Rose spices.
Further, pre-freezing temperature when microwave vacuum freeze is dry in described step (1) is-30 ~-20 DEG C, and vacuum tightness is 0.092 ~ 0.01MPa, and microwave power is 6 ~ 8 watts.
Further, described supercritical extraction is divided into four-stage according to extraction pressure: the first stage: extraction pressure 8 ~ 14Mpa, extraction time is 60 ~ 70s, subordinate phase: extraction pressure 15 ~ 21Mpa, extraction time is 50 ~ 60s, the phase III: extraction pressure 22 ~ 28Mpa, and extraction time is 40 ~ 50s, fourth stage: extraction pressure 28 ~ 34Mpa, extraction time is 30 ~ 40s.
Further, the maximum molecular weight that the film that in described step (4), membrane filtration is selected can retain is 6000 ~ 8000, and pressure during membrane filtration is 0.1 ~ 0.4MPa.
Preparation method of the present invention is simple, adopt the method for supercritical extraction stage by stage carry out Rose spices extraction and extraction pressure carry out successively from low to high, to greatest extent the aroma component extraction in Rose can be come, the Rose spices adopting the present invention to prepare not only maintains the original appearance of rose fresh idea perfume (or spice), and body note, the flavor matter content of basic note is high, through GC-MS composition analysis, the Rose spices of preparation identifies more than 50 kind of flavor matter, and form the main flavor matter of Rose Essentielle, wherein geraniol, Geraniol, phenylethyl alcohol, vernol, farnesol, the content of the sub-phenol methyl ether of cloves and ester class thereof is 41.51%, spices fragrance is fresh mellow and full, stable lasting, there is natural rose and spend odour characteristics true to nature, macromolecular wax in extract is eliminated by membrane sepn, the Rose spices obtained has good solvability.
Embodiment
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment one: a kind of preparation method of Rose spices, comprises the steps:
(1) raw materials pretreatment: pre-freezing temperature-30 DEG C, vacuum tightness is 0.092MPa, and microwave power is 6 watts, and the water content making raw material is 5.5%, completes drying, dried raw material pulverizing is become 40 object fine particles;
(2) supercritical extraction: the Rose raw material after pulverizing is loaded in the extraction kettle of supercritical extracting equipment, carry out supercritical carbon dioxide extraction stage by stage, the temperature of extraction kettle is 35 DEG C, the flow of carbonic acid gas is 17 liters/min, after supercritical carbon dioxide extraction terminates, in the separating still of supercritical extracting equipment, take out rose extracting thing, the temperature of separating still is 53 DEG C, and the pressure of separating still is 5.0Mpa;
Supercritical extraction is divided into four-stage according to extraction pressure: the first stage: extraction pressure 8Mpa, extraction time is 60s, subordinate phase: extraction pressure 15Mpa, extraction time is 50s, phase III: extraction pressure 22Mpa, extraction time is 40s, fourth stage: extraction pressure 28Mpa, and extraction time is 30s;
(3) dissolving of supercritical extract: be separated the rose extracting thing obtained with anhydrous alcohol solution, the mass ratio of dehydrated alcohol and rose extracting thing is 490:4.7, at room temperature slowly stirring makes rose extracting thing fully dissolve in ethanol, obtains rose extracting thing solution;
(4) cross film: rose extracting thing solution step (3) obtained carries out membrane filtration, the macromole wax in removing rose extracting thing solution, the maximum molecular weight that the film that membrane filtration is selected can retain is 6000, and pressure during membrane filtration is 0.1MPa;
(5) filtered liquid concentrates: the rose extracting thing solution by membrane filtration is carried out concentrating under reduced pressure on the rotary evaporator, and bath temperature is 40 DEG C, and vacuum tightness is 0.098Mpa, and the enriched material obtained is drop into material quantity 25 ‰, namely obtains Rose spices.
Embodiment two: a kind of preparation method of Rose spices, comprises the steps:
(1) raw materials pretreatment: new fresh-rose is carried out microwave vacuum freeze drying, pre-freezing temperature-20 DEG C, vacuum tightness is 0.01MPa, microwave power is 8 watts, the water content making raw material is 7.5%, completes drying, dried raw material pulverizing is become 60 object fine particles;
(2) supercritical extraction: the Rose raw material after pulverizing is loaded in the extraction kettle of supercritical extracting equipment, carry out supercritical carbon dioxide extraction stage by stage, the temperature of extraction kettle is 50 DEG C, the flow of carbonic acid gas is 23 liters/min, after supercritical carbon dioxide extraction terminates, in the separating still of supercritical extracting equipment, take out rose extracting thing, the temperature of separating still is 58 DEG C, and the pressure of separating still is 5.5Mpa;
Supercritical extraction is divided into four-stage according to extraction pressure: the first stage: extraction pressure 14Mpa, extraction time is 70s, subordinate phase: extraction pressure 21Mpa, extraction time is 60s, phase III: extraction pressure 28Mpa, extraction time is 50s, fourth stage: extraction pressure 34Mpa, and extraction time is 40s;
(3) dissolving of supercritical extract: be separated the rose extracting thing obtained with anhydrous alcohol solution, the mass ratio of dehydrated alcohol and rose extracting thing is 510:5.4, at room temperature slowly stirring makes rose extracting thing fully dissolve in ethanol, obtains rose extracting thing solution;
(4) cross film: rose extracting thing solution step (3) obtained carries out membrane filtration, the macromole wax in removing rose extracting thing solution, the maximum molecular weight that the film that membrane filtration is selected can retain is 8000, and pressure during membrane filtration is 0.4MPa;
(5) filtered liquid concentrates: the rose extracting thing solution by membrane filtration is carried out concentrating under reduced pressure on the rotary evaporator, and bath temperature is 50 DEG C, and vacuum tightness is 0.090Mpa, and the enriched material obtained is drop into material quantity 32 ‰, namely obtains Rose spices.
Embodiment three: a kind of preparation method of Rose spices, comprises the steps:
(1) raw materials pretreatment: new fresh-rose is carried out microwave vacuum freeze drying, pre-freezing temperature-25 DEG C, vacuum tightness is 0.09MPa, microwave power 7 watts, the water content making raw material is 6.5%, completes drying, dried raw material pulverizing is become 50 object fine particles;
(2) supercritical extraction: the Rose raw material after pulverizing is loaded in the extraction kettle of supercritical extracting equipment, carry out supercritical carbon dioxide extraction stage by stage, the temperature of extraction kettle is 40 DEG C, the flow of carbonic acid gas is 20 liters/min, after supercritical carbon dioxide extraction terminates, in the separating still of supercritical extracting equipment, take out rose extracting thing, the temperature of separating still is 55 DEG C, and the pressure of separating still is 5.2Mpa;
Supercritical extraction is divided into four-stage according to extraction pressure: the first stage: extraction pressure 11Mpa, extraction time is 65s, subordinate phase: extraction pressure 18Mpa, extraction time is 55s, phase III: extraction pressure 25Mpa, extraction time is 44s, fourth stage: extraction pressure 31Mpa, and extraction time is 37s;
(3) dissolving of supercritical extract: be separated the rose extracting thing obtained with anhydrous alcohol solution, the mass ratio of dehydrated alcohol and rose extracting thing is 500:4.9, at room temperature slowly stirring makes rose extracting thing fully dissolve in ethanol, obtains rose extracting thing solution;
(4) cross film: rose extracting thing solution step (3) obtained carries out membrane filtration, the macromole wax in removing rose extracting thing solution, the maximum molecular weight that the film that membrane filtration is selected can retain is 7000, and pressure during membrane filtration is 0.3MPa;
(5) filtered liquid concentrates: the rose extracting thing solution by membrane filtration is carried out concentrating under reduced pressure on the rotary evaporator, and bath temperature is 46 DEG C, and vacuum tightness is 0.095Mpa, and the enriched material obtained is drop into material quantity 29 ‰, namely obtains Rose spices.
Rose spices prepared by Example two carries out GC-MS detection, and testing conditions is: column temperature: 50 DEG C (stopping 1min) 10 DEG C/min100 DEG C (stopping 8min) 5 DEG C/min240 DEG C (stopping 20min); Carrier gas He; Injector temperature 230 DEG C, EI ionizes mode, ion source temperature 200 DEG C; Ionizing energy 70eV, interface temperature: 250 DEG C; Quality of scanning scope 30 ~ 350; Sample size 0.3uL.In inspection Rose spices, main aroma component is geraniol, Geraniol, phenylethyl alcohol, vernol, farnesol, the sub-phenol methyl ether of cloves and ester class thereof, and content is: 41.51%.
Claims (4)
1. a preparation method for Rose spices, is characterized in that: comprise the steps:
(1) raw materials pretreatment: carry out microwave vacuum freeze drying for raw material with new fresh-rose, the water content making raw material is 5.5 ~ 7.5%, completes drying, is then crushed into 40 ~ 60 object fine particles;
(2) supercritical extraction: the Rose raw material after pulverizing is loaded in the extraction kettle of supercritical extracting equipment, carry out supercritical carbon dioxide extraction, the temperature of extraction kettle is 35 ~ 50 DEG C, the flow of carbonic acid gas is 17 ~ 23 liters/min, after supercritical carbon dioxide extraction terminates, in the separating still of supercritical extracting equipment, take out rose extracting thing, the temperature of separating still is 53 ~ 58 DEG C, and the pressure of separating still is 5.0 ~ 5.5Mpa;
(3) dissolving of supercritical extract: be separated the rose extracting thing obtained with anhydrous alcohol solution, the mass ratio of dehydrated alcohol and rose extracting thing is 490 ~ 510:4.7 ~ 5.4, at room temperature slowly stirring makes rose extracting thing fully dissolve in ethanol, obtains rose extracting thing solution;
(4) film is crossed: rose extracting thing solution step (3) obtained carries out membrane filtration, the macromole wax in removing rose extracting thing solution;
(5) filtered liquid concentrates: the rose extracting thing solution by membrane filtration is carried out concentrating under reduced pressure on the rotary evaporator, bath temperature is 40 ~ 50 DEG C, vacuum tightness is 0.090 ~ 0.098Mpa, and the enriched material obtained is drop into raw materials quality 25 ~ 32 ‰, namely obtains Rose spices.
2. the preparation method of Rose spices as claimed in claim 1, is characterized in that: pre-freezing temperature when microwave vacuum freeze is dry in described step (1) is-30 ~-20 DEG C, and vacuum tightness is 0.092 ~ 0.01MPa, and microwave power is 6 ~ 8 watts.
3. the preparation method of Rose spices as claimed in claim 1, it is characterized in that: described supercritical extraction is divided into four-stage according to extraction pressure: the first stage: extraction pressure 8 ~ 14Mpa, extraction time is 60 ~ 70s, subordinate phase: extraction pressure 15 ~ 21Mpa, extraction time is 50 ~ 60s, the phase III: extraction pressure 22 ~ 28Mpa, and extraction time is 40 ~ 50s, fourth stage: extraction pressure 28 ~ 34Mpa, extraction time is 30 ~ 40s.
4. the preparation method of Rose spices as claimed in claim 1, is characterized in that: the maximum molecular weight that the film that in described step (4), membrane filtration is selected can retain is 6000 ~ 8000, and pressure during membrane filtration is 0.1 ~ 0.4MPa.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105907478A (en) * | 2016-07-06 | 2016-08-31 | 鹰潭华宝香精香料有限公司 | Preparation method of composite herb spice |
| CN107057853A (en) * | 2017-01-16 | 2017-08-18 | 云南中烟新材料科技有限公司 | A kind of cigarette rose composite particles and its application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105907478A (en) * | 2016-07-06 | 2016-08-31 | 鹰潭华宝香精香料有限公司 | Preparation method of composite herb spice |
| CN107057853A (en) * | 2017-01-16 | 2017-08-18 | 云南中烟新材料科技有限公司 | A kind of cigarette rose composite particles and its application |
| CN107057853B (en) * | 2017-01-16 | 2020-06-16 | 云南中烟新材料科技有限公司 | Rose composite particles for cigarettes and application thereof |
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Application publication date: 20160127 |