CN103966027A - Preparation method of compound rosemary extract - Google Patents

Preparation method of compound rosemary extract Download PDF

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Publication number
CN103966027A
CN103966027A CN201410204635.3A CN201410204635A CN103966027A CN 103966027 A CN103966027 A CN 103966027A CN 201410204635 A CN201410204635 A CN 201410204635A CN 103966027 A CN103966027 A CN 103966027A
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rosmarinus officinalis
extract
base
extraction
leaf
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CN201410204635.3A
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CN103966027B (en
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殷飞
韩婷
胡忠豪
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Shenzhen Tianxiang Fu Biotechnology Co. Ltd.
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Jiaxing City Obtains Encyclopaedia Novel Material Science And Technology Ltd
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Abstract

The invention discloses a preparation method of a compound rosemary extract. The preparation method comprises the following steps: (1) freezing fresh rosemary leaf stems in a low-temperature environment; (2) taking out the rosemary leaf stems from a freezing room, and freeze-drying the rosemary leaf stems in vacuum; (3) grinding the rosemary leaf stems; (4) performing ethanol extraction on rosemary leaf stem powder by stirring; (5) centrifuging extracting liquid, collecting supernatant liquid, and concentrating to obtain a rosemary ethanol extract; (6) depositing the centrifuged rosemary and performing supercritical CO2 extraction; (7) collecting rosemary extracts from a primary separation kettle and a secondary separation kettle; (8) mixing the ethanol extract, the primary separation extract and the secondary separation extract and compounding to obtain the compound rosemary extract. The compound rosemary extract prepared by adopting the method has the effects of effectively improving the aroma quantity and the aroma quality of cigarettes, improving the mouth feel of the cigarettes and increasing the smoke concentration of the cigarettes.

Description

The preparation method of the composite extract of a kind of Rosmarinus officinalis
Technical field
The present invention relates to a kind of preparation method of tobacco spice, particularly relate to the preparation method of the composite extract of a kind of Rosmarinus officinalis.
Background technology
Rosmarinus officinalis is Labiatae Rosmarinus plant, is evergreen dwarf shrub, and country of origin is Europe and Mediterranean.Rosmarinus officinalis, due to its unique odour characteristics, is widely used in the middle of tobacco, perfumed soap, makeup, toothpaste etc.In addition, have a large amount of antioxidant components in Rosmarinus officinalis, these antioxidant components have higher antioxygenation.
In Field of Tobacco, the application of rosemary extract in the middle of tobacco is less, rosemary ethereal oil is owing to containing the aroma components such as a large amount of α-pinenes, cineole, camphor, borneol, kautschin, these nonpolar extracts are applied in the middle of tobacco, may effectively improve concentration and the quality of flue gas.In the middle of current research, to Rosmarinus officinalis ethanol extraction to be applied to research in tobacco considerably less, Rosmarinus officinalis ethanol extraction it be unclear that the castering action of flue gas, and the impact of mouthfeel on cigarette of these middle polarity extracts and rudimentary property extract, flue gas, strength still needs that we do further research.
summary of the invention
The technical problem solving: conventional extracting method not to Rosmarinus officinalis extract extract by different level rear composite usage in tobacco, and it is lower to extract the rosemary extract extraction yield obtaining, be applied in the middle of tobacco, mouthfeel, flue gas concentration and quality to tobacco, the lifting of strength are less, can not improve preferably the quality of tobacco.
Technical scheme: the invention discloses the preparation method of the composite extract of a kind of Rosmarinus officinalis, preparation method comprises the following steps: (1) gets fresh Rosmarinus officinalis base of leaf, carries out freezing under low temperature environment; (2) from refrigeration chamber, take out Rosmarinus officinalis base of leaf, by Rosmarinus officinalis base of leaf vacuum lyophilization; (3) Rosmarinus officinalis base of leaf is taken out from freeze drier, pulverize Rosmarinus officinalis base of leaf, be placed in dry environment; (4) get Rosmarinus officinalis base of leaf powder, Rosmarinus officinalis base of leaf powder is stirred to extraction with ethanol; (5) extracting solution is carried out after extracting centrifugally, collect after supernatant concentration and obtain Rosmarinus officinalis ethanol extraction; (6) the Rosmarinus officinalis precipitation after centrifugal is carried out to supercritical carbon dioxide extraction; (7) collect the rosemary extract in flash trapping stage still and the second-order separation still; (8) ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:3:1~1:4:1, composite after mixing is the composite extract of Rosmarinus officinalis.
A preparation method for the composite extract of Rosmarinus officinalis, preparation method comprises the following steps: (1) gets fresh Rosmarinus officinalis base of leaf, and Rosmarinus officinalis base of leaf is launched, and is under the environment of-6~-9 DEG C, to carry out freezingly in temperature, and freezing time is 6h~10h; (2) from refrigeration chamber, take out Rosmarinus officinalis base of leaf, by Rosmarinus officinalis base of leaf vacuum lyophilization, the pressure of vacuum lyophilization is 11Pa~17Pa, and sublimation drying is 5h~7h; (3) Rosmarinus officinalis base of leaf is taken out from freeze drier, pulverize Rosmarinus officinalis base of leaf, being crushed to base of leaf powder is 200~300 orders, is placed in dry environment; (4) get Rosmarinus officinalis base of leaf powder, Rosmarinus officinalis base of leaf powder is stirred to extraction with ethanol, solid-liquid ratio is 1:6~1:10, and extracting temperature is 40 DEG C~50 DEG C, and extraction time is 2h~4h; (5) extracting solution is carried out after extracting centrifugally, collect after supernatant concentration and obtain Rosmarinus officinalis ethanol extraction; (6) the Rosmarinus officinalis precipitation after centrifugal is carried out to supercritical carbon dioxide extraction, supercritical extraction pressure is 21MPa~27MPa, and extraction temperature is 50 DEG C~60 DEG C, and flash trapping stage pressure is 8.5~9MPa, and the second-order separation pressure is 6.5MPa, and extraction time is 4h; (7) collect the rosemary extract in flash trapping stage still and the second-order separation still; (8) ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:3:1~1:4:1, composite after mixing is the composite extract of Rosmarinus officinalis.
Wherein, described supercritical extraction pressure is preferably 25MPa.By supercritical extraction pressure is preferably to 25MPa, the flash trapping stage extract that supercritical extraction obtains and the second-order separation extract extraction yield have all obtained effective raising.
Wherein, flash trapping stage pressure is preferably 9MPa.Flash trapping stage pressure is preferably 9MPa, and after the flash trapping stage extract obtaining and ethanol extraction and the second-order separation extract are composite, its improvement and castering action to tobacco is the most obvious.
Wherein, during with extraction using alcohol, solid-liquid ratio is preferably 1:10.Solid-liquid ratio is preferably 1:10, effectively raises Rosmarinus officinalis extraction using alcohol rate.
Wherein, ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:4:1, composite after mixing is the composite extract of Rosmarinus officinalis.Under this mass ratio, the castering action maximum of the rosemary extract obtaining in tobacco.
Beneficial effect: in preparation method of the present invention, Rosmarinus officinalis extraction using alcohol rate has been up to 21.5%, in supercritical extraction process, flash trapping stage extraction yield is up to 6.9%, and secondary extraction yield has been up to 4.6%, the extraction yield of preparing higher than conventional wet distillation or additive method greatly.In addition, Rosmarinus officinalis ethanol extraction and supercritical extract are carried out composite, the compound obtaining according to the mass ratio of 1:4:1 has improved mouthfeel, flue gas concentration and quality, the strength etc. of cigarette very significantly.
Embodiment
Embodiment 1
(1) getting fresh Rosmarinus officinalis base of leaf 2kg, Rosmarinus officinalis base of leaf is launched, is under the environment of-9 DEG C, to carry out freezingly in temperature, and freezing time is 10h; (2) from refrigeration chamber, take out Rosmarinus officinalis base of leaf, by Rosmarinus officinalis base of leaf vacuum lyophilization, the pressure of vacuum lyophilization is 17Pa, and sublimation drying is 5h; (3) Rosmarinus officinalis base of leaf is taken out from freeze drier, pulverize Rosmarinus officinalis base of leaf, being crushed to base of leaf powder is 300 orders, is placed in dry environment; (4) get Rosmarinus officinalis base of leaf powder, Rosmarinus officinalis base of leaf powder is stirred to extraction with ethanol, solid-liquid ratio is 1:8, and extracting temperature is 50 DEG C, and extraction time is 2h; (5) extracting solution is carried out after extracting centrifugally, collect after supernatant concentration and obtain Rosmarinus officinalis ethanol extraction; (6) the Rosmarinus officinalis precipitation after centrifugal is carried out to supercritical carbon dioxide extraction, supercritical extraction pressure is 21MPa, and extraction temperature is 60 DEG C, and flash trapping stage pressure is 8.5MPa, and the second-order separation pressure is 6.5MPa, and extraction time is 4h; (7) collect the rosemary extract in flash trapping stage still and the second-order separation still; (8) ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:3:1, composite after mixing is the composite extract of Rosmarinus officinalis.
Embodiment 2
(1) getting fresh Rosmarinus officinalis base of leaf 1kg, Rosmarinus officinalis base of leaf is launched, is under the environment of-6 DEG C, to carry out freezingly in temperature, and freezing time is 6h; (2) from refrigeration chamber, take out Rosmarinus officinalis base of leaf, by Rosmarinus officinalis base of leaf vacuum lyophilization, the pressure of vacuum lyophilization is 14Pa, and sublimation drying is 7h; (3) Rosmarinus officinalis base of leaf is taken out from freeze drier, pulverize Rosmarinus officinalis base of leaf, being crushed to base of leaf powder is 200 orders, is placed in dry environment; (4) get Rosmarinus officinalis base of leaf powder, Rosmarinus officinalis base of leaf powder is stirred to extraction with ethanol, solid-liquid ratio is 1:6, and extracting temperature is 40 DEG C, and extraction time is 4h; (5) extracting solution is carried out after extracting centrifugally, collect after supernatant concentration and obtain Rosmarinus officinalis ethanol extraction; (6) the Rosmarinus officinalis precipitation after centrifugal is carried out to supercritical carbon dioxide extraction, supercritical extraction pressure is 25MPa, and extraction temperature is 50 DEG C, and flash trapping stage pressure is 9MPa, and the second-order separation pressure is 6.5MPa, and extraction time is 4h; (7) collect the rosemary extract in flash trapping stage still and the second-order separation still; (8) ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:4:1, composite after mixing is the composite extract of Rosmarinus officinalis.
Embodiment 3
(1) getting fresh Rosmarinus officinalis base of leaf 3kg, Rosmarinus officinalis base of leaf is launched, is under the environment of-8 DEG C, to carry out freezingly in temperature, and freezing time is 8h; (2) from refrigeration chamber, take out Rosmarinus officinalis base of leaf, by Rosmarinus officinalis base of leaf vacuum lyophilization, the pressure of vacuum lyophilization is 11Pa, and sublimation drying is 6h; (3) Rosmarinus officinalis base of leaf is taken out from freeze drier, pulverize Rosmarinus officinalis base of leaf, being crushed to base of leaf powder is 250 orders, is placed in dry environment; (4) get Rosmarinus officinalis base of leaf powder, Rosmarinus officinalis base of leaf powder is stirred to extraction with ethanol, solid-liquid ratio is 1:10, and extracting temperature is 45 DEG C, and extraction time is 3h; (5) extracting solution is carried out after extracting centrifugally, collect after supernatant concentration and obtain Rosmarinus officinalis ethanol extraction; (6) the Rosmarinus officinalis precipitation after centrifugal is carried out to supercritical carbon dioxide extraction, supercritical extraction pressure is 27MPa, and extraction temperature is 55 DEG C, and flash trapping stage pressure is 8.5MPa, and the second-order separation pressure is 6.5MPa, and extraction time is 4h; (7) collect the rosemary extract in flash trapping stage still and the second-order separation still; (8) ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:3:1, composite after mixing is the composite extract of Rosmarinus officinalis.
The extraction using alcohol rate of embodiment 1, embodiment 2, embodiment 3, one-level extraction yield, secondary extraction yield result are as follows.
Extraction using alcohol rate: ethanol enriched material quality/Rosmarinus officinalis total mass × 100%
One-level extraction yield: one-level extract quality/Rosmarinus officinalis total mass × 100%
Secondary extraction yield: secondary extract quality/Rosmarinus officinalis total mass × 100%
Embodiment 1 Embodiment 2 Embodiment 3
Extraction using alcohol rate 11.8% 15.6% 21.5%
One-level extraction yield 4.6% 6.9% 6.7%
Secondary extraction yield 1.4% 4.6% 4.2%
The solid-liquid ratio of embodiment 3 is 1:10 as can be seen from the table, and the extraction using alcohol amount that it prepares is also the highest.In addition, the supercritical extraction pressure in embodiment 2 is preferably 25MPa, and one-level extraction yield and secondary extraction yield, all higher than the 27MPa of embodiment 3, are different from the larger phenomenon of the larger extraction yield of pressure in conventional supercritical extraction.
By composite the Rosmarinus officinalis of embodiment 1, embodiment 2, embodiment 3 extract acetic acid ethyl dissolution, the composite extract concentrations of Rosmarinus officinalis is 1wt%, is evenly sprayed on pipe tobacco, and sprinkling amount is the 0.5wt% of pipe tobacco weight, makes cigarette and smoke panel test after balance.Reference examples is to have added the cigarette of the rosemary ethereal oil that wet distillation method obtains, and the concentration of rosemary ethereal oil is also 1wt%, and sprinkling amount is also the 0.5wt% of pipe tobacco weight, and comprehensive sensory quality assessment result is as follows:
Embodiment 1: flue gas is full, fragrance is full, mouthfeel is moderate, pleasant impression is better, Titian effect is comparatively obvious.
Embodiment 2: flue gas is strong, fragrance is full, coordination and elegant, delicate mouthfeel is soft and smooth, pleasant impression is comfortable, Titian effect is very obvious.
Embodiment 3: aromatic strongly fragrant, the fragrance of cigarette is coordinated, mouthfeel is moderate, Titian effect is comparatively obvious.
Reference examples: flue gas slightly increases, fragrance slightly promotes, mouthfeel is general, pleasant impression is poor, Titian effect is not outstanding.

Claims (6)

1. a preparation method for the composite extract of Rosmarinus officinalis, is characterized in that preparation method comprises the following steps: (1) gets fresh Rosmarinus officinalis base of leaf, carries out freezing under low temperature environment; (2) from refrigeration chamber, take out Rosmarinus officinalis base of leaf, by Rosmarinus officinalis base of leaf vacuum lyophilization; (3) Rosmarinus officinalis base of leaf is taken out from freeze drier, pulverize Rosmarinus officinalis base of leaf, be placed in dry environment; (4) get Rosmarinus officinalis base of leaf powder, Rosmarinus officinalis base of leaf powder is stirred to extraction with ethanol; (5) extracting solution is carried out after extracting centrifugally, collect after supernatant concentration and obtain Rosmarinus officinalis ethanol extraction; (6) the Rosmarinus officinalis precipitation after centrifugal is carried out to supercritical carbon dioxide extraction; (7) collect the rosemary extract in flash trapping stage still and the second-order separation still; (8) ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:3:1~1:4:1, composite after mixing is the composite extract of Rosmarinus officinalis.
2. the preparation method of the composite extract of a kind of Rosmarinus officinalis according to claim 1, it is characterized in that preparation method comprises the following steps: (1) gets fresh Rosmarinus officinalis base of leaf, Rosmarinus officinalis base of leaf is launched, and is under the environment of-6~-9 DEG C, to carry out freezingly in temperature, and freezing time is 6h~10h; (2) from refrigeration chamber, take out Rosmarinus officinalis base of leaf, by Rosmarinus officinalis base of leaf vacuum lyophilization, the pressure of vacuum lyophilization is 11Pa~17Pa, and sublimation drying is 5h~7h; (3) Rosmarinus officinalis base of leaf is taken out from freeze drier, pulverize Rosmarinus officinalis base of leaf, being crushed to base of leaf powder is 200~300 orders, is placed in dry environment; (4) get Rosmarinus officinalis base of leaf powder, Rosmarinus officinalis base of leaf powder is stirred to extraction with ethanol, solid-liquid ratio is 1:6~1:10, and extracting temperature is 40 DEG C~50 DEG C, and extraction time is 2h~4h; (5) extracting solution is carried out after extracting centrifugally, collect after supernatant concentration and obtain Rosmarinus officinalis ethanol extraction; (6) the Rosmarinus officinalis precipitation after centrifugal is carried out to supercritical carbon dioxide extraction, supercritical extraction pressure is 21MPa~27MPa, and extraction temperature is 50 DEG C~60 DEG C, and flash trapping stage pressure is 8.5~9MPa, and the second-order separation pressure is 6.5MPa, and extraction time is 4h; (7) collect the rosemary extract in flash trapping stage still and the second-order separation still; (8) ethanol extraction, flash trapping stage extract, the second-order separation extract are mixed according to the mass ratio of 1:3:1~1:4:1, composite after mixing is the composite extract of Rosmarinus officinalis.
3. the preparation method of the composite extract of a kind of Rosmarinus officinalis according to claim 1, is characterized in that described supercritical extraction pressure is 25MPa.
4. the preparation method of the composite extract of a kind of Rosmarinus officinalis according to claim 1, is characterized in that flash trapping stage pressure is 9MPa.
5. the preparation method of the composite extract of a kind of Rosmarinus officinalis according to claim 1, while it is characterized in that with extraction using alcohol, solid-liquid ratio is 1:10.
6. the preparation method of the composite extract of a kind of Rosmarinus officinalis according to claim 1, it is characterized in that ethanol extraction, flash trapping stage extract, the second-order separation extract to mix according to the mass ratio of 1:4:1, composite after mixing is the composite extract of Rosmarinus officinalis.
CN201410204635.3A 2014-05-15 2014-05-15 A kind of preparation method of the composite extract of Herba Rosmarini Officinalis Expired - Fee Related CN103966027B (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104164455A (en) * 2014-08-19 2014-11-26 云南中烟工业有限责任公司 Rosmarinus officinalis L. fermentation broth extract as well as preparation method and application thereof
CN104397362A (en) * 2014-12-15 2015-03-11 昆山市畜牧兽医站 Preparation technology for rosemary powder and application of rosemary powder to laying hen feed
CN105686067A (en) * 2016-03-11 2016-06-22 李贵生 Rosemary type cigarette
CN108753461A (en) * 2018-06-05 2018-11-06 佛山皖阳生物科技有限公司 A kind of preparation method of biology peptide composite antioxidant
CN109022152A (en) * 2018-08-30 2018-12-18 湖北中烟工业有限责任公司 A kind of rosemary tobacco aromaticss and its preparation method and application
CN115486530A (en) * 2022-10-21 2022-12-20 湖南祥民制药有限公司 Rosemary freeze-drying method
CN116019219A (en) * 2022-12-30 2023-04-28 东莞市吉纯生物技术有限公司 A buccal product containing herba Rosmarini officinalis extract and its preparation method

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JPH03293001A (en) * 1990-04-11 1991-12-24 Chisso Corp Method for deodorizing antioxidant component extracted from natural resouce
CN1316494A (en) * 2000-04-06 2001-10-10 张高 Process for extracting antioxidizing agent and perfume from rosemary
CN1781545A (en) * 2001-02-09 2006-06-07 新纪元公司 Method for extracting herbal medicine
CN102199092A (en) * 2010-03-26 2011-09-28 禹州市森源本草天然产物有限公司 Production technology for acquiring two antioxidant agents from Rosmarinus officinalis L.

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03293001A (en) * 1990-04-11 1991-12-24 Chisso Corp Method for deodorizing antioxidant component extracted from natural resouce
CN1316494A (en) * 2000-04-06 2001-10-10 张高 Process for extracting antioxidizing agent and perfume from rosemary
CN1781545A (en) * 2001-02-09 2006-06-07 新纪元公司 Method for extracting herbal medicine
CN102199092A (en) * 2010-03-26 2011-09-28 禹州市森源本草天然产物有限公司 Production technology for acquiring two antioxidant agents from Rosmarinus officinalis L.

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104164455A (en) * 2014-08-19 2014-11-26 云南中烟工业有限责任公司 Rosmarinus officinalis L. fermentation broth extract as well as preparation method and application thereof
CN104397362A (en) * 2014-12-15 2015-03-11 昆山市畜牧兽医站 Preparation technology for rosemary powder and application of rosemary powder to laying hen feed
CN105686067A (en) * 2016-03-11 2016-06-22 李贵生 Rosemary type cigarette
CN108753461A (en) * 2018-06-05 2018-11-06 佛山皖阳生物科技有限公司 A kind of preparation method of biology peptide composite antioxidant
CN109022152A (en) * 2018-08-30 2018-12-18 湖北中烟工业有限责任公司 A kind of rosemary tobacco aromaticss and its preparation method and application
CN115486530A (en) * 2022-10-21 2022-12-20 湖南祥民制药有限公司 Rosemary freeze-drying method
CN115486530B (en) * 2022-10-21 2024-03-26 湖南祥民制药有限公司 Freeze-drying method of rosemary
CN116019219A (en) * 2022-12-30 2023-04-28 东莞市吉纯生物技术有限公司 A buccal product containing herba Rosmarini officinalis extract and its preparation method

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