CN107474958B - Method for preparing saffron crocus extract by using pervaporation membrane - Google Patents

Method for preparing saffron crocus extract by using pervaporation membrane Download PDF

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CN107474958B
CN107474958B CN201710700321.6A CN201710700321A CN107474958B CN 107474958 B CN107474958 B CN 107474958B CN 201710700321 A CN201710700321 A CN 201710700321A CN 107474958 B CN107474958 B CN 107474958B
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saffron
extract
cigarettes
aroma
saffron extract
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CN107474958A (en
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庞登红
尹团章
陈�胜
谭烨
王珊
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China Tobacco Hubei Industrial LLC
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/0003Compounds of unspecified constitution defined by the chemical reaction for their preparation
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24BMANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
    • A24B3/00Preparing tobacco in the factory
    • A24B3/12Steaming, curing, or flavouring tobacco
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/36Pervaporation; Membrane distillation; Liquid permeation
    • B01D61/362Pervaporation

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Seasonings (AREA)
  • Fats And Perfumes (AREA)

Abstract

The invention provides a method for preparing saffron crocus extract by using a pervaporation membrane. The preparation method specifically comprises the following steps: (1) extracting dry flos croci under reflux to obtain extractive solution; (2) concentrating stigma croci Sativi extractive solution; (3) enriching the aroma substances in the concentrated waste liquid by using a pervaporation membrane; (4) and reversely supplementing the enriched aroma substances into the concentrated solution to obtain the saffron extract for cigarettes. The prepared saffron extract for cigarettes retains the characteristic aroma of saffron, has pure aroma, has the effects of increasing cigarette aroma, improving smoke quality, endowing cigarettes with fresh and sweet aroma, reducing stimulation, covering offensive odor, softening and smoothing smoke, improving oral comfort, increasing the sweet feeling of cigarettes and the like when being added into the cigarettes, and improves the adaptability of the saffron extract in the cigarettes.

Description

Method for preparing saffron crocus extract by using pervaporation membrane
Technical Field
The invention relates to a preparation method of essence and flavor for cigarettes, in particular to a method for reversely supplementing aroma substances by a pervaporation membrane and preparing a saffron extract for cigarettes.
Background
In modern cigarette production, flavoring is regarded as a non-negligible technology, and cigarette products are rich in characteristics due to the selection of various spices, and bring unique fragrance and satisfaction to consumers during smoking. The natural perfume is widely used in cigarettes due to the characteristics of rich aroma, unique aroma characteristics, pure and mild aroma quality and the like, at present, the natural perfume for cigarettes is mostly extracted by adopting a solvent, and the greatest defect of the process is that the aroma loss is large in the concentration process, so that the current situation that aroma substances are lost due to concentration in the solvent extraction process is changed, and the process becomes a hotspot of research.
Pervaporation (Pervaporation) is an emerging membrane separation technology, which realizes mass transfer by using the chemical potential difference of certain components at the upstream and downstream of a feed liquid membrane as a driving force, and realizes selection by using the difference of affinity and mass transfer resistance of the membrane to different components in the feed liquid. The pervaporation process has the advantages of high energy utilization efficiency, high selectivity, compact device, simple and convenient operation and control, flexible and variable scale and the like. Therefore, the method is applied to the separation of near-boiling and constant-boiling mixtures which are difficult to separate or cannot be separated by common rectification, the removal of trace water in organic solvents and mixed solvents, the recovery of a small amount of organic matters in waste water, the separation and reaction coupling of organic matters/organic matters, the continuous removal of reaction products and the like, and has obvious economic and technical advantages. However, the preparation of the saffron extract for cigarettes is not reported.
Saffron (the scientific name is Polianthes tuberosa), also called evening primrose and evening primrose, and plants of crocus of Amaryllidaceae are distributed in Mexico, south America and other areas. The saffron contains aromatic substances such as saffron aldehyde, furfural, dihydro-beta-ionone, isophorone, dihydroactinidiolide and the like, and the aromatic substances have good effect on the aroma of cigarettes.
The concentrated waste liquor of saffron crocus is treated by utilizing the pervaporation membrane technology, the aroma substances are collected and are reversely supplemented into the saffron crocus extract, and the saffron crocus extract which has pure aroma, obvious characteristic aroma and better application effect in cigarettes can be obtained.
Disclosure of Invention
The invention aims to provide a method for reversely supplementing aroma substances by a pervaporation membrane and preparing a saffron extract for cigarettes.
The invention provides a method for preparing a saffron extract for cigarettes by using a pervaporation membrane, which is characterized by comprising the following steps of:
(1) taking dry saffron crocus, adding water with the weight being 10-20 times of that of the dry saffron crocus, performing reflux extraction, standing and cooling an extracting solution, and collecting filtrate to obtain a saffron extracting solution;
(2) concentrating stigma croci Sativi extractive solution at 60-80 deg.C under reduced pressure to relative density of 1.20-1.30 to obtain stigma croci Sativi extract A; collecting the waste liquid after the saffron crocus extract is concentrated;
(3) selecting a POMS-PEI composite membrane (a poly octyl methyl siloxane-polyetherimide composite membrane) as a pervaporation membrane, carrying out vaporization and permeation treatment on the waste liquid obtained after the concentration of the saffron extract in the step (2) under the conditions that the heating temperature is 50-80 ℃, the feeding speed is 10-100ml/min, liquid nitrogen is used for cooling, and the fragrance substance collecting pressure is 20-100Pa, and collecting fragrance substances;
(4) and (3) reversely supplementing the aroma substances subjected to vaporization and permeation into the saffron extract A concentrated in the step (2), stirring, and uniformly mixing to obtain the saffron extract for cigarettes.
And (2) carrying out reflux extraction on the dry saffron flowers in the step (1) at 100 ℃ for 3-5 h.
The invention utilizes the vaporization osmotic membrane technology to reversely supplement aroma substances to prepare the saffron extract, utilizes the pervaporation membrane technology to collect aromatic substances such as saffron aldehyde, dihydro-beta-ionone, isophorone and the like in the saffron concentrated waste liquid, and reversely supplements the aromatic substances into the saffron extract to prepare the special saffron extract for cigarettes. The POMS-PEI membrane adopted by the invention is an existing composite membrane, and the composite membrane adopted by the invention is a product purchased from GKSS company of Germany; the POMS-PEI membrane is used for enriching saffron aroma substances, and the recovery amount of the aroma substances is obviously higher than that of EVA38, POMS, PDMS and PEI.
Compared with the traditional saffron extract, the relative contents of 13 aroma substances such as furfural, isophorone, crocinal, 2,4, 4-trimethyl-3-formaldehyde-5-hydroxy-2, 5-cyclohexadiene-1-one and the like of the saffron extract prepared by the method are increased. The additive is added into cigarettes, has the effects of increasing cigarette aroma amount, improving smoke quality, endowing the cigarettes with fresh and sweet aroma, reducing stimulation, covering offensive odor, softening and smoothing smoke, improving oral comfort, increasing cigarette sweet feeling and the like, and has an overall evaluation effect obviously superior to that of the traditional saffron extract.
The characteristic saffron extract with high characteristic aroma substance content, pure aroma and good cigarette application effect is prepared by the method, and the extract has characteristic flower aroma and pure aroma. The saffron extract is added into cigarettes, so that the cigarette fragrance amount is increased, the smoke quality is improved, the cigarettes are endowed with fresh and sweet fragrance, the stimulation is reduced, the offensive odor is covered, the smoke is softened and refined, the oral comfort level is improved, the cigarette sweet feeling is increased, and the adaptability of the saffron extract in the cigarettes is improved. The invention changes waste into valuable, improves the quality of the saffron extract and improves the adaptability of the saffron extract in cigarettes.
Detailed Description
The technical problems associated with the present invention will be described in further detail with reference to examples.
Embodiment 1, a method for preparing saffron extract for cigarette by pervaporation membrane, which is characterized by comprising the following steps:
(1) taking dry saffron crocus, adding 10 times of water, reflux-extracting at 100 deg.C for 3-5 hr, standing, cooling, and collecting filtrate to obtain saffron extract;
(2) concentrating the stigma croci Sativi extractive solution collected in step (1) at 60 deg.C under reduced pressure to relative density of 1.20 to obtain stigma croci Sativi extract A, and collecting the concentrated waste liquid;
(3) and (3) selecting a POMS-PEI pervaporation membrane, carrying out vaporization and permeation treatment on the concentrated waste liquid of the saffron extract collected in the step (2) under the conditions of heating temperature of 50 ℃, feeding speed of 10ml/min, liquid nitrogen cooling and fragrance substance collecting pressure of 20Pa, and collecting fragrance substances.
(4) And (3) reversely supplementing the aroma substances vaporized and permeated in the step (3) into the saffron extract A concentrated in the step (2), stirring and uniformly mixing to obtain the saffron extract for cigarettes.
Embodiment 2, a method for preparing saffron extract for cigarette by pervaporation membrane, which is characterized by comprising the following steps:
(1) taking dry saffron flowers, adding 15 times of water, reflux-extracting at 100 deg.C for 3-5 hr, standing, cooling, and collecting filtrate to obtain saffron extract;
(2) concentrating the stigma croci Sativi extractive solution collected in step (1) at 70 deg.C under reduced pressure to relative density of 1.25 to obtain stigma croci Sativi extract A, and collecting the concentrated waste liquid;
(3) selecting a POMS-PEI pervaporation membrane, carrying out vaporization and permeation treatment on the concentrated waste liquid of the saffron extract collected in the step (2) under the conditions of heating temperature of 65 ℃, feeding speed of 50ml/min, liquid nitrogen cooling and fragrance substance collecting pressure of 60Pa, and collecting fragrance substances;
(4) and (3) reversely supplementing the aroma substances after vaporization and permeation collected in the step (3) into the saffron extract A concentrated in the step (2), stirring and uniformly mixing to obtain the saffron extract for cigarettes.
Embodiment 3, a method for preparing saffron extract for cigarette by pervaporation membrane, which is characterized by comprising the following steps:
(1) taking dry saffron flowers, adding water with the weight 20 times of the dry saffron flowers, performing reflux extraction at 100 ℃ for 3-5 hours, standing and cooling an extracting solution, and collecting filtrate to obtain a saffron extracting solution;
(2) concentrating the stigma croci Sativi extractive solution collected in step (1) at 70 deg.C under reduced pressure to relative density of 1.20 to obtain stigma croci Sativi extract A, and collecting the concentrated waste liquid;
(3) selecting a POMS-PEI pervaporation membrane, carrying out vaporization and permeation treatment on the concentrated waste liquid of the saffron extract collected in the step (2) under the conditions of heating temperature of 70 ℃, feeding speed of 50ml/min, liquid nitrogen cooling and fragrance substance collecting pressure of 100Pa, and collecting fragrance substances;
(4) and (3) reversely supplementing the aroma substances collected in the step (3) after vaporization and permeation into the saffron extract A concentrated in the step (2), stirring and uniformly mixing to obtain the saffron extract for cigarettes.
Embodiment 4, a method for preparing saffron extract for cigarette by pervaporation membrane, which is characterized by comprising the following steps:
(1) taking dry saffron flowers, adding water with the weight 20 times of the dry saffron flowers, performing reflux extraction at 100 ℃ for 3-5 hours, standing and cooling an extracting solution, and collecting filtrate to obtain a saffron extracting solution;
(2) concentrating the stigma croci Sativi extractive solution collected in step (1) at 80 deg.C under reduced pressure to relative density of 1.30 to obtain stigma croci Sativi extract A, and collecting the concentrated waste liquid;
(3) and (3) selecting a POMS-PEI pervaporation membrane, carrying out vaporization and permeation treatment on the concentrated waste liquid of the saffron extract collected in the step (2) under the conditions of heating temperature of 80 ℃, feeding speed of 100ml/min, liquid nitrogen cooling and fragrance substance collecting pressure of 100Pa, and collecting fragrance substances.
(4) And (3) reversely supplementing the aroma substances after vaporization and permeation collected in the step (3) into the saffron extract A concentrated in the step (2), stirring and uniformly mixing to obtain the saffron extract for cigarettes.
Test one: the inventor adopts different pervaporation membranes to carry out vaporization and permeation treatment on the waste liquid after the saffron extract is concentrated, analyzes the influence of different pervaporation membranes on the recovery amount of the fragrance substances of the saffron extract, and finds the specific experimental results in table 1:
TABLE 1 Effect of different membranes on saffron extract aroma recovery
Kind of membrane Recovery (‰)
EVA38 0.26
POMS Is not separated out
PDMS 0.45
PEI 0.32
POMS-PEI 0.85
As can be seen from the comparative data in table 1, compared with EVA38, POMS, PDMS, and PEI, the POMS-PEI composite film used in the present invention has the highest recovery amount of saffron extract aroma.
And (2) test II: the prepared saffron extract prepared by the method in the application is analyzed and compared with the fragrance components of the saffron extract prepared by the traditional solvent method, and the specific results are shown in table 2:
TABLE 2 comparison of the relative contents of characteristic aroma components of saffron crocus extract extracted by conventional solvent and the method of the present application
Figure BDA0001380193500000061
Figure BDA0001380193500000071
As can be seen from table 2, compared with the conventional solvent extraction, the saffron extract prepared in the present application has increased relative contents of 13 saffron characteristic aroma substances such as furfural, isophorone, crocetin, 2,4, 4-trimethyl-3-formaldehyde-5-hydroxy-2, 5-cyclohexadiene-1-one, and the like.
And (3) test III: comparing the odor of the saffron extract prepared by the application with the odor of the saffron extract prepared by the conventional steam distillation method, wherein the comparison result is shown in the following table 3:
table 3 traditional solvent extraction and comparison of the odor of saffron extract prepared herein
Treatment method Steam distillation This application
Smelling incense Sweet and paste incense Has characteristic flower fragrance and pure fragrance
And (4) testing: the saffron extract prepared by the method in the application and the saffron extract prepared by the conventional steam distillation method are respectively added into blank cut tobacco according to 0.1 percent of the weight of the cut tobacco, and the rolled cigarettes are respectively subjected to smoking evaluation by a smoking evaluation group, wherein the specific sensory evaluation effect is shown in the table 4:
table 4 comparison of the sensory evaluation results of conventional solvent extraction and the herein prepared saffron extract added to cigarettes
Figure BDA0001380193500000081
It can be seen through the comparison of smelling of traditional solvent extraction saffron extract and the saffron extract prepared in this application and sense organ evaluation effect (table 3 and table 4), the saffron extract fragrance that utilizes the method preparation in this application is purer, the characteristic fragrant is more obvious, add in the cigarette, have the volume of increasing fragrance, improve smoke quality, give cigarette fresh and sweet fragrant, reduce the stimulation, cover miscellaneous gas, soft flue gas is fine and smooth, oral cavity comfort level becomes good, has effects such as the sense of returning sweet, the effect is obviously superior to the saffron extract of traditional solvent extraction preparation.
The above description is only a detailed description of specific embodiments of the present invention, and should not be taken as limiting the invention, and any modifications, equivalents, improvements, etc. made on the design concept of the present invention should be included in the protection scope of the present invention.

Claims (1)

1. A method for preparing a saffron extract for cigarettes by using a pervaporation membrane is characterized by comprising the following steps of:
(1) taking dry saffron crocus, adding water with the weight being 10-20 times of that of the dry saffron crocus, performing reflux extraction at 100 ℃ for 3-5 hours, standing and cooling an extracting solution, and collecting filtrate to obtain a saffron extracting solution;
(2) concentrating stigma croci Sativi extractive solution at 60-80 deg.C under reduced pressure to relative density of 1.20-1.30 to obtain stigma croci Sativi extract A; collecting the waste liquid after the saffron crocus extract is concentrated;
(3) selecting a POMS-PEI composite membrane as a pervaporation membrane, carrying out vaporization and permeation treatment on the concentrated waste liquid of the saffron extract obtained in the step (2) under the conditions that the heating temperature is 50-65 ℃, the feeding speed is 10-50ml/min, liquid nitrogen is used for cooling, and the fragrance substance collecting pressure is 20-100Pa, and collecting fragrance substances;
(4) and (3) reversely supplementing the aroma substances subjected to vaporization and permeation into the saffron extract A concentrated in the step (2), stirring, and uniformly mixing to obtain the saffron extract for cigarettes.
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CN110804497A (en) * 2019-11-18 2020-02-18 湖北中烟工业有限责任公司 Preparation method of saffron extract for tobacco bead blasting

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CN101301112A (en) * 2008-04-30 2008-11-12 广西中烟工业公司 Additive agent for flavoring natural tobacco and preparation method and use thereof
CN101619271A (en) * 2009-07-02 2010-01-06 华顺香料(上海)有限公司 Traditional Chinese medicine combination spice for cigarette as well as preparation method and application thereof
CN103385338A (en) * 2013-06-09 2013-11-13 南京工业大学 Method for recovering aroma components in production process of instant tea powder

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CN106148013A (en) * 2016-08-31 2016-11-23 陈爱梅 A kind of plant perfume low-temperature extraction technology
CN106957880A (en) * 2016-10-13 2017-07-18 湖北中烟工业有限责任公司 A kind of immobilization beta glucuroide prepares method of the cigarette with safranine flower extract

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101301112A (en) * 2008-04-30 2008-11-12 广西中烟工业公司 Additive agent for flavoring natural tobacco and preparation method and use thereof
CN101619271A (en) * 2009-07-02 2010-01-06 华顺香料(上海)有限公司 Traditional Chinese medicine combination spice for cigarette as well as preparation method and application thereof
CN103385338A (en) * 2013-06-09 2013-11-13 南京工业大学 Method for recovering aroma components in production process of instant tea powder

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