CN111004679A - Lysimachia capillipes extract and essence - Google Patents
Lysimachia capillipes extract and essence Download PDFInfo
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- CN111004679A CN111004679A CN201911166572.6A CN201911166572A CN111004679A CN 111004679 A CN111004679 A CN 111004679A CN 201911166572 A CN201911166572 A CN 201911166572A CN 111004679 A CN111004679 A CN 111004679A
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Abstract
The invention relates to a method for preparing a lysimachia capillipes extract, comprising the following steps: (1) applying water (2) to the lysimachia capillipes hemsl raw material to carry out steam distillation on the product obtained in the step (1), and collecting steam condensate to obtain lysimachia capillipes hemsl hydrosol; (3.10) performing reverse osmosis concentration on the hydrolat obtained in the step (2) by using a reverse osmosis membrane, and collecting trapped fluid to obtain a first extract; (3.20) continuing steam distillation on the product of the step 2 to collect residues after distillation; (3.21) adding a polar solvent into the residue obtained in the step 3.20 for extraction, and filtering after extraction to obtain a filtrate; (3.22) centrifuging the filtrate obtained in the step 3.21 to obtain a centrifugal clear liquid; (3.23) concentrating the centrifuged supernatant of step 3.22 by vacuum evaporation to obtain a second extract. The herba Lysimachiae Foenumgraeci extract obtained by the above method can effectively improve the sensory quality of tobacco products.
Description
Technical Field
The invention belongs to the field of tobacco, and particularly relates to a lysimachia capillipes extract and essence.
Background
Lysimachia capillipes Hemsl, also known as Manyleaf rhododendron leaf, Phyllanthus pubescens and Lysimachia foenum-graecum, is a plant of the genus Pelargonium of the family Primulaceae and widely distributed in Guizhou, Jiangxi, Fujian and other areas of China.
Disclosure of Invention
The existing plant extract extraction method is usually an effective extract produced by a batch of raw materials, and the residual residue is treated as waste, so that the method has high cost and is not beneficial to environmental protection.
The present disclosure creatively proposes an integrated lysimachia capillipes extraction process that extracts two different styles from a batch of lysimachia capillipes raw materials, each of the two different styles having significant characteristics, that can be used to improve the sensory quality of tobacco products. Moreover, it was unexpected that the two extracts of different styles could also be used in combination to further improve the organoleptic qualities of the tobacco product.
In some aspects, there is provided a method of preparing a lysimachia capillipes extract, comprising the steps of:
(1) applying water to the lysimachia capillipes hemsl raw material, wherein the weight of the water is 5-20% (for example, 10-15%) of the principle weight of the lysimachia capillipes hemsl;
(2) performing steam distillation on the product obtained in the step (1), wherein the flow rate of a steam condensate per hour is 3-10 times (for example, 4-5 times, 5-6 times, 6-7 times, 7-8 times or 8-9 times) of the weight of the lysimachia capillipes hemsl raw material, the distillation time is 3-4 hours, and collecting the steam condensate, namely the lysimachia capillipes hemsl pure dew;
(3.10) performing reverse osmosis concentration on the hydrolat obtained in the step (2) by using a reverse osmosis membrane, and collecting trapped fluid to obtain a first extract;
(3.20) continuing steam distillation on the product obtained in the step (2) for 1-2 hours, wherein the flow rate of the steam condensate per hour is 3-10 times (for example, 4-5 times, 5-6 times, 6-7 times, 7-8 times or 8-9 times) of the weight of the lysimachia capillipes hemsl raw material, and collecting residues after distillation;
(3.21) adding a polar solvent which is 10-30 times (for example, 15-20 times, 20-25 times) the mass of the residue into the residue obtained in the step 3.20 for extraction at 60-100 ℃ (for example, 70-80 ℃, 80-90 ℃ and 90-100 ℃) for 60-180min (for example, 60-80min, 80-100min, 100-120min, 120-140min, 140-160min and 160-180min), and filtering after extraction to obtain a filtrate;
(3.22) centrifuging the filtrate obtained in the step 3.21 to obtain a centrifugal clear liquid;
(3.23) concentrating the centrifuged supernatant of step 3.22 by vacuum evaporation to obtain a second extract, wherein the relative density of the second extract at 20 ℃ is 1.0-1.3 (e.g., 1.1-1.2).
And (3) the step (3.10) and the step (3.20) are not performed in sequence.
The above method can obtain two kinds of Lysimachia capillipes extracts with completely different styles, namely a first extract and a second extract.
The first extract had a characteristic odour of lysimachia capillipes, i.e. a medicinal herb odour, which was quite pronounced.
The second extract has substantially no characteristic odor of Lysimachia capillipes, i.e., herb odor, but retains the aroma and many active ingredients of Lysimachia capillipes.
It is noteworthy that step 3.20 is particularly important for obtaining a high quality second extract of the present disclosure, and the absence of this step would result in the second extract failing to achieve the beneficial effects of the present disclosure. The residue obtained in step 3.20 has substantially no characteristic odour components of lysimachia capillipes.
In some embodiments, in step 3.10, the reverse osmosis parameters are as follows: the membrane entrance pressure is 1.8-2.2 MPa (such as 1.9-2 MPa, 2-2.1 MPa), the membrane exit pressure is 0.8-1.2 MPa (such as 1.9-2 MPa, 2-2.1 MPa), the temperature is 25-30 ℃, the flux is 70-90 kg/h (such as 75-80, 80-85 kg/h), and the concentration multiple is 70-90 times (such as 80 times).
In some embodiments, the polar solvent in step 3.21 is pure water or an aqueous ethanol solution with a mass fraction of 40% to 95% (e.g., 40% to 50%, 50% to 60%, 60% to 70%, 70% to 80%, or 80% to 90%).
In some embodiments, the above method, wherein step 3.21 is performed repeatedly for 2-5 times.
In some embodiments, in step 3.22, the centrifugation is performed at a speed of 5000 to 16000rpm at a temperature of 10 to 30 ℃ for 10 to 30 min.
In some embodiments, the above methods, wherein the vacuum concentration is performed using a single-effect concentration apparatus or a double-effect concentration apparatus.
In some embodiments, the lysimachia capillipes raw material is dried whole lysimachia capillipes grass.
In some embodiments, step (1) comprises: cutting the sun-dried whole lysimachia capillipes into sections of 10-20cm to obtain lysimachia capillipes raw materials;
in some embodiments, step (1) comprises: applying water to the lysimachia capillipes hemsl raw material, wherein the weight of the water is 8-12% of that of the lysimachia capillipes hemsl raw material.
In some embodiments, step (2) comprises: putting the product obtained in the step (1) into a steam distillation device, introducing steam, controlling the opening of a steam valve to enable the flow of steam condensate to be M, wherein the steam inlet pressure is 0.2-0.4 MPa, and the steam inlet pressure is1Collecting water vapor condensate for 2.5-3.5 hours per hour, namely the lysimachia capillipes hemsl hydrosol; m14-6 m, wherein m is the weight of the lysimachia capillipes hemsl raw material.
In some embodiments, step (3.10) comprises: and (3) performing reverse osmosis on the hydrolat obtained in the step (2) by using a reverse osmosis membrane, wherein the parameters are as follows: the membrane feeding pressure is 1.8-2.2 MPa, the membrane discharging pressure is 0.8-1.2 MPa, the temperature is 25-30 ℃, and the concentration multiple is 70-90 times.
In some embodiments, step (3.20) comprises: the step (A) is2) Continuously distilling the residue for 1.5-2.5 h, and controlling the flow of the water vapor condensate to be M2Per hour, M2Collecting residues after distillation, wherein m is 4-6 m and is the weight of the lysimachia capillipes hemsl raw material;
in some embodiments, step (3.21) comprises: adding 15-25 times by mass of ethanol aqueous solution (with the concentration of 60-80 wt%) into the residue in the previous step, soaking and extracting at the extraction temperature of 75-85 ℃ for 150-200 min for 1-2 times, and collecting filtrate;
in some embodiments, step (3.22) comprises: centrifuging the filtrate obtained in the step (3.21) at the rotation speed of 8000-10000 rpm at the temperature of 10-30 ℃ for 10-60 min to obtain a centrifuged clear solution;
in some embodiments, step (3.23) comprises: and (4) concentrating the centrifugal clear liquid obtained in the step (3.22) by adopting a single-effect concentration unit, wherein the equipment parameters are set as follows: the opening of the steam valve is 80-90%, the steam pressure is-0.006-0.01 Mpa, the steam temperature is 70-80 ℃, and the feeding flow is 0.2-0.3 m3The feed temperature is 25-35 ℃, the circulating temperature is 45-55 ℃, the condenser pressure is-0.006-0.01 Mpa, the condenser temperature is 10-15 ℃, and the evaporation capacity is 0.2-0.25 m3And/h, obtaining a second extract with a relative density of 1-1.2 at 20 ℃.
In some aspects, there is provided a lysimachia capillipes extract, which is the first extract prepared by any one of the methods described above.
In some aspects, there is provided a lysimachia capillipes extract, which is the second extract prepared by any one of the methods described above.
In some aspects, a lysimachia capillipes extract composition is provided that contains the first extract and the second extract.
In some embodiments, the weight ratio of the first extract to the second extract in the lysimachia capillipes extract composition is 1:8 to 12.
In some aspects, there is provided the use of lysimachia capillipes or a lysimachia capillipes extract for the preparation of a tobacco product.
In some embodiments, the first extract is present in the smoking article in an amount of 1/107～1/106。
In some embodiments, the second extract is present in the smoking article in an amount of 1/105～1/104。
In some embodiments, the lysimachia capillipes composition is present in the tobacco product in an amount of 1/106～1/105。
In some embodiments, the tobacco product is a tobacco leaf, a tobacco shred, or an electronic cigarette liquid.
In some embodiments, the lysimachia capillipes extract is any lysimachia capillipes extract (e.g., the first extract or the second extract) described above or any lysimachia capillipes extract composition described above.
In some aspects, a tobacco product is provided that contains lysimachia capillipes or a lysimachia capillipes extract.
In some embodiments, the lysimachia capillipes extract is any one of the lysimachia capillipes extracts described above or any one of the lysimachia capillipes extract compositions described above.
In some embodiments, the tobacco product is a tobacco leaf, a tobacco shred, or an electronic cigarette liquid.
In some aspects, a lysimachia capillipes essence is provided comprising any of the above mentioned lysimachia capillipes extracts or any of the above mentioned lysimachia capillipes extract compositions.
In some embodiments, the lysimachia capillipes essence further contains one or more of the following: ethanol aqueous solution, propylene glycol, sorbitol and xylitol.
Description of the terms
As used herein, the following terms are used, which terms may have the following meanings:
the single/double effect external circulation vacuum concentrator includes heater, evaporating chamber, condenser, liquid receiver, etc.
The single-effect vacuum concentration apparatus may be as described in: ' Gulin, Taoyuigui main weaving; liu hantao, wu honor vice consolidations, "food machinery and equipment [ M ]. beijing: china textile Press, 2016.06 ", section 10.2".
The dual effect vacuum concentration apparatus may be as described in: ' Gulin, Taoyuigui main weaving; liu hantao, a sovereign assistant, food machinery and equipment [ M ]. beijing: china textile Press, 2016.06 ", section 10.3.2.1".
The term "steam distillation" may be either direct steam distillation or water distillation, i.e. passing the steam through the lysimachia capillipes raw material, then condensing the steam and collecting the condensate. During this time, the lysimachia capillipes raw material was not soaked in water.
Relative density refers to density relative to water.
Advantageous effects
The extract preparation method/extract/essence/tobacco product disclosed by the invention has one or more of the following beneficial effects:
(1) the integrated extraction process can extract two extracts with different styles from a batch of raw materials, improves the utilization rate of the raw materials, reduces the cost and is more environment-friendly;
(2) the two extracts with different styles are combined for use, so that unexpected improvement of sensory quality can be brought to the tobacco products;
(3) before the steam extraction, water is applied to the lysimachia capillipes raw material, which is helpful for improving the quality of the extract;
(4) controlling the temperature of reverse osmosis concentration to be lower than 25 ℃ helps to improve the quality of the extract.
Embodiments of the present invention will be described in detail below with reference to the drawings and examples, but those skilled in the art will understand that the following drawings and examples are only for illustrating the present invention and are not to be construed as limiting the scope of the present invention. Various objects and advantageous aspects of the present invention will become apparent to those skilled in the art from the accompanying drawings and the following detailed description of the preferred embodiments.
Drawings
FIG. 1 is a schematic diagram showing a process for preparing a Lysimachia capillipes extract.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1.1
Cutting 20kg of sun-dried whole lysimachia capillipes into sections of 15cm to obtain lysimachia capillipes raw materials, and then applying 2kg of water to the lysimachia capillipes raw materials;
step (2) placing the product obtained in the step (1) in steam distillation equipment, introducing steam, controlling the opening of a steam valve to ensure that the flow of steam condensate is 100kg/h and the time is 3 hours, and collecting 300kg of steam condensate, namely the lysimachia capillipes hemsl hydrolat pure dew;
step (3.10) reverse osmosis concentration of the purified water obtained in step 2 by using a reverse osmosis membrane, and collection of the trapped fluid, specifically comprising the following steps (3.11) and (3.12)
And (3.11) concentrating the pure dew obtained in the step (2) by adopting a pilot plant RO membrane reverse osmosis, wherein the equipment is RNF-2500 type roll-type membrane multifunctional pilot plant equipment, the model of a mold core is GSM-RE2540-TE, the membrane outlet pressure is controlled to be 0.6 +/-0.2 MPa, the membrane inlet pressure is controlled to be 1.2 +/-0.2 MPa, the pump frequency is 50Hz, the material temperature is 15 ℃, and the concentration multiple is 10 +/-1 times.
And (3.12) concentrating the product of the step (3.12) by adopting a small-scale RO membrane reverse osmosis, wherein the equipment is RNF-0460-.
The overall concentration factor for steps 3.11 and 3.12 is about 90 fold.
Example 1.2:
step (3.20) continuing to distill the residue of the lysimachia capillipes hemsl in the example 1.1 for 2 hours, controlling the flow of the steam condensate to be 100Kg/h, and collecting the distilled residue; this step is performed in order to sufficiently remove characteristic style components of lysimachia capillipes (i.e., herb odor);
step (3.21) adding 20 times by mass of 70% edible ethanol aqueous solution into the residue in the previous step, extracting at 80 ℃ for 180min for 1 time, and collecting the filtrate;
step (3.22) centrifuging the filtrate obtained in step (3.21) at 9000rpm at 20 ℃ for 30min to obtain a centrifuged clear solution;
and (3.23) concentrating the centrifugal clear liquid obtained in the step (3.22) by adopting a single-effect concentration unit, wherein the equipment parameters are set as follows: the opening of the steam valve is 85 percent, the steam pressure is-0.008 Mpa, the steam temperature is 76 ℃, and the feeding flow is 0.26m3The feed temperature is 30 ℃, the circulating temperature is 50 ℃, the condenser pressure is-0.008 Mpa, the condenser temperature is 12 ℃, and the evaporation capacity is 0.22m3H is used as the reference value. 20kg of a second extract was obtained, which had a relative density of 1.1 at 20 ℃.
2. Analysis and detection of the aroma components of the extract:
2.1.1 sample preparation
(1) HS-GC-MS sample preparation: and (3) putting 2.0g of sample into a headspace bottle, adding 400 mu L of saturated saline solution, adding 100 mu L of 2-hexanone methanol working solution, and sealing the cap to be tested.
(2) GC-MS sample preparation: taking 1-3 g of sample, adding 10ml of dichloromethane extract according to the condition of the sample, mechanically shaking for 20min, taking the clear liquid, preparing the sample to be tested.
(3) SPME sample preparation: and (3) putting 1.0g of sample into a headspace bottle, adding 5ml of purified water, sealing the cap, and testing.
2.1.2HS-GC-MS combinations
(1) Static headspace: keeping the furnace temperature at 90 ℃ for 60 min; the sampling needle is 110 ℃, and the transmission line is 130 ℃; injecting sample for 0.15min, and withdrawing needle for 0.5 min; pressurizing for 2.0min, circulating for 70min by GC analysis, injecting sample under high pressure, keeping constant, injecting sample in time mode, and injecting sample 35Psi by chromatographic column.
(2) Chromatographic conditions are as follows: SUPELCO SPB-624(60m × 0.25mm × 0.14 μm); temperature programming: keeping at 60 deg.C for 1min, increasing to 170 deg.C at 2 deg.C/min, increasing to 240 deg.C at 50 deg.C/min, and keeping for 10 min.
And (3) qualitative analysis: the NIST2014 library, in principle with a degree of qualitative >80, was partly combined with literature and empirical determinations.
Semi-quantitative analysis: the internal standard 2-hexanone is uniformly adopted for internal standard-semi-quantification.
2.1.3GC-MS combinations
A chromatographic column: HP-INNOWAX (19091N-136,260 ℃, 60 m.times.0.25 mm.times.0.25 μm);
sample inlet temperature: 240 ℃, sample size: 1 mu L of the solution; carrier gas: helium, split ratio 10: l;
temperature rising procedure: column temperature 60 deg.C (keeping for 2min), heating to 180 deg.C at 2 deg.C/min, and heating to 230 deg.C at 5 deg.C/min (keeping for 40 min);
transmission line temperature: 240 ℃; ion source temperature: 230 ℃; temperature of the quadrupole rods: 150 ℃;
EI voltage: 70 eV;
TIC full scan detection, scan range: 35-450 amu.
And (3) qualitative analysis: the NIST2014 library, in principle with a degree of qualitative >80, was partly combined with literature and empirical determinations.
Semi-quantitative analysis: and uniformly adopting an internal standard phenethyl acetate for internal standard-semi-quantification.
2.1.4 Solid Phase Microextraction (SPME)
(1) SPME extraction fiber (Supelco, USA, 30/50 μm DVB/CAR/PDMS)
(2) Agilent DB-17ms quartz capillary column (60m × 0.25mm × 0.25 μm); temperature rising procedure: keeping the temperature at 60 ℃ for 2min, heating to 240 ℃ at the speed of 2 ℃/min, keeping the temperature for 2min, heating to 300 ℃ at the speed of 10 ℃/min, and keeping the temperature for 20 min; the flow rate of carrier gas (He) is 1.0mL/min, the temperature of a sample inlet is 250 ℃, and the sample is injected without shunting.
Mass spectrum conditions: an ion source: EI; electron energy: 70 eV; transmission line temperature: 250 ℃; ion source temperature: 250 ℃; the temperature of a four-level bar is 150 ℃; solvent retardation: 8 min; SCAN scanning is adopted, and the mass scanning range m/z is 45-300.
And (5) carrying out qualitative component search by adopting a last spectral library, and calculating the relative content of each component by adopting a peak area percentage method.
2.2 Studies of the aroma Components of the first extract
The first extract was analyzed by HS-GC-MS (combined headspace gas chromatography-mass spectrometry) and GC-MS (combined gas chromatography-mass spectrometry) and the analysis results obtained are shown in table 1.1. The two analysis methods detect 43 effective components in total, wherein 12 effective components are aroma components of tobacco leaves, and the proportion of the aroma components in the detected effective components is 27.9 percent, which explains the reason of the coordination of the lysimachia capillipes extract and cigarettes from the analysis point of view.
33 compounds are detected in total by HS-GC-MS, and 9 of the compounds are aroma components of tobacco leaves. These 33 compounds are essentially volatile and semi-volatile components such as aldehydes, ketones, lactones, and the like, and in particular the high proportion of aldehydes, which explains why the first extract has a strong flavor characteristic of lysimachia capillipes, since essential oils, which are generally used to represent the flavor characteristic of natural fragrance raw materials, are essentially dominated by aldehydes.
13 compounds are detected by GC-MS in total, and 5 of the compounds are the aroma components of tobacco leaves.
TABLE 1.1 comparison of the major aroma components of the first extract analyzed by HS-GC-MS and GC-MS
Remarks are: the component is the aroma component of tobacco leaf
2.3 Studies of the aroma Components of the second extract
The second extract mainly contains the functional components of the lysimachia capillipes and the main components of the second extract are semi-volatile or nonvolatile substances.
The flavor components of the second extract were analyzed by SPME (solid phase microextraction) and GC-MS (gas chromatography-mass spectrometry), and the results are shown in table 1.2 for reasons of harmony with cigarettes.
The SPME detects 44 compounds in total, and 12 of the compounds are the aroma components of tobacco leaves. The 44 compounds are mainly semi-volatile components such as long-carbon paraffin, macromolecular alcohols and the like, a part of oxygen-heterocyclic volatile components and a small amount of 2-methyl-2-butenal which is a characteristic style component of lysimachia capillipes; the analysis result also proves the feasibility of the refining integrated process, namely, the functional components of the lysimachia capillipes are enriched, meanwhile, the gain in the aspect of aroma is kept, and most of the characteristic style components of the lysimachia capillipes are removed.
12 compounds are detected by GC-MS, and 3 of the compounds are aroma components of tobacco leaves.
TABLE 1.2 comparison of the main aroma components of the second extract analyzed by SPME and GC-MS
Remarks are: the component is the aroma component of tobacco leaf
Application example 1
Diluting the mixed solution prepared by mixing the first extract, the food-grade ethanol aqueous solution, the propylene glycol, the sorbitol and the xylitol according to the mass ratio of 4:100:1:2:1 by 10 times, adding the diluted mixed solution to the cut tobacco in a spraying mode according to the addition amount of 0.01 percent of the weight of the cut tobacco, and preparing the cigarette with the number of 1A.
(the weight ratio of the first extract to the tobacco shred is about 4:107)
Application example 2
Diluting the mixed solution prepared by mixing the second extract, the food-grade ethanol aqueous solution, the propylene glycol, the sorbitol and the xylitol according to the mass ratio of 4:10:1:1:1 by 10 times, adding the diluted mixed solution to the cut tobacco in a spraying mode according to the addition amount of 0.1% of the weight of the cut tobacco, and preparing the cigarette with the serial number 2A.
(second extract and tobacco shred weight)The ratio is about 2.3: 105)
Application example 3
Diluting the mixed solution prepared by mixing the first extract, the second extract, the food-grade ethanol aqueous solution, the propylene glycol, the sorbitol and the xylitol according to the mass ratio of 1:10:50:3:1:1 by 10 times, adding the diluted mixed solution to the cut tobacco in a spraying mode according to the addition amount of 0.05 percent of the weight of the cut tobacco, and preparing the cigarette with the number of 3A.
(the weight ratio of the composition of the first extract and the second extract to the cut tobacco is 8.3: 106)
Qualitative and quantitative evaluation
The organization professional cigarette evaluation personnel qualitatively and quantitatively evaluate the cigarettes 1A-3A. The scoring standard of quantitative evaluation refers to the sensory quality evaluation of cigarettes 1A to 3A according to the national standard (GB5606.4-2005), the scoring evaluation is shown in Table 2.1, and the description evaluation is shown in Table 2.2 below.
TABLE 2.1 evaluation of cigarettes 1A, 2A, 3A by sensory quality grading
| Item | Gloss 5 | Fragrance 32 | Tune 6 | Miscellaneous gas 12 | Irritation 20 | Aftertaste 25 | Total up to |
| Blank space | - | 29 | 5 | 10 | 18 | 22 | 84 |
| 1A | - | 30.5 | 5.5 | 11 | 19 | 22.5 | 88.5 |
| 2A | - | 30.5 | 5.5 | 11 | 19.5 | 23 | 89.5 |
| 3A | - | 31 | 5.5 | 11.5 | 19.5 | 23.5 | 91 |
TABLE 2.2 sensory quality description evaluation Table for cigarettes 1A, 2A, 3A
As shown in the table above, the cigarettes 1A, 2A and 3A all had better scores than the blank.
The score and evaluation of cigarette 3A was best, superior to cigarettes 1A and 2A, indicating that the combination of the first and second extracts indeed improved the sensory quality of the cigarettes.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention and not to limit it; although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art will understand that: modifications to the specific embodiments of the invention or equivalent substitutions for parts of the technical features may be made; without departing from the spirit of the present invention, it is intended to cover all aspects of the invention as defined by the appended claims.
Claims (15)
1. A method of preparing a lysimachia capillipes extract comprising the steps of:
(1) applying water to the lysimachia capillipes hemsl raw material, wherein the weight of the water is 5-20% of the principle weight of the lysimachia capillipes hemsl;
(2) performing steam distillation on the product obtained in the step (1), wherein the distillation time is 3-4 hours, controlling the hourly flow of a steam condensate to be 3-10 times of the weight of the lysimachia capillipes hemsl raw material, and collecting the steam condensate, namely the lysimachia capillipes hemsl pure dew;
(3.10) performing reverse osmosis concentration on the hydrolat obtained in the step (2) by using a reverse osmosis membrane, and collecting trapped fluid to obtain a first extract;
(3.20) continuing steam distillation on the product obtained in the step (2) for 1-2 hours, wherein the hourly flow rate of a steam condensate is 3-10 times of the weight of the lysimachia capillipes hemsl raw material, and collecting residues after distillation;
(3.21) adding a polar solvent which is 10-30 times of the residue in mass into the residue obtained in the step 3.20 for extraction at the temperature of 60-100 ℃ for 60-180min, and filtering after extraction to obtain a filtrate;
(3.22) centrifuging the filtrate obtained in the step 3.21 to obtain a centrifugal clear liquid;
(3.23) concentrating the centrifuged clear liquid in the step 3.22 by adopting a vacuum evaporation concentration method to obtain a second extract, wherein the relative density of the second extract at 20 ℃ is 1.0-1.3;
optionally, the first extract is mixed with the second extract.
2. The method of claim 1, wherein the reverse osmosis concentration is performed at a temperature of 25 ℃ or less, for example 10 to 25 ℃ in step 3.10.
3. The method of claim 1, step 3.10 comprising:
step (3.11) performing reverse osmosis concentration on the pure dew obtained in the step (2) by using a CSM-RE2540-TE reverse osmosis membrane, controlling the membrane outlet pressure to be 0.4-0.8 Mpa, the membrane inlet pressure to be 1.2 +/-0.2 Mpa, the pump frequency to be 40-60 Hz, the material temperature to be 10-25 ℃, and the concentration multiple to be 8-12 times;
and (3.12) performing reverse osmosis concentration on the concentrate in the step (3.11) by using a Suez/GE-1812 reverse osmosis membrane, controlling the membrane outlet pressure to be 1.8-2.2 Mpa, the pump frequency to be 40-60 Hz, the material temperature to be 10-25 ℃, and the concentration multiple to be 7-9 times.
4. The method according to claim 1, wherein in step 3.21, the polar solvent is pure water or ethanol aqueous solution with concentration of 40-95 wt%.
5. The method according to claim 1, wherein step 3.21 is repeatedly performed 2 to 5 times.
6. The method according to claim 1, wherein in step 3.22, the centrifugation is performed at a speed of 5000-16000 rpm at a temperature of 10-30 ℃ for 10-30 min.
7. The process of claim 1, step 3.23, wherein the vacuum concentration is carried out using a single effect concentration device or a double effect concentration device.
8. The method according to claim 1, wherein the lysimachia capillipes raw material is dried whole lysimachia capillipes grass.
9. A Lysimachia capillipes extract which is the first extract obtained by the method of any one of claims 1 to 8.
10. A Lysimachia capillipes extract which is the second extract obtained by the method of any one of claims 1 to 8.
11. A lysimachia capillipes extract composition comprising a first extract according to claim 9 and a second extract according to claim 10;
preferably, the weight ratio of the first extract to the second extract is 1: 8-12.
12. Use of lysimachia capillipes or an extract of lysimachia capillipes for the preparation of a tobacco product;
preferably, the tobacco product is a tobacco leaf, a tobacco shred or an electronic cigarette liquid.
13. The use according to claim 12, the lysimachia capillipes extract being the lysimachia capillipes extract of claim 9, the lysimachia capillipes extract of claim 10 or the lysimachia capillipes extract composition of claim 11.
14. A tobacco product comprises Lysimachia capillipes or a Lysimachia capillipes extract;
preferably, the lysimachia capillipes extract of claim 9, the lysimachia capillipes extract of claim 10 or the lysimachia capillipes extract composition of claim 11;
preferably, the tobacco product is a tobacco leaf, a tobacco shred or an electronic cigarette liquid.
15. A lysimachia capillipes essence containing the lysimachia capillipes extract of claim 9, the lysimachia capillipes extract of claim 10 or the lysimachia capillipes extract composition of claim 11;
preferably, the lysimachia capillipes essence further contains one or more of the following substances: ethanol aqueous solution, propylene glycol, sorbitol and xylitol.
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| CN111004679B (en) | 2023-04-07 |
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