CN114276870A - Comprehensive utilization process of folium artemisiae argyi - Google Patents
Comprehensive utilization process of folium artemisiae argyi Download PDFInfo
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to a comprehensive utilization process of folium artemisiae argyi, in particular to a preparation process of folium artemisiae argyi essential oil and a secondary development and utilization process of folium artemisiae argyi residues, wherein the process comprises the following steps: (1) fully drying and crushing the folium artemisiae argyi raw material; (2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, and introducing carbon dioxide for supercritical extraction; (3) separating the extracted mixed materials through a separation kettle; (4) adding absolute ethyl alcohol into the crude argy wormwood leaf oil under stirring, and filtering to remove impurities; (5) distilling the filtrate under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil; (6) after extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
Description
Technical Field
The invention belongs to the technical field of plant extraction, and particularly relates to a preparation process of folium artemisiae argyi essential oil and a secondary development and utilization process of folium artemisiae argyi residues.
Background
Folium artemisiae argyi, name of traditional Chinese medicine. Is leaf of Artemisia argyi Levl. et Vant. Has effects of warming channels, stopping bleeding, dispelling cold, relieving pain, eliminating dampness, and relieving itching. Folium Artemisiae Argyi has antibacterial, reticuloendothelial cell phagocytosis enhancing, antiasthmatic, anaphylactic shock resisting, antitussive, expectorant, gallbladder function promoting, and uterus exciting effects, and has effects on cardiovascular system, blood coagulation, blood platelet, and central nervous system.
The folium artemisiae argyi is rich in various bioactive components, wherein volatile oil is a main active component group of the folium artemisiae argyi, the content of the volatile oil of the folium artemisiae argyi is 1.23%, and the volatile oil of the folium artemisiae argyi becomes a research hotspot at the current stage. The folium Artemisiae Argyi volatile oil has antibacterial, antiinflammatory, disinfectant, anthelmintic, whitening, hemostatic, antiallergic, sneezing, and antipruritic effects, and is an important raw material for food, perfume, and chemical industry.
The extraction method of volatile oil of folium Artemisiae Argyi can be divided into steam distillation, microwave-assisted method, supercritical fluid extraction, ultrasonic-assisted method, solvent method, squeezing method, semi-bionic method, active ion water method, enzyme method, and charging method. Wangweisheng researches a process for extracting folium artemisiae argyi volatile oil by a CO2 supercritical extraction method (the yield is improved by 97.67% compared with the yield extracted by a steam distillation method, the method selectively extracts, separates and purifies effective components, but the obtained volatile oil is not pure, so that the volatile oil is easy to lose in the treatment process.
At present, the method for extracting the blumea oil which is simpler and cheaper is a steam distillation method, and has the defects of easy damage of heat-sensitive components, mixed components, low purity and the like, and low yield of the blumea oil.
The invention provides a novel method for extracting the argyi leaf oil, which does not destroy thermosensitive components, improves the purity of essential oil and the yield, and can develop and utilize the argyi leaf residues for the second time.
Disclosure of Invention
The invention provides a comprehensive utilization method of folium artemisiae argyi.
The method comprises the following steps:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a sieve with 10-80 meshes;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, wherein the main extraction parameters are as follows: the extraction temperature is 35-50 ℃, the extraction pressure is 16-30MPa, the flow of carbon dioxide is 20-50L/h.kg, and the extraction time is 1-2 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, the main parameter of separation: the pressure of the separation I is 5-8MPa, and the temperature is 40-70 ℃; the pressure of the separation II is 4-6MPa, and the temperature is 20-40 DEG C
(4) Adding anhydrous ethanol into folium Artemisiae Argyi crude oil under stirring, filtering to remove impurities
(5) Distilling the filtrate under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil.
(6) After extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
The folium artemisiae argyi essential oil obtained by the invention has the eucalyptol content of more than 0.50mg/g, and the detection method comprises the following steps:
gas chromatography for determining content of eucalyptol in volatile oil
1, using polyethylene glycol 20000(PEG-20M) and silicone (OV-17) as fixative under chromatographic conditions, wherein the coating concentrations are respectively 10% and 2%; the coated carrier is loaded into the same column (PEG at the sample inlet end) in a ratio (mass ratio) of 7: 3; the column temperature is (110 +/-5) DEG C; the carrier gas is N2, and the flow rate is 1.5 ml/min; the split ratio is 20: 1; the temperature of the sample inlet is 180 ℃, and the temperature of the detector is 230 ℃; the number of theoretical plates is not less than 2500 calculated according to the eucalyptol peak; the separation degree of the eucalyptol and adjacent impurity peaks meets the requirement.
2 determination of correction factor
Taking a proper amount of cyclohexanone, precisely weighing, adding n-hexane for dissolving and diluting into a solution with the mass concentration of 50g/l, and taking the solution as an internal standard solution. And precisely weighing about 100mg of eucalyptol reference substance, placing into a 10ml volumetric flask, precisely adding 2ml of internal standard solution, diluting to scale with n-hexane, shaking up, injecting 1 μ l into a gas chromatograph, continuously injecting for 3-5 times, measuring peak area, and calculating correction factor.
3 measurement method
Drying the collected folium artemisiae argyi volatile oil by using anhydrous sodium sulfate, filtering, precisely weighing, taking about 100mg of a sample, precisely weighing, placing in a 10ml volumetric flask, precisely adding 2ml of internal standard solution, dissolving by using n-hexane and diluting to a scale, shaking up to be used as a sample solution. Injecting 1 μ l into gas chromatograph, measuring, and calculating eucalyptol content (mg/g).
The moxa leaf residue, the agilawood and the elm bark powder are uniformly mixed, extruded and molded, and dried to prepare the moxa, and the preparation method comprises the following steps:
(1) taking the folium artemisiae argyi dregs out of the extraction kettle,
pulverizing agilawood and elm bark into powder of 60-80 meshes, taking 10 parts of each, adding 80 parts of folium artemisiae argyi material residues, adding 20 parts of water, and uniformly mixing in a container to obtain the moxa mud;
(3) and extruding and molding the moxa stick to prepare a strip shape, wherein the length of the incense body is 30-35cm, and the diameter is 2-3 mm. Drying the bar incense in an oven at 40-50 deg.C for 2 hr to obtain final product.
The moxa obtained by the invention can be burnt for 1.5 hours each time.
The method of the invention, such as technical conditions, technical parameters and the like, is obtained by experimental screening on the basis of the prior art, and the screening process is as follows:
preferably, the crushed materials in the step (1) are sieved by a 40-60-mesh sieve, and undersize materials are taken;
the core of the invention lies in the screening of extraction conditions, the extraction results are different under different conditions, the following is
The screening steps and screening results of the extraction conditions of the invention are as follows:
screening of extraction pressure, temperature and flow
| Serial number | Extraction pressure (Mpa) | Extraction temperature (. degree.C.) | Flow (L/h kg) | Yield (%) |
| 1 | 20-24 | 35-40 | 25-30 | 4.12 |
| 2 | 20-24 | 40-45 | 30-35 | 3.54 |
| 3 | 20-24 | 45-50 | 35-40 | 4.15 |
| 4 | 24-28 | 35-40 | 25-30 | 4.38 |
| 5 | 24-28 | 40-45 | 30-35 | 5.40 |
| 6 | 24-28 | 45-50 | 35-40 | 5.14 |
| 7 | 28-32 | 35-40 | 25-30 | 4.22 |
| 8 | 28-32 | 40-45 | 30-35 | 4.66 |
| 9 | 28-32 | 45-50 | 35-40 | 4.32 |
The result shows that the extraction pressure is 24-28Mpa, the extraction temperature is 40-45 ℃, and the flow is best 30-35L/h.kg; screening of extraction time
Taking 1000g of crushed folium artemisiae argyi powder, loading the crushed folium artemisiae argyi powder into a 5L supercritical extraction device, starting a high-pressure pump, a hot water and cooling system matched with the high-pressure pump, setting the extraction pressure to be 24-28Mpa, the extraction temperature to be 40-45 ℃, the flow rate to be 30-35L/h.kg, discharging an extract from the bottom of a separation column every 15min after extraction process parameters are stable, and weighing. The results are as follows:
the result shows that the effect is best when the extraction time is 1.0-1.25 hours
Preferably, the separation I in the step (3) has the pressure of 6-7MPa and the temperature of 50-60 ℃;
preferably, the addition amount of the absolute ethyl alcohol in the step (4) is 1 time of that of the crude oil;
preferably, the reduced pressure distillation temperature of the step (5) is 40-50 ℃;
preferably, in the step (6), the use ratio of the folium artemisiae argyi dregs, the agilawood and the elm bark is 8: 1: 1;
the folium artemisiae argyi essential oil has better purity and higher yield, and the folium artemisiae argyi material residues can be developed and utilized for the second time.
The beneficial effects of the invention are further illustrated by experimental data below
| Yield of volatile oil | Eucalyptol content | |
| Method of example 1 of the invention | 5.04％ | 0.52mg/g |
| Steam distillation method | 1.12％ | 0.26mg/g |
| Method for Wangsheng and the like | 1.44％ | 0.32mg/g |
Research on a process for extracting volatile oil from folium artemisiae argyi by a CO2 supercritical extraction method in 09.2017 of Chinese medicine; maintaining the bear; lijing et al disclose the following:
the optimal extraction conditions of the folium artemisiae argyi volatile oil are that the extraction pressure is 20MPa, the extraction temperature is 30 ℃, the separation pressure is 8MPa, the separation temperature is 55 ℃, the average volatile oil yield is 1.443%, and the average eucalyptol content is 0.318 mg/g.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto.
Example 1:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a 40-mesh sieve;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, and setting extraction parameters as follows: the extraction temperature is 45 ℃, the extraction pressure is 28MPa, the carbon dioxide flow is 35L/h.kg, and the extraction time is 1 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, and the separation parameter sets for: the pressure of the separation I is 7MPa, and the temperature is 50 ℃; the pressure of the separation II is 4MPa, and the temperature is 30 DEG C
(4) Adding 1 time of anhydrous ethanol into folium Artemisiae Argyi crude oil under stirring, filtering to remove impurities
(5) Distilling the filtrate at 45 deg.C under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil.
(6) After extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
1000g of the feed is fed at this time, 50.4g of the folium artemisiae argyi essential oil is collected, and the yield of the folium artemisiae argyi essential oil is 5.04%.
Example 2:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a 40-mesh sieve;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, and setting extraction parameters as follows: the extraction temperature is 45 ℃, the extraction pressure is 24MPa, the flow of carbon dioxide is 35L/h.kg, and the extraction time is 1 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, and the separation parameter sets for: the pressure of the separation I is 6MPa, and the temperature is 55 ℃; the pressure of the separation II is 4MPa, and the temperature is 30 DEG C
(4) Adding 1 time of anhydrous ethanol into folium Artemisiae Argyi crude oil under stirring, filtering to remove impurities
(5) Distilling the filtrate at 45 deg.C under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil.
(6) After extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
1000g of the feed is fed at this time, 54g of folium artemisiae argyi essential oil is collected, and the yield of the folium artemisiae argyi essential oil is 5.40%.
Example 3:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a 40-mesh sieve;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, and setting extraction parameters as follows: the extraction temperature is 45 ℃, the extraction pressure is 24MPa, the carbon dioxide flow is 30L/h.kg, and the extraction time is 1 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, and the separation parameter sets for: the pressure of the separation I is 7MPa, and the temperature is 50 ℃; the pressure of the separation II is 4MPa, and the temperature is 30 DEG C
(4) Adding 1 time of anhydrous ethanol into folium Artemisiae Argyi crude oil under stirring, filtering to remove impurities
(5) Distilling the filtrate at 45 deg.C under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil.
(6) After extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
1000g of the feed is fed at this time, 41.5g of the argy wormwood leaf essential oil is collected, and the yield of the argy wormwood leaf essential oil is 4.15%.
The scope of the invention includes, but is not limited to, the following:
1. supercritical extraction and separation process parameter range
2. Method for obtaining essential oil by combining extraction and reduced pressure distillation
3. And (4) secondary development and utilization of the folium artemisiae argyi residues.
Claims (6)
1. The comprehensive utilization process of the folium artemisiae argyi is characterized by comprising the following steps of: firstly, extracting folium artemisiae argyi essential oil by a supercritical carbon dioxide extraction method, and then further processing extracted medicine dregs to prepare the spice.
2. The process according to claim 1, characterized in that it comprises the following steps: (1) fully drying and crushing the folium artemisiae argyi raw material; (2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, and introducing carbon dioxide for supercritical extraction; (3) separating the extracted mixed materials through a separation kettle; (4) adding absolute ethyl alcohol into the crude argy wormwood leaf oil under stirring, and filtering to remove impurities; (5) distilling the filtrate under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil; (6) after extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
3. The process according to claim 1, characterized in that it comprises the following steps:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a sieve with 10-80 meshes;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, wherein the main extraction parameters are as follows: the extraction temperature is 35-50 ℃, the extraction pressure is 16-30MPa, the flow of carbon dioxide is 20-50L/h.kg, and the extraction time is 1-2 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, the main parameter of separation: the pressure of the separation I is 5-8MPa, and the temperature is 40-70 ℃; the pressure of the separation II is 4-6MPa, and the temperature is 20-40 ℃;
(4) adding absolute ethyl alcohol into the crude argy wormwood leaf oil under stirring, and filtering to remove impurities;
(5) distilling the filtrate under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil;
(6) after extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
4. The process according to claim 1, characterized in that it comprises the following steps:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a 40-mesh sieve;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, and setting extraction parameters as follows: the extraction temperature is 45 ℃, the extraction pressure is 28MPa, the carbon dioxide flow is 35L/h.kg, and the extraction time is 1 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, and the separation parameter sets for: the pressure of the separation I is 7MPa, and the temperature is 50 ℃; the pressure of the separation II is 4MPa, and the temperature is 30 ℃;
(4) adding 1 time of absolute ethyl alcohol into the crude artemisia argyi oil under stirring, and filtering to remove impurities;
(5) distilling the filtrate at 45 deg.C under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil;
(6) after extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
5. The process according to claim 1, characterized in that it comprises the following steps:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a 40-mesh sieve;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, and setting extraction parameters as follows: the extraction temperature is 45 ℃, the extraction pressure is 24MPa, the flow of carbon dioxide is 35L/h.kg, and the extraction time is 1 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, and the separation parameter sets for: the pressure of the separation I is 6MPa, and the temperature is 55 ℃; the pressure of the separation II is 4MPa, and the temperature is 30 ℃;
(4) adding 1 time of absolute ethyl alcohol into the crude artemisia argyi oil under stirring, and filtering to remove impurities;
(5) distilling the filtrate at 45 deg.C under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil;
(6) after extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
6. The process according to claim 1, characterized in that it comprises the following steps:
(1) fully drying and crushing the folium artemisiae argyi raw material, and sieving the dried and crushed folium artemisiae argyi raw material by a 40-mesh sieve;
(2) putting the crushed folium artemisiae argyi raw material into a supercritical extraction kettle, introducing carbon dioxide for supercritical extraction, and setting extraction parameters as follows: the extraction temperature is 45 ℃, the extraction pressure is 24MPa, the carbon dioxide flow is 30L/h.kg, and the extraction time is 1 h;
(3) the mixed material after the extraction separates through the separation cauldron, and wherein the chinese mugwort leaf crude oil is discharged from I bottom of separation cauldron, and moisture is discharged from II bottoms of separation, and the separation parameter sets for: the pressure of the separation I is 7MPa, and the temperature is 50 ℃; the pressure of the separation II is 4MPa, and the temperature is 30 ℃;
(4) adding 1 time of absolute ethyl alcohol into the crude artemisia argyi oil under stirring, and filtering to remove impurities;
(5) distilling the filtrate at 45 deg.C under reduced pressure to recover ethanol to obtain folium Artemisiae Argyi essential oil;
(6) after extraction is finished, taking the folium artemisiae argyi residue in the extraction kettle out, adding agilawood and elm bark powder, uniformly mixing, carrying out extrusion forming, and drying to obtain the folium artemisiae argyi.
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| CN102326590A (en) * | 2011-09-28 | 2012-01-25 | 许银亚 | Mugwort leaf mosquito incense |
| CN105532761A (en) * | 2016-02-17 | 2016-05-04 | 广西大学 | Folium artemisiae argyi mosquito-repellent incense and manufacturing method thereof |
| CN109198366A (en) * | 2018-07-11 | 2019-01-15 | 安徽靳氏食品有限公司 | A kind of Salted duck egg wraps up in material and its processing technology |
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| CN102326590A (en) * | 2011-09-28 | 2012-01-25 | 许银亚 | Mugwort leaf mosquito incense |
| CN105532761A (en) * | 2016-02-17 | 2016-05-04 | 广西大学 | Folium artemisiae argyi mosquito-repellent incense and manufacturing method thereof |
| CN109198366A (en) * | 2018-07-11 | 2019-01-15 | 安徽靳氏食品有限公司 | A kind of Salted duck egg wraps up in material and its processing technology |
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