阅读说明：本技术 一种仙草浓缩液的制备方法 (Preparation method of Mesona chinensis Benth concentrated solution ) 是由 王志鹏 胡建红 李坚 陈增自 于 2021-11-25 设计创作，主要内容包括：本发明提供一种仙草浓缩液的制备方法,包括以下步骤：S1.原料预处理：将仙草切草后,进行负压吸尘；S2.提取：S21.超临界CO2萃取,将预处理的仙草进行超临界CO2萃取,以乙醇作为夹带剂进行超临界萃取,得到萃取液和仙草渣；S22.水提：将所述仙草渣投入逆流提取设备中,加入水煮沸,熬煮2～5h,过滤,得到水提液；S3.过滤：将所述萃取液和水提液混合得到提取液,然后经过纳滤膜过滤得到过滤液；S4.浓缩：将过滤液采用反渗透膜浓缩得到仙草浓缩液。该方法采用超临界CO2萃取和水提结合的提取方法,能够可最大限度地保留仙草提取液中的风味物质,充分保持仙草的香味。(The invention provides a preparation method of a Mesona chinensis Benth concentrated solution, which comprises the following steps: s1, raw material pretreatment: cutting mesona chinensis benth, and then performing negative pressure dust collection; s2, extraction: s21, performing supercritical CO2 extraction, namely performing supercritical CO2 extraction on the pretreated Mesona chinensis Benth, and performing supercritical extraction by using ethanol as an entrainer to obtain an extract and Mesona chinensis Benth residues; s22, water extraction: putting the mesona blume residues into a countercurrent extraction device, adding water, boiling, decocting for 2-5 h, and filtering to obtain a water extract; s3, filtering: mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate; s4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution. The method adopts supercritical CO2 extraction and water extraction combined extraction method, can maximally retain flavor substances in Mesona chinensis Benth extract, and fully maintain Mesona chinensis Benth fragrance.)

1. The preparation method of the mesona chinensis benth concentrated solution is characterized by comprising the following steps of:

s1, raw material pretreatment: cutting mesona chinensis benth, and then performing negative pressure dust collection;

s2, extraction:

s21. supercritical CO₂Extracting, subjecting the pretreated Mesona chinensis to supercritical CO extraction₂Extracting, namely performing supercritical extraction by using ethanol as an entrainer to obtain extract liquor and mesona chinensis benth residues;

s22, water extraction: putting the mesona blume residues into a countercurrent extraction device, adding water, boiling, decocting for 2-5 h, and filtering to obtain a water extract;

s3, filtering: mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate;

s4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution.

2. The method as claimed in claim 1, wherein the negative pressure suction pressure is-1.5 to-2 MPa in step S1.

3. The method of claim 1, wherein the ethanol concentration in step S21 is 85-95 wt%.

4. The method for preparing Mesona chinensis Benth concentrated solution according to claim 1, wherein in step S21, the extraction pressure is 20-40 MPa, the extraction temperature is 35-50 ℃, the extraction time is 1-4 h, and CO is added₂The flow rate is 15-30L/h, and the dosage of ethanol is 0.5-1 mL/g.

5. The method for preparing Mesona chinensis Benth concentrated solution according to claim 1, wherein in step S21, water is added according to a ratio of 1: 10-20.

6. The method for preparing a concentrated Mesona chinensis Benth solution as claimed in claim 1, wherein in step S21, water extraction is performed to obtain water extractive solution and residue, the residue is subjected to secondary water extraction, and the water extractions of the two water extractions are combined.

7. The method for preparing the mesona chinensis benth concentrated solution as claimed in claim 1, wherein in step S3, the cut-off molecular weight of the nanofiltration membrane is 400-600 daltons.

8. The method for preparing Mesona chinensis Benth concentrated solution according to claim 1, wherein the reverse osmosis membrane enrichment process is carried out by using a two-stage reverse osmosis membrane system.

[ technical field ] A method for producing a semiconductor device

The invention relates to the technical field of biology, and in particular relates to a preparation method of a Mesona chinensis Benth concentrated solution.

[ background of the invention ]

Mesona chinensis Benth is also called Mesona chinensis Benth, and plant of Mesona genus of Labiatae family. Is an important plant resource for both medicine and food. Is a natural green food in plants, and has high nutritional and medicinal values. The herb of fagopyrum cymosum is used for folk in hundreds of years to prepare a cool spot beverage which is heat clearing, summer heat clearing, cool and refreshing.

At present, the Chinese mesona concentrated solution is obtained by extracting mesona to obtain mesona juice and then directly concentrating. The common extraction of the immortal grass juice adopts a traditional sodium alkali extraction method by boiling water, the sodium content of the product is high, so that the sodium intake of a human body is excessive, the risk of hypertension is increased, and the extracted aroma substances are incomplete, so that the aroma of the immortal grass cannot be maintained. The concentration is generally carried out by vacuum reduced pressure concentration, and the defect is that the aromatic substances of the Mesona chinensis Benth are completely lost along with the evaporation of water. The invention patent CN201711191367.6 discloses a preparation method of a Mesona chinensis Benth concentrated solution, which comprises the steps of firstly adopting an essential oil recovery device to collect volatile substances in the decocting and extracting process of Mesona chinensis Benth, then filtering the extracting solution, adopting an ultrafiltration ceramic membrane element to separate Mesona chinensis Benth polysaccharide gum from the extracting solution and other small molecule Mesona chinensis Benth flavor substances, and simultaneously concentrating the Mesona chinensis Benth polysaccharide gum, so that the problem of reduced aroma caused by vacuum reduced pressure concentration is solved, but the aroma substances comprise various components, water-soluble substances and fat-soluble substances, so that insufficient extraction is caused; and a plurality of components which are low in volatility and easy to pyrolyze can be dissipated in the water boiling process, so that the flavor substances in the mesona chinensis benth extracting solution are not retained to the maximum extent.

[ summary of the invention ]

In view of the above, the present invention provides a method for preparing a concentrated Mesona chinensis solution by using supercritical CO₂The extraction method combining extraction and water extraction can furthest retain flavor substances in the Mesona chinensis Benth extract and fully maintain the flavor of the Mesona chinensis Benth.

In order to solve the technical problems, the invention adopts the following technical scheme:

a preparation method of Mesona chinensis Benth concentrated solution comprises the following steps:

s1, raw material pretreatment: cutting Mesona chinensis Benth, and vacuum-sucking.

S2, extraction:

s21. supercritical CO₂Extracting, subjecting the pretreated Mesona chinensis to supercritical CO extraction₂Extracting, and performing supercritical extraction with ethanol as entrainer to obtain extractive solution and Mesona chinensis Benth residue.

S22, water extraction: and putting the Mesona chinensis Benth residue into a countercurrent extraction device, adding water, boiling, decocting for 2-5 h, and filtering to obtain a water extract.

S3, filtering: and mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate.

S4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution.

Preferably, in step S1, the negative pressure dust suction pressure is-1.5 to-2 MPa.

Preferably, the ethanol concentration is 85-95 wt%.

Preferably, the extraction pressure is 20-40 MPa, the extraction temperature is 35-50 ℃, the extraction time is 1-4 h, and CO is added₂The flow rate is 15-30L/h, and the dosage of ethanol is 0.5-1 mL/g.

Preferably, water is added according to the material-water ratio of 1: 10-20.

Preferably, in step S21, the water extraction is performed to obtain a water extract and a residue, and the residue is subjected to the second water extraction, and the water extractions of the two water extractions are combined.

Preferably, the molecular weight cut-off of the nanofiltration membrane is 400-600 daltons.

Preferably, the reverse osmosis membrane enrichment process is implemented by utilizing a two-stage reverse osmosis membrane system.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

1. the preparation method of the mesona chinensis benth concentrated solution adopts supercritical CO₂The extraction method combining extraction and water extraction can furthest retain flavor substances in the Mesona chinensis Benth extract and fully maintain the flavor of the Mesona chinensis Benth.

2. The preparation method of the mesona concentrated solution firstly adopts supercritical CO₂Extracting to get a solution at near room temperature and CO₂The gas is extracted under a cover, so that the heat is effectively preventedOxidation and dissipation of sensitive substances. Therefore, the effective components of the herbs are kept in the extract, and the high-boiling point, low-volatility and easily-pyrolyzed substances can be extracted at the temperature far lower than the boiling point of the substances. Then, water extraction is carried out under the boiling condition, the position which is difficult to extract is continuously extracted, fat-soluble aroma substances and water-soluble aroma substances can be completely extracted, and flavor substances in the mesona chinensis benth extracting solution are reserved to the maximum extent.

3. The preparation method of the Mesona chinensis Benth concentrated solution has the advantages that aromatic substances of Mesona chinensis Benth are not easy to lose through nanofiltration membrane filtration and membrane concentration processes.

[ detailed description ] embodiments

In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

Example 1

A preparation method of Mesona chinensis Benth concentrated solution comprises the following steps:

s1, raw material pretreatment: cutting Mesona chinensis Benth, and vacuum-sucking. The negative pressure dust collection pressure is-1.5 to-2 MPa.

S2, extraction:

s21. supercritical CO₂Extracting, subjecting the pretreated Mesona chinensis to supercritical CO extraction₂Extracting, and performing supercritical extraction with ethanol as entrainer to obtain extractive solution and Mesona chinensis Benth residue. The ethanol concentration was 90 wt%. The extraction pressure is 30MPa, the extraction temperature is 35 ℃, the extraction time is 3h, and CO is added₂The flow rate is 20L/h, and the dosage of the ethanol is 0.7 mL/g.

S22, water extraction: and putting the Mesona chinensis slag into a countercurrent extraction device, and adding water according to the material-water ratio of 1: 15. Adding water, boiling, decocting for 4 hr, and filtering to obtain water extractive solution.

S3, filtering: and mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate.

S4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution.

Example 2

A preparation method of Mesona chinensis Benth concentrated solution comprises the following steps:

s1, raw material pretreatment: cutting Mesona chinensis Benth, and vacuum-sucking. The negative pressure dust collection pressure is-1.5 to-2 MPa.

S2, extraction:

s21. supercritical CO₂Extracting, subjecting the pretreated Mesona chinensis to supercritical CO extraction₂Extracting, and performing supercritical extraction with ethanol as entrainer to obtain extractive solution and Mesona chinensis Benth residue. The ethanol concentration was 93 wt%. The extraction pressure is 30MPa, the extraction temperature is 45 ℃, the extraction time is 3h, and CO is added₂The flow rate is 20L/h, and the dosage of the ethanol is 0.8 mL/g.

S22, water extraction: and putting the Mesona chinensis slag into a countercurrent extraction device, and adding water according to the material-water ratio of 1: 15. Adding water, boiling for 2 hr, filtering to obtain primary water extractive solution and residue, extracting the residue with water for the second time to obtain secondary water extractive solution, and mixing the primary water extractive solution and the secondary water extractive solution to obtain water extract.

S3, filtering: and mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate. The molecular weight cut-off of the nanofiltration membrane is 400-600 daltons.

S4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution.

Example 3

A preparation method of Mesona chinensis Benth concentrated solution comprises the following steps:

s1, raw material pretreatment: cutting Mesona chinensis Benth, and vacuum-sucking. The negative pressure dust collection pressure is-1.5 to-2 MPa.

S2, extraction:

s21. supercritical CO₂Extracting, subjecting the pretreated Mesona chinensis to supercritical CO extraction₂Extracting, and performing supercritical extraction with ethanol as entrainer to obtain extractive solution and Mesona chinensis Benth residue. The ethanol concentration was 95 wt%. The extraction pressure is 40MPa, the extraction temperature is 40 ℃, the extraction time is 3h, and CO is added₂The flow rate is 30L/h, and the dosage of the ethanol is 1 mL/g.

S22, water extraction: and putting the Mesona chinensis slag into a countercurrent extraction device, and adding water according to the material-water ratio of 1: 10. Adding water, boiling for 2 hr, filtering to obtain primary water extractive solution and residue, extracting the residue with water for the second time to obtain secondary water extractive solution, and mixing the primary water extractive solution and the secondary water extractive solution to obtain water extract.

S3, filtering: and mixing the extract and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain a filtrate. The molecular weight cut-off of the nanofiltration membrane is 400-600 daltons.

S4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution. The reverse osmosis membrane enrichment process is to utilize a secondary reverse osmosis membrane system for enrichment.

Comparative example 1

A preparation method of Mesona chinensis Benth concentrated solution comprises the following steps:

s1, raw material pretreatment: cutting Mesona chinensis Benth, and vacuum-sucking. The negative pressure dust collection pressure is-1.5 to-2 MPa.

S2, extraction:

and putting the Mesona chinensis slag into a countercurrent extraction device, and adding water according to the material-water ratio of 1: 15. Adding water, boiling for 2 hr, filtering to obtain primary water extractive solution and residue, extracting the residue with water for the second time to obtain secondary water extractive solution, and mixing the primary water extractive solution and the secondary water extractive solution to obtain water extract.

S3, filtering: and mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate. The molecular weight cut-off of the nanofiltration membrane is 400-600 daltons.

S4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution.

Comparative example 2

A preparation method of Mesona chinensis Benth concentrated solution comprises the following steps:

s1, raw material pretreatment: cutting Mesona chinensis Benth, and vacuum-sucking. The negative pressure dust collection pressure is-1.5 to-2 MPa.

S2, supercritical CO₂Extracting, subjecting the pretreated Mesona chinensis to supercritical CO extraction₂Extracting with ethanol as entrainer by supercritical extraction to obtain extractive solution and extractGrass residue. The ethanol concentration was 93 wt%. The extraction pressure is 30MPa, the extraction temperature is 45 ℃, the extraction time is 3h, and CO is added₂The flow rate is 20L/h, and the dosage of the ethanol is 0.8 mL/g.

S3, filtering: and mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate. The molecular weight cut-off of the nanofiltration membrane is 400-600 daltons.

S4, concentrating: concentrating the filtrate with reverse osmosis membrane to obtain concentrated Mesona chinensis solution.

Comparative example 3

A preparation method of Mesona chinensis Benth concentrated solution comprises the following steps:

s1, raw material pretreatment: cutting Mesona chinensis Benth, and vacuum-sucking. The negative pressure dust collection pressure is-1.5 to-2 MPa.

S2, extraction:

s21. supercritical CO₂Extracting, subjecting the pretreated Mesona chinensis to supercritical CO extraction₂Extracting, and performing supercritical extraction with ethanol as entrainer to obtain extractive solution and Mesona chinensis Benth residue. The ethanol concentration was 93 wt%. The extraction pressure is 30MPa, the extraction temperature is 45 ℃, the extraction time is 3h, and CO is added₂The flow rate is 20L/h, and the dosage of the ethanol is 0.8 mL/g.

S22, water extraction: and putting the Mesona chinensis slag into a countercurrent extraction device, and adding water according to the material-water ratio of 1: 15. Adding water, boiling for 2 hr, filtering to obtain primary water extractive solution and residue, extracting the residue with water for the second time to obtain secondary water extractive solution, and mixing the primary water extractive solution and the secondary water extractive solution to obtain water extract.

S3, filtering: and mixing the extract liquor and the water extract to obtain an extract, and filtering by using a nanofiltration membrane to obtain filtrate. The molecular weight cut-off of the nanofiltration membrane is 400-600 daltons.

S4, concentrating: vacuum concentrating under reduced pressure.

And (3) experimental verification:

(1) the experimental method comprises the following steps: mesona chinensis concentrate was prepared by the methods of examples 1-3 and comparative examples 1-3.

(2) The test method comprises the following steps: the Baume degree, the concentration of the concentrated juice and the mouthfeel were measured, and the mouthfeel score was 10 points in total.

(3) As a result: see table 1 below.

TABLE 1 statistics of results

Group of	Baumei degree (degree)	Juice concentration (degree)	Mouthfeel scoring
				Example 1	5.5	10.8	9
Example 2	5.5	11.8	9
				Example 3	5.5	11.5	9
Comparative example 1	5.5	9.3	7
				Comparative example 2	5.5	9.5	7
Comparative example 3	5.5	10.3	7

As can be seen from Table 1, the juice concentrations of examples 1-3 were higher for the same Baume degrees, and comparative examples 1-3 used supercritical CO alone₂Extraction and water extraction, low juice concentration, incomplete extraction of aroma substances and low taste score.

Comparative example 3 the use of vacuum pressure reduction caused loss of aroma and therefore also affected the mouthfeel.

Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.