CN1813835A - Active constituent normal-temperature superhigh pressure extracting method from manyprickle acanthopanax material - Google Patents
Active constituent normal-temperature superhigh pressure extracting method from manyprickle acanthopanax material Download PDFInfo
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- CN1813835A CN1813835A CNA2005101190470A CN200510119047A CN1813835A CN 1813835 A CN1813835 A CN 1813835A CN A2005101190470 A CNA2005101190470 A CN A2005101190470A CN 200510119047 A CN200510119047 A CN 200510119047A CN 1813835 A CN1813835 A CN 1813835A
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- radix
- manyprickle acanthopanax
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Abstract
The present invention relates to a normal temperature ultrahigh pressure extraction method for extracting effective component from manyprickle acanthopanax raw material. Said method includes the following steps: drying manyprickle acanthopanax (leaf, slem and root), pretreating, pulverizing and sieving with 10-80 meshes, adding manyprickle acanthopanax powder into dilute ethyl alcohol solvent (whose concentration is 30%-70%) according to the solid-liquid ratio of 1 g:5-50 ml or hydrochloric (sulfuric) acid (whose concentration is 10-4-10-3M). after they are mixed and sealed, placing said mixture material in a high-pressure container, applying 50-600 MPa pressure at normal temperature, making extraction, retaining pressure for 1-30 min, releasing pressure, filtering to remove residue and collecting filtrate so as to obtain the extract containing effective component.
Description
(1) technical field
The present invention relates to a kind of from the Radix Et Caulis Acanthopanacis Senticosi raw material method of effective component extracting.Belong to biological technical field.
(2) background technology
Retrieve data bases such as " Chinese Chinese medicine bibliographic data base ", " Chinese patent searching system data base ", " Chinese pharmacy literature data base ", U.S PATENT DATABASE, MEDLINE data base, do not seen the report that the normal-temperature superhigh pressure extracting method of effective ingredient in the relevant Radix Et Caulis Acanthopanacis Senticosi raw material identical with this patent research is arranged.The research report that utilizes high-pressure microwave extraction method, atmospheric pressure reflux extraction method and soxhlet extraction to extract effective ingredient in the Chinese medicine Radix Et Caulis Acanthopanacis Senticosi raw material is arranged.Effective ingredient is better than the extracting method that these have been reported in the normal temperature high voltage extraction Radix Et Caulis Acanthopanacis Senticosi raw material but adopt, and has the advantage that extraction time is short, extraction ratio is high, extract is easy to the later separation purification.
(3) technology contents
(1) technical problem
Utilize high pressure technique effective component extracting from the Radix Et Caulis Acanthopanacis Senticosi raw material at room temperature, can reduce the production cost of effective ingredient, improve productive rate.
(2) technical scheme
The character faster that the present invention utilizes the dissolution equilibrium of the infiltration of solvent under the high pressure and solute to carry out, to be crushed to the pulverizing of 10 to 80 purpose Radix Et Caulis Acanthopanacis Senticosis is placed in the polythene film bag, add an amount of Diluted Alcohol, after sealing this polythene film bag is put into high-pressure bottle, pressurised extraction 1～30min, extract 1～3 time,, can obtain effective ingredient extractum behind the recovery ethanol extracting liquid filtering.
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) Manyprickle Acanthopanax Root is put into polythene film bag, add the Diluted Alcohol of enough submergence materials.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, sets enough pressure, extracts.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, decompression recycling ethanol promptly obtains effective ingredient extractum.
Illustrate:
(1) the Radix Et Caulis Acanthopanacis Senticosi raw material is root, stem and the leaf of Radix Et Caulis Acanthopanacis Senticosi.
(2) Radix Et Caulis Acanthopanacis Senticosi is through after pulverizing, and its surface area increases, and is big with the contact area of solvent, can accelerate the extraction rate of effective ingredient, if can increase the isolating difficulty of extracting liquid filtering but granularity is too little, can cross 40 mesh sieves after general the pulverizing and get final product.
(3) effective ingredient in the Radix Et Caulis Acanthopanacis Senticosi raw material is soluble in the Diluted Alcohol, and this solvent can be used as the solvent of effective ingredient high pressure extract.
(4) grade of high pressure extract pressure is 50～600MPa.
(5) time of high pressure extract is 1～30min, and this time is meant the dwell time, does not comprise boosting and the release time, boosts and the release time adds up to and is about 2min.
(6) for effective ingredient is as far as possible all extracted, can increase extraction time, experimental results show that when extraction time is 1～3 time, effective ingredient all to be extracted.
(7) effective ingredient is meant Saponin and flavone.
(8) effective ingredient that this extracting method extracted has following purposes:
A. can be used to develop various medicines (comprising: ball, sheet, cream, tincture, liquid drugs injection and injectable powder etc.);
B. can be used to develop various food, food additive and health product;
C. can be used to develop fine chemistry industry and various cosmetics.
(3) beneficial effect
(1) the extraction yield of high pressure extract method is higher, increases by 0.6% than ultrasonic extraction, and refluxing than water-bath increases by 1.7%.
(2) extraction time of high pressure extract method very short, only be 5 minutes.This has illustrated that fully the high pressure extract technology has high efficient in Radix Et Caulis Acanthopanacis Senticosi extracts active ingredients process, be any extracting method can not compare.
(3) reflux with respect to water-bath, impurity content is lower in the extracting solution of hyperpressure extraction, so not only can reduce the consumption of the used medicine of operation such as separation and purification in a large number, and has shortened the time that operations such as separation and purification take equipment.
(4) hyperpressure extraction carries out in room temperature, and extraction time is extremely short, can avoid some that heat sensitive effective ingredient is lost activity like this, and we will continue research this point in the experiment afterwards.
(5) research and the conclusion thereof about the Radix Et Caulis Acanthopanacis Senticosi technology for extracting effective component has universality, and other the extraction of Chinese medicine, food additive and cosmetics additive is all had reference value.
Therefore, the present invention can realize reducing greatly the target of Radix Et Caulis Acanthopanacis Senticosi production cost, has huge economic benefit and social benefit.
(4) specific embodiment
Embodiment 1
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 45% Diluted Alcohol.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 500MPa extracts, and extraction time is respectively 1,5 and 30min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Extraction time (min) | Extraction ratio (%) |
| 1 | 1 | 7.50 |
| 2 | 5 | 7.53 |
| 3 | 30 | 7.56 |
Embodiment 2
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 20 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 50% Diluted Alcohol.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 500MPa extracts, and extraction time is 5min, and material is extracted 1～3 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Extraction time (inferior) | Extraction ratio (%) |
| 1 | 1 | 7.73 |
| 2 | 2 | 7.71 |
| 3 | 3 | 7.74 |
Embodiment 3
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 30 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 55% Diluted Alcohol.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, respectively setting pressure be 50,300 and 600MPa extract, extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum is used gas chromatographic detection flavone extraction ratio.
| Sequence number | Extract pressure (MPa) | Extraction ratio (%) |
| 1 | 50 | 7.53 |
| 2 | 300 | 7.65 |
| 3 | 600 | 7.73 |
Embodiment 4
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 50 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, add 50,200 respectively, the Diluted Alcohol of 500ml.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 500MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Solvent volume (ml) | Extraction ratio (%) |
| 1 | 10 | 7.51 |
| 2 | 50 | 7.77 |
| 3 | 100 | 7.79 |
Embodiment 5
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, add the Diluted Alcohol (concentration is respectively 30%, 50%, 70%) of 50ml respectively.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Concentration of alcohol | Extraction ratio (%) |
| 1 | 30％ | 7.35 |
| 2 | 50％ | 7.66 |
| 3 | 70％ | 7.70 |
Embodiment 6
(1) Radix Et Caulis Acanthopanacis Senticosi raw material (root, stem and leaf) is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 30% Diluted Alcohol.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Raw material | Extraction ratio (%) |
| 1 | Root | 3.35 |
| 2 | Stem | 4.66 |
| 3 | Leaf | 7.57 |
Embodiment 7
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 70 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, add 50ml respectively, concentration is 10
-4, 10
-3.5, 10
-3The sulphuric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 100MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Sulfuric acid concentration | Extraction ratio (%) |
| 1 | 20％ | 2.33 |
| 2 | 40％ | 2.56 |
| 3 | 60％ | 2.78 |
Embodiment 8
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 60 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, add 50ml respectively, concentration is 10
-3The sulphuric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 100MPa extracts, and extraction time is 5min, extracts 1,2,3 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Number of times | Extraction ratio (%) |
| 1 | 1 | 2.31 |
| 2 | 2 | 2.52 |
| 3 | 3 | 2.74 |
Embodiment 9
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, (concentration is respectively 10 to add the hydrochloric acid of 50ml respectively
-4, 10
-3.5, 10
-3M).
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 400MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Concentration of hydrochloric acid | Extraction ratio (%) |
| 1 | 10 -4M | 2.05 |
| 2 | 10 -3.5M | 2.36 |
| 3 | 10 -3M | 2.60 |
Embodiment 10
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 40% ethanol.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, respectively setting pressure be 50,300 and 600MPa extract, extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Extract pressure | Extraction ratio (%) |
| 1 | 50 | 2.34 |
| 2 | 300 | 2.67 |
| 3 | 600 | 2.73 |
Embodiment 11
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, (concentration is respectively 10 to add the sulphuric acid of 50ml respectively
-4, 10
-3.5, 10
-3M).
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 500MPa extracts respectively, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Sulfuric acid concentration | Extraction ratio (%) |
| 1 | 10 -4M | 2.34 |
| 2 | 10 -3.5M | 2.62 |
| 3 | 10 -3M | 2.71 |
Embodiment 12
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-3The sulphuric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 1,5 and 30min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Extraction time (min) | Extraction ratio (%) |
| 1 | 1 | 2.45 |
| 2 | 5 | 2.76 |
| 3 | 30 | 2.80 |
Embodiment 13
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The hydrochloric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 1,5 and 30min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Extraction time (min) | Extraction ratio (%) |
| 1 | 1 | 2.25 |
| 2 | 5 | 2.56 |
| 3 | 30 | 2.60 |
Embodiment 14
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The hydrochloric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1,2,3 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
0
| Sequence number | Number of times | Extraction ratio (%) |
| 1 | 1 | 2.35 |
| 2 | 2 | 2.16 |
| 3 | 3 | 2.07 |
Embodiment 15
(1) Radix Et Caulis Acanthopanacis Senticosi raw material (root, stem and leaf) is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The dilute sulfuric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Raw material | Extraction ratio (%) |
| 1 | Root | 2.27 |
| 2 | Stem | 2.04 |
| 3 | Leaf | 2.01 |
Embodiment 16
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, (concentration is respectively 10 to add the sulphuric acid of 50ml respectively
-4, 10
-3.5, 10
-3M).
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Sulfuric acid concentration | Extraction ratio (%) |
| 1 | 30％ | 7.11 |
| 2 | 50％ | 7.23 |
| 3 | 70％ | 7.34 |
Embodiment 17
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, (concentration is respectively 10 to add the hydrochloric acid of 50ml respectively
-4, 10
-3.5, 10
-3M).
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Concentration of hydrochloric acid | Extraction ratio (%) |
| 1 | 30％ | 7.10 |
| 2 | 50％ | 7.25 |
| 3 | 70％ | 7.36 |
Embodiment 18
(1) Radix Et Caulis Acanthopanacis Senticosi raw material (root, stem and leaf) is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The dilute hydrochloric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Raw material | Extraction ratio (%) |
| 1 | Root | 2.21 |
| 2 | Stem | 2.01 |
| 3 | Leaf | 2.00 |
Embodiment 19
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-3.5The sulphuric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, respectively setting pressure be 50,300 and 600MPa extract, extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Extract pressure | Extraction ratio (%) |
| 1 | 50 | 2.12 |
| 2 | 300 | 2.31 |
| 3 | 600 | 2.53 |
Embodiment 20
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The hydrochloric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, respectively setting pressure be 50,300 and 600MPa extract, extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Extract pressure | Extraction ratio (%) |
| 1 | 50 | 2.20 |
| 2 | 300 | 2.43 |
| 3 | 600 | 2.51 |
Embodiment 21
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, add 50,200 respectively, 500ml concentration is 10
-4The M dilute sulfuric acid.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 500MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Solvent volume (ml) | Extraction ratio (%) |
| 1 | 10 | 2.23 |
| 2 | 50 | 2.31 |
| 3 | 100 | 2.45 |
Embodiment 22
(1) Radix Et Caulis Acanthopanacis Senticosi is pulverized, crossed 40 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, add 50,200 respectively, 500ml concentration is 10
-4The M dilute sulfuric acid.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 500MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Solvent volume (ml) | Extraction ratio (%) |
| 1 | 10 | 2.21 |
| 2 | 50 | 2.35 |
| 3 | 100 | 2.48 |
Embodiment 23
(1) Radix Et Caulis Acanthopanacis Senticosi raw material (root, stem and leaf) is pulverized, crossed 80 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The dilute hydrochloric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Raw material | Extraction ratio (%) |
| 1 | Root | 2.56 |
| 2 | Stem | 2.76 |
| 3 | Leaf | 2.35 |
Embodiment 24
(1) Radix Et Caulis Acanthopanacis Senticosi raw material (root, stem and leaf) is not pulverized.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The dilute hydrochloric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the Saponin extraction ratio with the visible spectrophotometry detection.
| Sequence number | Raw material | Extraction ratio (%) |
| 1 | Root | 1.73 |
| 2 | Stem | 1.54 |
| 3 | Leaf | 1.12 |
Embodiment 25
(1) Radix Et Caulis Acanthopanacis Senticosi raw material (root, stem and leaf) is pulverized, crossed 80 mesh sieves.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The dilute sulfuric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Raw material | Extraction ratio (%) |
| 1 | Root | 7.79 |
| 2 | Stem | 7.83 |
| 3 | Leaf | 7.96 |
Embodiment 26
(1) Radix Et Caulis Acanthopanacis Senticosi raw material (root, stem and leaf) is not pulverized.
(2) the 1g Manyprickle Acanthopanax Root is put into polythene film bag, adding 50ml concentration is 10
-4The dilute sulfuric acid of M.
(3) polythene film bag that Manyprickle Acanthopanax Root will be housed is put into high-pressure bottle, and setting pressure is that 300MPa extracts, and extraction time is 5min, extracts 1 time.
(4) after extraction is finished,, remove medicinal residues with extracting liquid filtering.
(5) filtrate is joined in the concentrator, the reclaim under reduced pressure organic solvent promptly obtains effective ingredient extractum.
(6) effective ingredient extractum can be got the flavone extraction ratio with the visible spectrophotometry detection.
| Sequence number | Raw material | Extraction ratio (%) |
| 1 | Root | 6.75 |
| 2 | Stem | 6.56 |
| 3 | Leaf | 6.18 |
Claims (4)
1. the method for an effective component extracting from the Radix Et Caulis Acanthopanacis Senticosi raw material is characterized in that this extracting method has the following steps:
A. pretreatment, fragmentation and preparation steps carry out raw material to prepare by a certain percentage and mix homogeneously with the extraction solvent after the pretreatment fragmentation;
B. seal step, the raw material of above-mentioned preparation and the mixture that extracts solvent are contained in high-pressure bottle after, seal this high-pressure bottle; Perhaps first sealed high-pressure vessel is introduced said mixture again;
C. the step of boosting at room temperature to above-mentioned high-pressure bottle pressurization, is elevated to pressure the predetermined pressure of 50MPa to 600MPa;
D. the pressurize step under above-mentioned predetermined pressure, keep-uped pressure 1～30 minute;
E. release step is unloaded above-mentioned high-pressure bottle and is depressed into normal pressure, takes out mixture in the container then.
According to claim 1 described a kind of from the Radix Et Caulis Acanthopanacis Senticosi raw material method of effective component extracting, it is characterized in that: the extraction that material to be processed and solvent are infiltrated capable effective ingredient.This extracting method has following feature:
A. the machined object pretreatment is become not pulverize or pulverize the back and cross 10 mesh sieve to 80 mesh sieves;
B. be 30%～70% ratio with pretreated machined object in the concentration of Diluted Alcohol solvent, perhaps (concentration is 10 in salt (sulfur) acid
-4～10
-3M) after mixed and the sealing, be seated in the airtight container;
C. in the pressure limit of 50～600MPa, can adopt batch (-type) to boost or directly boost;
D. be extracted in time of 1～30 minute and finish;
E. extraction time is generally 1～3 time.
According to claim 1 described a kind of from the Radix Et Caulis Acanthopanacis Senticosi raw material method of effective component extracting, this extracting method has following feature:
A. solid-to-liquid ratio is 1: 5～1: 100;
B. machined object is put into polythene film bag or other flexible containers;
C. extract flavone compound and oside compound.
4. according to claim 1, the effective ingredient that this extracting method extracted has following purposes:
A. can be used to develop various medicines;
B. can be used to develop various health product, food and food additive;
C. can be used to develop fine chemistry industry and various cosmetics.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005101190470A CN100484533C (en) | 2005-12-06 | 2005-12-06 | Active constituent normal-temperature superhigh pressure extracting method from manyprickle acanthopanax material |
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|---|---|---|---|
| CNB2005101190470A CN100484533C (en) | 2005-12-06 | 2005-12-06 | Active constituent normal-temperature superhigh pressure extracting method from manyprickle acanthopanax material |
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|---|---|
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| CN100484533C CN100484533C (en) | 2009-05-06 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103960384A (en) * | 2014-05-23 | 2014-08-06 | 天津华泰森淼生物工程技术股份有限公司 | Preparation method of ultrahigh-pressure strong tea capable of being brewed by cold water |
| CN104187653A (en) * | 2014-08-13 | 2014-12-10 | 张志科 | Composition, tea cream and application |
| CN107496472A (en) * | 2017-08-07 | 2017-12-22 | 武汉爱民制药股份有限公司 | A kind of method of ultra high pressure extraction otoginsenoside |
| CN108323663A (en) * | 2018-03-12 | 2018-07-27 | 大连军门保健食品有限公司 | A kind of Radix Et Caulis Acanthopanacis Senticosi polysaccharide health beverages and the method that Radix Et Caulis Acanthopanacis Senticosi polysaccharide is extracted in joining from slender acanthopanax |
-
2005
- 2005-12-06 CN CNB2005101190470A patent/CN100484533C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103960384A (en) * | 2014-05-23 | 2014-08-06 | 天津华泰森淼生物工程技术股份有限公司 | Preparation method of ultrahigh-pressure strong tea capable of being brewed by cold water |
| CN104187653A (en) * | 2014-08-13 | 2014-12-10 | 张志科 | Composition, tea cream and application |
| CN107496472A (en) * | 2017-08-07 | 2017-12-22 | 武汉爱民制药股份有限公司 | A kind of method of ultra high pressure extraction otoginsenoside |
| CN108323663A (en) * | 2018-03-12 | 2018-07-27 | 大连军门保健食品有限公司 | A kind of Radix Et Caulis Acanthopanacis Senticosi polysaccharide health beverages and the method that Radix Et Caulis Acanthopanacis Senticosi polysaccharide is extracted in joining from slender acanthopanax |
Also Published As
| Publication number | Publication date |
|---|---|
| CN100484533C (en) | 2009-05-06 |
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Assignee: Jilin Guotai super high pressure Biological Technology Co., Ltd. Assignor: Jilin University Contract fulfillment period: 2007.9.1 to 2013.9.1 contract change Contract record no.: 2009220000053 Denomination of invention: Active constituent normal-temperature superhigh pressure extracting method from manyprickle acanthopanax material Granted publication date: 20090506 License type: Exclusive license Record date: 2009.7.13 |
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