CN105477900A - Quality stability control method for traditional Chinese medicine hot reflux extraction concentration process - Google Patents
Quality stability control method for traditional Chinese medicine hot reflux extraction concentration process Download PDFInfo
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- CN105477900A CN105477900A CN201510918868.4A CN201510918868A CN105477900A CN 105477900 A CN105477900 A CN 105477900A CN 201510918868 A CN201510918868 A CN 201510918868A CN 105477900 A CN105477900 A CN 105477900A
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- 238000000034 method Methods 0.000 title claims abstract description 54
- 238000000605 extraction Methods 0.000 title claims abstract description 26
- 238000010992 reflux Methods 0.000 title claims abstract description 21
- 239000003814 drug Substances 0.000 title claims abstract description 20
- 238000001514 detection method Methods 0.000 claims abstract description 18
- 239000012141 concentrate Substances 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 13
- 238000012544 monitoring process Methods 0.000 claims abstract description 8
- 239000002904 solvent Substances 0.000 claims abstract description 6
- 239000000284 extract Substances 0.000 claims description 55
- 238000004821 distillation Methods 0.000 claims description 18
- 235000008216 herbs Nutrition 0.000 claims description 13
- 239000004480 active ingredient Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000012530 fluid Substances 0.000 claims description 7
- 239000000470 constituent Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- 238000003809 water extraction Methods 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 235000008100 Ginkgo biloba Nutrition 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- BOJKULTULYSRAS-OTESTREVSA-N Andrographolide Chemical compound C([C@H]1[C@]2(C)CC[C@@H](O)[C@]([C@H]2CCC1=C)(CO)C)\C=C1/[C@H](O)COC1=O BOJKULTULYSRAS-OTESTREVSA-N 0.000 description 2
- 241000050051 Chelone glabra Species 0.000 description 2
- 241000218628 Ginkgo Species 0.000 description 2
- 235000011201 Ginkgo Nutrition 0.000 description 2
- 239000009636 Huang Qi Substances 0.000 description 2
- ASLUCFFROXVMFL-UHFFFAOYSA-N andrographolide Natural products CC1(CO)C(O)CCC2(C)C(CC=C3/C(O)OCC3=O)C(=C)CCC12 ASLUCFFROXVMFL-UHFFFAOYSA-N 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 239000003651 drinking water Substances 0.000 description 2
- 235000020188 drinking water Nutrition 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 229930182478 glucoside Natural products 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
- 150000002338 glycosides Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- CJWQYWQDLBZGPD-UHFFFAOYSA-N isoflavone Natural products C1=C(OC)C(OC)=CC(OC)=C1C1=COC2=C(C=CC(C)(C)O3)C3=C(OC)C=C2C1=O CJWQYWQDLBZGPD-UHFFFAOYSA-N 0.000 description 2
- 235000008696 isoflavones Nutrition 0.000 description 2
- -1 isoflavones glucoside Chemical class 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 244000194101 Ginkgo biloba Species 0.000 description 1
- 239000009429 Ginkgo biloba extract Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 229940068052 ginkgo biloba extract Drugs 0.000 description 1
- 235000020686 ginkgo biloba extract Nutrition 0.000 description 1
- 150000002605 large molecules Chemical class 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0207—Control systems
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- Engineering & Computer Science (AREA)
- Automation & Control Theory (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a quality stability control method in a traditional Chinese medicine hot reflux extraction concentration process, which comprises the following steps: 1) adding the traditional Chinese medicine tablets and an extraction solvent into an extraction tank, starting an extraction program, wherein the extraction tank is also in through connection with a detection pool and a circulating pump, and a near-infrared detector detects the extracting solution in the detection pool in real time; 2) after extracting for a period of time, the extracting solution in the extracting tank enters a concentrating tank, and the condensate of the concentrating tank flows back to the extracting tank; 3) when the solid content and the effective component content of the extracting solution are lower than the set values, the hot reflux extraction is finished; 4) continuing to concentrate in the concentration tank, collecting the concentrated condensate into a condensate storage tank, transferring all the extracting solution into the concentration tank, and closing the valve; 5) and monitoring the density of the concentrated solution in real time by an online density sensor, and finishing concentration when the density reaches a set value. The invention can effectively ensure the control of the quality stability in the process of extracting and concentrating the traditional Chinese medicine by hot reflux and ensure the stability and the uniformity of the product quality among batches.
Description
Technical field
The present invention relates to field of traditional Chinese medicine pharmacy.More particularly, the present invention relates to a kind of Chinese medicine refluxing extraction concentration process quality stability control method.
Background technology
Extract the process active ingredient in Chinese medicine be dissolved out from plant tissue with suitable solvent exactly.Extraction time, to the quality affecting extract, as the time is too short, then can be caused the extraction of active ingredient incomplete, cause final products defective; As overlong time, then may cause the stripping of impurity, affect the quality of extract, finally cause product defective, considerably increase energy consumption simultaneously.
Circumfluence distillation is concentrated be by extractions with concentrate combined integrated, utilize the pressure reduction of extraction and concentration to realize Dynamic Extraction.Extract certain hour in circumfluence distillation concentration process after, extract is gone to concentration tank, concentration and evaporation produce steam through condensing reflux in extractor.Existing circumfluence distillation concentration process extracts terminal, the judgement of striking point all adopts artificial experience to judge, human error is large, and automaticity is low, can not ensure stability and the homogeneity of product quality.
Summary of the invention
An object of the present invention is to solve at least the problems referred to above and/or defect, and the advantage will illustrated at least is below provided.
A further object of the invention is by Chinese medicine refluxing extraction concentration process quality stability control method, the quick judgement to extraction, striking point can be realized, effective guarantee traditional Chinese herbs by thermal reflux extracts the control of concentration process quality stability, ensures stability and the homogeneity of final products.
In order to realize according to these objects of the present invention and other advantage, provide a kind of traditional Chinese herbs by thermal reflux and extract concentration process quality stability control method, it comprises the steps:
1) Chinese medicine tablet after only making and Extraction solvent is added to extractor, heating, open vacuum system, start circumfluence distillation program, start circumfluence distillation process, described extractor also through connection one detection cell and make extract fluid, circulating pump of flowing through sensing chamber, returning extractor bottom extractor, near infrared detector detects the extract in detection cell in real time;
2) through step 1) a period of time is extracted to described Chinese medicine tablet after, make the extract in extractor enter concentration tank, make the condensate liquid in concentration tank be back to extractor simultaneously;
3) when described near infrared detector detects the solid content of extract in detection cell and active constituent content lower than process set value, be judged to arrive circumfluence distillation terminal, the described circulating pump on closedown extractor and the condensate liquid in concentration tank are back to the valve of extractor;
4) concentration tank continues to concentrate extract, and concentrated condensed fluid collection is in condensate tank, and the extract in tank to be extracted is all transferred in concentration tank, closes the valve between extractor and concentration tank;
5) density of online density sensor Real-Time Monitoring concentrate concentration tank arranged, when density reaches process set value, is judged to reach striking point, closes concentration processes.
Preferably, wherein, step 2) in make extract enter concentration tank from extractor by liquid level difference or kinetic pump.
Preferably, wherein, described step 1) ~ 4) in vacuum all maintain-0.08 ~-0.04MPa, ensure Chinese medicine extraction at a lower temperature, Chinese medicine thermal sensitivity active ingredient is prevented to be damaged, and the stripping of large molecule inert matter, but consider financial cost, vacuum can not be too high.
Preferably, wherein, described Extraction solvent is water or ethanol, is respectively used to extract the water-soluble or alcohol soluble substance matter in Chinese medicine.
Preferably, wherein, the temperature of described water extraction is 50 ~ 100 DEG C, and the temperature of described alcohol extracting is 40 ~ 80 DEG C, to ensure the abundant extraction of Effective Component of Chinese Medicine.
Preferably, wherein, the temperature of described concentration step is 50 ~ 80 DEG C, has both ensured the effectively concentrated of Effective Component of Chinese Medicine, and turn avoid the too high destruction to active ingredient of temperature.
Preferably, wherein, step 3) described in the solid content setting value of circumfluence distillation terminal be 0.5 ~ 1g/L, the setting value of active ingredient is 0.1 ~ 0.5mg/L, generally, after the solid content of Chinese medicine and active ingredient reach described setting value respectively, extract hot reflux operation if proceed, not only the extraction efficiency of active ingredient is very low, and may can introduce invalid impurity on the contrary.
Preferably, wherein, described step 5) in the relative density of concentrate be 1.0 ~ 1.30g/ml, namely reach technique needs of subsequent operation, turn avoid and continue to concentrate the impact that product stability is caused and the higher financial cost brought.
The present invention at least comprises following beneficial effect:
(1) the present invention uses near infrared detector to carry out Real-Time Monitoring to the parameter such as solid content, active ingredient of the extract of extractor, avoid the shortcoming of conventional offline acquisition testing information delay, achieve the programme-controlled of production and automation, improve the control to extraction process;
(2) concentration tank of the present invention is provided with online density sensor and carries out Real-Time Monitoring to the density of concentrate, both ensure that the control to concentration technology, and the backtracking that also can be product quality provides necessary data reference;
(3) The present invention reduces the labour intensity of operating personnel, and avoid the error of artificial sample detecting, achieve the control to traditional Chinese medicine extraction concentration process quality stability, stability and homogeneity between improve batch, for improving tcm product steady quality and the modernization of Chinese medicine provides new technology.
Part is embodied by explanation below by other advantage of the present invention, target and feature, part also will by research and practice of the present invention by those skilled in the art is understood.
Accompanying drawing explanation
Fig. 1 is the schematic diagram that in one embodiment of the invention, traditional Chinese herbs by thermal reflux extracts concentration process quality stability control method.
In figure: 1, extractor, 2, concentration tank, 3, condenser, 4, condensate tank, 5, circulating pump, 6, detection cell, 7, near infrared detector, the 8, first valve, the 9, second valve, the 10, the 3rd valve, 11, online density sensor, 12, vacuum system.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention/invention is described in further detail, can implements according to this with reference to description word to make those skilled in the art.
Should be appreciated that used hereinly such as " to have ", other element one or more do not allotted in " comprising " and " comprising " term or the existence of its combination or interpolation.
Example 1:
Ginkgo leaf circumfluence distillation concentration process quality stability control method, comprises the steps:
1) with reference to Fig. 1, getting 300Kg ginkgo leaf drops in extractor 1, add 2400L drinking water, heating, opens vacuum system 12, start circumfluence distillation program, 80 DEG C, start circumfluence distillation process under vacuum-0.05Mpa, open circulating pump 5, make extract flow through detection cell 6 and get back in extractor 1, near infrared detector 7 detects extract in detection cell in real time, and Testing index is solid content and GINKGO BILOBA EXTRACT;
2) after extracting 30min, open the 3rd valve 10, extract in extractor 1 is because liquid level difference is from flowing in concentration tank 2, start concentration processes, the temperature of concentration tank controls at 70 ~ 80 DEG C, extract constantly enters in concentration tank 2, and concentrated condensate liquid is constantly back in extractor 1, realizes Dynamic Extraction;
3) when near infrared detector 7 detects the solid content of extract in detection cell 6 lower than 1g/L, or/and when active ingredient flavonoid of ginkgo biloba is lower than 0.5mg/L, then be judged to arrive circumfluence distillation terminal, close circumfluence distillation program, close the second valve 9, circulating pump 5 and near infrared detector 7;
4) concentration tank 2 continues to concentrate extract, and concentrated condensed fluid collection is in condensate tank 4, and the extract in tank 1 to be extracted is all transferred in concentration tank 2, closes the 3rd valve 10;
5) density of online density sensor 11 Real-Time Monitoring concentrate, when density reaches 1.15g/cm3, is judged to reach striking point, closes the first valve 8, concentrated end.
Example 2:
Radix Astragali circumfluence distillation concentration process quality stability control method, comprises the steps:
1) with reference to Fig. 1, get the 300Kg Radix Astragali to drop in extractor 1, add 2400L drinking water, after infiltrating half an hour, heating, open vacuum system, start circumfluence distillation program, 90 DEG C, vacuum-0.08Mpa starts circumfluence distillation process, open circulating pump 5, making extract flow through detection cell 6 gets back in extractor 1, and near infrared detector 7 detects extract in detection cell in real time, and Testing index is solid content and root of large-flowered skullcap first glycosides and Mao Rui isoflavones glucoside;
2) after extracting 2h, open the 3rd valve 10, extract in extractor 1 is squeezed in concentration tank 2 by kinetic pump, start concentration processes, the temperature of concentration tank controls at 65 ~ 75 DEG C, extract constantly enters in concentration tank 2, and concentrated condensate liquid is constantly back in extractor 1, realizes Dynamic Extraction;
3) when near infrared detector 7 detects the solid content of extract in detection cell 6 lower than 0.8g/L, or/and when the content of active ingredient root of large-flowered skullcap first glycosides and Mao Rui isoflavones glucoside is all lower than 0.3mg/L, then be judged to arrive circumfluence distillation terminal, close circumfluence distillation program, close the second valve 9, circulating pump 5 and near infrared detector 7;
4) concentration tank 2 continues to concentrate extract, and concentrated condensed fluid collection is in condensate tank 4, and the extract in tank 1 to be extracted is all transferred in concentration tank 2, closes the 3rd valve 10;
5) density of online density sensor 11 Real-Time Monitoring concentrate, when relative density reaches 1.0g/cm3, is judged to reach striking point, closes the first valve 8, concentrated end.
Example 3:
Herba Andrographitis circumfluence distillation concentration process quality stability control method, comprises the steps:
1) with reference to Fig. 1, getting 400Kg Herba Andrographitis drops in extractor 1, the volume fraction adding 2400L is the ethanol of 90%, and heating, opens vacuum system, start circumfluence distillation program, 50 DEG C, vacuum-0.06Mpa starts circumfluence distillation process, open circulating pump 5, make extract flow through detection cell 6 and get back in extractor 1, near infrared detector 7 detects extract in detection cell in real time, and Testing index is solid content and andrographolide;
2) after extracting 5h, open the 3rd valve 10, extract in extractor 1 is because liquid level difference is from flowing in concentration tank 2, start concentration processes, the temperature of concentration tank controls at 50 ~ 60 DEG C, extract constantly enters in concentration tank 2, and concentrated condensate liquid is constantly back in extractor 1, realizes Dynamic Extraction;
3) when near infrared detector 7 detects the solid content of extract in detection cell 6 lower than 0.5g/L, or/and when the content of active ingredient andrographolide is lower than 0.1mg/L, then be judged to arrive circumfluence distillation terminal, close circumfluence distillation program, close the second valve 9, circulating pump 5 and near infrared detector 7;
4) concentration tank 2 continues to concentrate extract, and concentrated condensed fluid collection is in condensate tank 4, and the extract in tank 1 to be extracted is all transferred in concentration tank 2, closes the 3rd valve 10;
5) density of online density sensor 11 Real-Time Monitoring concentrate, when relative density reaches 1.28g/cm3, is judged to reach striking point, closes the first valve 8, concentrated end.
Here the number of devices illustrated and treatment scale are used to simplify explanation of the present invention.The application of concentration process quality stability control method is extracted to traditional Chinese herbs by thermal reflux of the present invention, modifications and variations will be readily apparent to persons skilled in the art.
Although embodiment of the present invention are open as above, it is not restricted to listed in description and embodiment utilization.It can be applied to various applicable the field of the invention completely.For those skilled in the art, can easily realize other amendment.Therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the legend described.
Claims (8)
1. traditional Chinese herbs by thermal reflux extracts a concentration process quality stability control method, it is characterized in that, comprises the steps:
1) Chinese medicine tablet after only making and Extraction solvent is added to extractor, heat up, open vacuum system, start circumfluence distillation program, start circumfluence distillation process, described extractor also through connection one detection cell and make extract fluid, circulating pump of flowing through sensing chamber, returning extractor bottom extractor, near infrared detector detects the extract in detection cell in real time;
2) through step 1) a period of time is extracted to described Chinese medicine tablet after, make the extract in extractor enter concentration tank, make the condensate liquid of concentration tank be back to extractor simultaneously;
3) when described near infrared detector detects the solid content of extract in detection cell and active constituent content lower than process set value, be judged to arrive circumfluence distillation terminal, the described circulating pump on closedown extractor and the condensate liquid in concentration tank are back to the valve of extractor;
4) concentration tank continues to concentrate extract, and concentrated condensed fluid collection is in condensate tank, and the extract in tank to be extracted is all transferred in concentration tank, closes the valve between extractor and concentration tank;
5) density of online density sensor Real-Time Monitoring concentrate concentration tank arranged, when density reaches process set value, is judged to reach striking point, closes concentration processes.
2. traditional Chinese herbs by thermal reflux as claimed in claim 1 extracts concentration process quality stability control method, it is characterized in that, step 2) in make extract enter concentration tank from extractor by liquid level difference or kinetic pump.
3. traditional Chinese herbs by thermal reflux as claimed in claim 1 extracts concentration process quality stability control method, it is characterized in that, described step 1) ~ 4) in vacuum all maintain-0.08 ~-0.04MPa.
4. traditional Chinese herbs by thermal reflux as claimed in claim 1 extracts concentration process quality stability control method, and it is characterized in that, described Extraction solvent is water or ethanol.
5. traditional Chinese herbs by thermal reflux as claimed in claim 4 extracts concentration process quality stability control method, and it is characterized in that, the temperature of described water extraction is 50 ~ 100 DEG C, and the temperature of described alcohol extracting is 40 ~ 80 DEG C.
6. traditional Chinese herbs by thermal reflux as claimed in claim 1 extracts concentration process quality stability control method, it is characterized in that, the temperature of described concentration tank controls to be 50 ~ 80 DEG C.
7. traditional Chinese herbs by thermal reflux as claimed in claim 1 extracts concentration process quality stability control method, it is characterized in that, step 3) described in the solid content setting value of circumfluence distillation terminal be 0.5 ~ 1g/L, the setting value of active ingredient is 0.1 ~ 0.5mg/L.
8. traditional Chinese herbs by thermal reflux as claimed in claim 1 extracts concentration process quality stability control method, it is characterized in that, described step 5) in the relative density of concentrate be 1.0 ~ 1.30g/ml.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106770010A (en) * | 2016-12-15 | 2017-05-31 | 扬子江药业集团有限公司 | A kind of weisu granules extract solution concentration process On-line near infrared analyzer detection method |
| CN110003999A (en) * | 2019-03-25 | 2019-07-12 | 苏州优养健康科技有限公司 | A kind of camellia seed cleaning powder and its preparation process |
| CN110251608A (en) * | 2019-07-29 | 2019-09-20 | 云南大唐汉方制药股份有限公司 | A kind of extraction of Resina Draconis effective component and method of quality control |
| TWI672170B (en) * | 2018-11-29 | 2019-09-21 | 大榮生物科技股份有限公司 | Traditional chinese herbal medicine extraction device |
| CN110327655A (en) * | 2019-07-24 | 2019-10-15 | 杨晓燕 | A kind of amino acid concentration highly effective extraction method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106770010A (en) * | 2016-12-15 | 2017-05-31 | 扬子江药业集团有限公司 | A kind of weisu granules extract solution concentration process On-line near infrared analyzer detection method |
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| CN110003999B (en) * | 2019-03-25 | 2021-11-05 | 苏州优养健康科技有限公司 | Camellia seed cleaning powder and preparation process thereof |
| CN110327655A (en) * | 2019-07-24 | 2019-10-15 | 杨晓燕 | A kind of amino acid concentration highly effective extraction method |
| CN110251608A (en) * | 2019-07-29 | 2019-09-20 | 云南大唐汉方制药股份有限公司 | A kind of extraction of Resina Draconis effective component and method of quality control |
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Application publication date: 20160413 |