CN108398401A - The extracting method of method of quality control and tanshin polyphenolic acid B in red sage root extract concentration process - Google Patents
The extracting method of method of quality control and tanshin polyphenolic acid B in red sage root extract concentration process Download PDFInfo
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- CN108398401A CN108398401A CN201810352110.2A CN201810352110A CN108398401A CN 108398401 A CN108398401 A CN 108398401A CN 201810352110 A CN201810352110 A CN 201810352110A CN 108398401 A CN108398401 A CN 108398401A
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- root extract
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- red sage
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- tanshin polyphenolic
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- 238000000034 method Methods 0.000 title claims abstract description 91
- 239000000284 extract Substances 0.000 title claims abstract description 85
- 239000002253 acid Substances 0.000 title claims abstract description 80
- 240000007164 Salvia officinalis Species 0.000 title claims abstract description 74
- 235000005412 red sage Nutrition 0.000 title claims abstract description 62
- 230000008569 process Effects 0.000 title claims abstract description 39
- 238000003908 quality control method Methods 0.000 title claims abstract description 32
- 238000000605 extraction Methods 0.000 claims description 22
- 238000005070 sampling Methods 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 235000017276 Salvia Nutrition 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000004497 NIR spectroscopy Methods 0.000 claims description 11
- 239000003153 chemical reaction reagent Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- 239000012445 acidic reagent Substances 0.000 claims description 4
- 238000012360 testing method Methods 0.000 claims description 4
- 235000021419 vinegar Nutrition 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- 239000000047 product Substances 0.000 abstract description 14
- 230000003647 oxidation Effects 0.000 abstract description 10
- 238000007254 oxidation reaction Methods 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 238000002329 infrared spectrum Methods 0.000 abstract description 7
- 239000012141 concentrate Substances 0.000 abstract description 6
- 238000012544 monitoring process Methods 0.000 abstract description 6
- 239000006227 byproduct Substances 0.000 abstract description 5
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 description 10
- 239000000463 material Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 7
- 230000008719 thickening Effects 0.000 description 6
- QAIPRVGONGVQAS-DUXPYHPUSA-N trans-caffeic acid Chemical compound OC(=O)\C=C\C1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-DUXPYHPUSA-N 0.000 description 6
- 238000001914 filtration Methods 0.000 description 5
- IANQTJSKSUMEQM-UHFFFAOYSA-N 1-benzofuran Chemical group C1=CC=C2OC=CC2=C1 IANQTJSKSUMEQM-UHFFFAOYSA-N 0.000 description 4
- 235000011135 Salvia miltiorrhiza Nutrition 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000008213 purified water Substances 0.000 description 4
- 244000132619 red sage Species 0.000 description 4
- PAFLSMZLRSPALU-MRVPVSSYSA-N (2R)-3-(3,4-dihydroxyphenyl)lactic acid Chemical compound OC(=O)[C@H](O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-MRVPVSSYSA-N 0.000 description 3
- ACEAELOMUCBPJP-UHFFFAOYSA-N (E)-3,4,5-trihydroxycinnamic acid Natural products OC(=O)C=CC1=CC(O)=C(O)C(O)=C1 ACEAELOMUCBPJP-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- PAFLSMZLRSPALU-QMMMGPOBSA-N Danshensu Natural products OC(=O)[C@@H](O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-QMMMGPOBSA-N 0.000 description 3
- PAFLSMZLRSPALU-UHFFFAOYSA-N Salvianic acid A Natural products OC(=O)C(O)CC1=CC=C(O)C(O)=C1 PAFLSMZLRSPALU-UHFFFAOYSA-N 0.000 description 3
- 229940074360 caffeic acid Drugs 0.000 description 3
- 235000004883 caffeic acid Nutrition 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- QAIPRVGONGVQAS-UHFFFAOYSA-N cis-caffeic acid Natural products OC(=O)C=CC1=CC=C(O)C(O)=C1 QAIPRVGONGVQAS-UHFFFAOYSA-N 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- SOXUSBQFIOBYJU-VPIXDIMLSA-N (2r)-2-[(e)-3-[2-[(e)-3-[(1r)-1-carboxy-2-(3,4-dihydroxyphenyl)ethoxy]-1-(3,4-dihydroxyphenyl)-3-oxoprop-1-en-2-yl]-3,4-dihydroxyphenyl]prop-2-enoyl]oxy-3-(3,4-dihydroxyphenyl)propanoic acid Chemical compound C([C@H](C(=O)O)OC(=O)\C=C\C=1C(=C(O)C(O)=CC=1)\C(=C/C=1C=C(O)C(O)=CC=1)C(=O)O[C@H](CC=1C=C(O)C(O)=CC=1)C(O)=O)C1=CC=C(O)C(O)=C1 SOXUSBQFIOBYJU-VPIXDIMLSA-N 0.000 description 2
- IBGBGRVKPALMCQ-UHFFFAOYSA-N 3,4-dihydroxybenzaldehyde Chemical compound OC1=CC=C(C=O)C=C1O IBGBGRVKPALMCQ-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- XLXWKULPMYZQSQ-UHFFFAOYSA-N Salvianolic acid E Natural products Cc1ccc(CC(OC(=O)C(=Cc2ccc(O)c(O)c2)c3c(O)c(O)ccc3C=CC(=O)OC(Cc4ccc(O)c(O)c4)C(=O)O)C(=O)O)cc1O XLXWKULPMYZQSQ-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000010931 ester hydrolysis Methods 0.000 description 2
- 238000004886 process control Methods 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- SNKFFCBZYFGCQN-VWUOOIFGSA-N salvianolic acid B Chemical compound C([C@H](C(=O)O)OC(=O)\C=C\C=1C=2[C@H](C(=O)O[C@H](CC=3C=C(O)C(O)=CC=3)C(O)=O)[C@H](OC=2C(O)=CC=1)C=1C=C(O)C(O)=CC=1)C1=CC=C(O)C(O)=C1 SNKFFCBZYFGCQN-VWUOOIFGSA-N 0.000 description 2
- 201000006474 Brain Ischemia Diseases 0.000 description 1
- 206010008120 Cerebral ischaemia Diseases 0.000 description 1
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical class OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 description 1
- 206010063837 Reperfusion injury Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 230000006907 apoptotic process Effects 0.000 description 1
- 210000001367 artery Anatomy 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 230000006652 catabolic pathway Effects 0.000 description 1
- 206010008118 cerebral infarction Diseases 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000006071 cream Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000003111 delayed effect Effects 0.000 description 1
- 238000006471 dimerization reaction Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 150000002240 furans Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- -1 more Preferably Substances 0.000 description 1
- 208000031225 myocardial ischemia Diseases 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 229960003371 protocatechualdehyde Drugs 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008439 repair process Effects 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- STCJJTBMWHMRCD-UHFFFAOYSA-N salvianolic acid B Natural products OC(=O)C(Cc1ccc(O)c(O)c1)OC(=O)C=Cc2cc(O)c(O)c3OC(C(C(=O)OC(Cc4ccc(O)c(O)c4)C(=O)O)c23)c5ccc(O)c(O)c5 STCJJTBMWHMRCD-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001225 therapeutic effect Effects 0.000 description 1
- 210000003556 vascular endothelial cell Anatomy 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/34—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having five-membered rings with one oxygen as the only ring hetero atom, e.g. isosorbide
- A61K31/343—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having five-membered rings with one oxygen as the only ring hetero atom, e.g. isosorbide condensed with a carbocyclic ring, e.g. coumaran, bufuralol, befunolol, clobenfurol, amiodarone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/537—Salvia (sage)
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/51—Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
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Abstract
A kind of method of quality control in red sage root extract concentration process, it is related to Chinese medicine production technology field, it uses near infrared spectrum to monitor red sage root extract on-line, to monitor the situation of change of red sage root extract tanshin polyphenolic acid B in concentration process in real time, foundation is provided for the further adjustment of concentration protocol, and then improves the quality of final products.Meanwhile this method effectively inhibits the degradation and oxidation of tanshin polyphenolic acid B, reduces interference of the by-product to the near infrared spectrum of tanshin polyphenolic acid B as far as possible, improve the accuracy of monitoring result by being further limited to concentration condition.A kind of extracting method of tanshin polyphenolic acid B, the extracting method have carried out accurate monitoring in real time in red sage root extract concentration process, to primary product tanshin polyphenolic acid B, have accomplished the controllable concentration of tanshin polyphenolic acid B, conducive to the tanshin polyphenolic acid B medicinal extract concentrate of high-quality high-purity is obtained.
Description
Technical field
The present invention relates to Chinese medicine production technology fields, in particular to the quality control in red sage root extract concentration process
The extracting method of method processed and tanshin polyphenolic acid B.
Background technology
Tanshin polyphenolic acid B (Lithospermic acid B) is one of phenolic acid class main component in red rooted salvia, and in Salvia miltiorrhiza
Content tops the list in material.Tanshin polyphenolic acid B has：To the protection of heart (to the protective effect of myocardial ischemia-reperfusion injury, micro- to heart
The Delayed Protection of vascular endothelial cell), to the protection (protective effect to cerebral ischemia) of brain and it is antitumor, to artery
The effects that preventive and therapeutic effect of atherosis, influence etc. to Apoptosis.
The structure of tanshin polyphenolic acid B is condensed and is formed by the danshensu of 3 molecules and the caffeic acid of 1 molecule, and there are two carboxyls for tool.
Its structure isTanshin polyphenolic acid B mostly be in the form of different salt existing for
(complex forms such as K+, Ca2+, Na+, NH4+), it is heated for a long time in high temperature, high alkalinity, hyperbaric environment, it is degradable and by
Oxidation.According to the literature：Danshensu, protocatechualdehyde, caffeic acid, alkannic acid, salvianolic acid E, purple are mainly generated after tanshin polyphenolic acid B degradation
Oxalic acid isomers (I, II, III), former alkannic acid and dimerization caffeic acid etc., wherein danshensu, alkannic acid is ester hydrolysis product, former youngster
Tea aldehyde is oxidation product, and salvianolic acid E is benzofuran open-loop products, according to the molecular structure of tanshin polyphenolic acid B, catabolite and each
The chemical constitution of product finds that tanshin polyphenolic acid B has degradation site at 3, is 2 ester bonds and 1 furan nucleus respectively, therefore infers that it is main
Degradation pathway includes two, and one is ester hydrolysis reaction, and another is benzofuran ring-opening reaction, and level-one catabolite is not
Stablize, the reactions such as hydrolysis, oxidation can further occur.
In the prior art, in tanshin polyphenolic acid B extracting method：It is that refluxing extraction is decocted using high temperature to obtain Salvia miltiorrhiza mostly
Liposoluble ingredient in material, such tanshin polyphenolic acid B heated for a long time degradable and oxidation, final rate of transform of tanshin polyphenolic acid B are very low；Salvia miltiorrhiza
Material component is more, complicated component, mutual dynamic conversion between ingredient, it is difficult to accomplish the maximization extraction of tanshin polyphenolic acid B, therefore cannot get height
Purity tanshin polyphenolic acid B.In tanshin polyphenolic acid B red sage root extract Concentrating Process Control：Domestic considerable enterprise is still with manually operated
Mode is produced, and labor intensity is big, and procedure parameter is difficult to record in time and correct control, product quality are difficult to control.Pass through
The automation of production process can not solve all problems of quality control in Chinese Traditional Medicine.Because automatic control system is only
To process control parameters (such as temperature, pressure, flow, density) rather than for the content of active ingredient in red sage root extract into
Row measures and takes corresponding control measure.
Invention content
The purpose of the present invention is to provide the method for quality control in a kind of red sage root extract concentration process, can be instant
The content for accurately measuring the tanshin polyphenolic acid B of red sage root extract after concentration, to preferably monitor concentration process.
Another object of the present invention is to provide a kind of extracting methods preparing tanshin polyphenolic acid B comprising above-mentioned Radix Salviae Miltiorrhizae extraction
Method of quality control in liquid concentration process, the extracting method is higher for the extraction efficiency of tanshin polyphenolic acid B, can obtain high-purity
Tanshin polyphenolic acid B medicinal extract concentrate.
What the embodiment of the present invention was realized in：
A kind of method of quality control in red sage root extract concentration process comprising：
By red sage root extract temperature be 50~90 DEG C, vacuum degree be -0.05~-0.08MPa under conditions of concentrated；
In concentration process, the red sage root extract after concentration is sampled, is measured and is calculated by near infrared spectroscopy
The content of tanshin polyphenolic acid B in collected sample.
A kind of extracting method of tanshin polyphenolic acid B comprising the method for quality control in above-mentioned red sage root extract concentration process.
The advantageous effect of the embodiment of the present invention is：
An embodiment of the present invention provides the method for quality control in a kind of red sage root extract concentration process, use near-infrared
Spectrum monitors red sage root extract on-line, to monitor the variation of red sage root extract tanshin polyphenolic acid B in concentration process in real time
Situation provides foundation for the further adjustment of concentration protocol, and then improves the quality of final products.Meanwhile this method pass through it is right
Concentration condition further limits, and effectively inhibits the degradation and oxidation of tanshin polyphenolic acid B, reduces by-product as far as possible to red phenol
The interference of the near infrared spectrum of sour B improves the accuracy of monitoring result.
The embodiment of the present invention additionally provides a kind of extracting method of tanshin polyphenolic acid B comprising above-mentioned red sage root extract is concentrated
Method of quality control in journey.The extracting method has carried out reality in red sage root extract concentration process, to primary product tanshin polyphenolic acid B
When accurately monitor, accomplished the controllable concentration of tanshin polyphenolic acid B, conducive to the tanshin polyphenolic acid B medicinal extract concentrate of high-quality high-purity is obtained.
Specific implementation mode
It in order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below will be in the embodiment of the present invention
Technical solution be clearly and completely described.The person that is not specified actual conditions in embodiment, builds according to normal condition or manufacturer
The condition of view carries out.Reagents or instruments used without specified manufacturer is the conventional production that can be obtained by commercially available purchase
Product.
Below to the method for quality control and tanshin polyphenolic acid B in a kind of red sage root extract concentration process of the embodiment of the present invention
Extracting method be specifically described.
An embodiment of the present invention provides the method for quality control in a kind of red sage root extract concentration process comprising：
S1. it is 50~90 DEG C in temperature by red sage root extract, vacuum degree carries out dense under conditions of being -0.05~-0.08MPa
Contracting.
Wherein, red sage root extract extracts to obtain using extracts reagent to red rooted salvia.Red rooted salvia can be
Fresh salvia miltiorrhiza after clean dry can also be the Radix Salviae Miltiorrhizae dry product directly bought on the market.Meanwhile in order to improve the effect of extraction
Rate can carry out crushing appropriate to red rooted salvia, increase its contact area with extracts reagent.Extracts reagent includes water and second
At least one of alcohol.Water and ethyl alcohol are tried as extraction using water and/or ethyl alcohol the preferable extracts reagent of human body compatibility
Agent will not cause any harm having residual even if in subsequent step to human body.Preferably, using water as extracts reagent, more
Preferably, water is to meet Chinese 2015 editions pharmacopeia purified waters.
Red rooted salvia and the mass ratio of extracts reagent are 1:10~20.Inventor has found by itself creative work, presses
When being extracted to Radix Salviae Miltiorrhizae according to aforementioned proportion, the medicinal ingredient being more advantageous in Radix Salviae Miltiorrhizae is dissolved into extracts reagent, the effect of extraction
Rate is higher.
The temperature that red rooted salvia extracts is 70~100 DEG C, and pH value is 2.5~5.5,1~2.5h of extraction time.Radix Salviae Miltiorrhizae
Main component in medicinal material is tanshin polyphenolic acid B, and tanshin polyphenolic acid B is in high temperature, high alkalinity, hyperbaric environment, heated for a long time, degradable
With aoxidized.Therefore the creative work for passing through inventor is found, is carried to red rooted salvia under lower temperature and acid condition
It takes, can effectively inhibit the degradation and oxidation of tanshin polyphenolic acid B, reduce the formation of by-product to the greatest extent, avoid the prison to follow-up tanshin polyphenolic acid B
Survey interferes.It further, can be by adding acid reagent, by red sage root extract in red rooted salvia extraction process
PH value is controlled in required range.Acid reagent includes at least one of hydrochloric acid and acetic acid.
For the same reason, in order to be likely to reduced the degradation and oxidation of tanshin polyphenolic acid B unexpectedly, inventor is in red sage root extract
Lower thickening temperature and lower concentration pressure are used in concentration process, to inhibit to the formation of by-product, into
Precision of the one step guarantee to the monitoring of tanshin polyphenolic acid B.
Method of quality control in a kind of red sage root extract concentration process that the embodiment of the present invention is provided further includes：
S2. in concentration process, the red sage root extract after concentration is sampled, is measured by near infrared spectroscopy
And calculate the content of tanshin polyphenolic acid B in collected sample.
Single-effect concentrator or dual-effect concentrator are used to the concentration of red sage root extract, for measuring the close red of near infrared spectrum
External linear light spectrometer is mounted on concentrator inner circulating tube road.Sampling to the red sage root extract after concentration includes multiple, phase
3~5min is spaced between adjacent double sampling.Further, it is that concentration is opened to the sampling time for the first time of the red sage root extract after concentration
10~20min after beginning.By multiple repairing weld, the content of tanshin polyphenolic acid B in the red sage root extract after concentration can be monitored in real time,
After it reaches required concentration, next process is transferred to.
Preferably, the test temperature of near infrared spectroscopy is 20~30 DEG C, and humidity is 30%~40%.To temperature and humidity
Control, influence of the environment to test result can be reduced as possible.Meanwhile it is preferable as a result, near-infrared exists in order to obtain precision
The scanning range of linear light spectrometer is 10000~4000cm-1, scanning times are 20~50 times, resolution ratio 8cm-1。
Further, the sample after detection can seal the preservation for carrying out the long period, as the later stage at 0~4 DEG C
Used in data check and Product recycling.
The embodiment of the present invention additionally provides a kind of extracting method of tanshin polyphenolic acid B comprising above-mentioned red sage root extract is concentrated
Method of quality control in journey, the extracting method is higher for the extraction efficiency of tanshin polyphenolic acid B, can obtain the danshinolic acid of high-purity
B medicinal extract concentrates.
The feature and performance of the present invention are described in further detail with reference to embodiments.
Embodiment 1
Present embodiments provide the method for quality control in a kind of red sage root extract concentration process comprising following steps：
S1. purified water 270L is added into extractor, opens stirring, heats the water to 80 DEG C with steam, is added suitable
Acid maintains the pH value 4.5 of liquid.The 15kg medicinal materials weighed up are put into extraction tank, the persistently stirring extraction at 80 DEG C of temperature
1h, filtering, obtains red sage root extract.
S2. above-mentioned red sage root extract is subjected to single-action concentration, 70 DEG C of thickening temperature, vacuum degree is -0.06MPa.It is concentrated into
Medicinal extract density is 1.10g/cm3.Sample detection content of danshinolic acid B in concentration process.
S3. after concentration starts 10min, first time sampling is carried out, it is later primary every 5min samplings, respectively by above-mentioned sample
It is measured by near infrared spectroscopy, and calculates the content of tanshin polyphenolic acid B in sample.
S4. the sample after detecting is sealed under 4 DEG C of environment and preserves for use.
Embodiment 2
Present embodiments provide the method for quality control in a kind of red sage root extract concentration process comprising following steps：
S1. purified water 300L is added into extractor, opens stirring, heats the water to 90 DEG C with steam, is added suitable
Acid maintains the pH value 3.5 of liquid.The 15kg medicinal materials weighed up are put into extraction tank, the persistently stirring extraction at 85 DEG C of temperature
1h, filtering, obtains red sage root extract.
S2. above-mentioned red sage root extract is subjected to single-action concentration, 80 DEG C of thickening temperature, vacuum degree is -0.07MPa.It is concentrated into
Medicinal extract density is 1.20g/cm3.Sample detection content of danshinolic acid B in concentration process.
S3. after concentration starts 20min, first time sampling is carried out, it is later primary every 5min samplings, respectively by above-mentioned sample
It is measured by near infrared spectroscopy, and calculates the content of tanshin polyphenolic acid B in sample.
S4. the sample after detecting is sealed under 4 DEG C of environment and preserves for use.
Embodiment 3
Present embodiments provide the method for quality control in a kind of red sage root extract concentration process comprising following steps：
S1. purified water 150L is added into extractor, opens stirring, heats the water to 95 DEG C with steam, is added suitable
Acid maintains the pH value 3.5 of liquid.The 15kg medicinal materials weighed up are put into extraction tank, the persistently stirring extraction at 90 DEG C of temperature
2h, filtering, obtains red sage root extract.
S2. above-mentioned red sage root extract is subjected to single-action concentration, 85 DEG C of thickening temperature, vacuum degree is -0.08MPa.It is concentrated into
Medicinal extract density is 1.15g/cm3.Sample detection content of danshinolic acid B in concentration process.
S3. after concentration starts 10min, first time sampling is carried out, it is later primary every 5min samplings, respectively by above-mentioned sample
It is measured by near infrared spectroscopy, and calculates the content of tanshin polyphenolic acid B in sample.
S4. the sample after detecting is sealed under 4 DEG C of environment and preserves for use.
Embodiment 4
Present embodiments provide the method for quality control in a kind of red sage root extract concentration process comprising following steps：
S1. ethyl alcohol 200L is added into extractor, opens stirring, ethyl alcohol is heated to 70 DEG C with steam, is added suitable
Acid maintains the pH value 2.5 of liquid.The 15kg medicinal materials weighed up are put into extraction tank, the persistently stirring extraction at 75 DEG C of temperature
2.5h, filtering, obtains red sage root extract.
S2. above-mentioned red sage root extract is subjected to single-action concentration, 50 DEG C of thickening temperature, vacuum degree is -0.05MPa.It is concentrated into
Medicinal extract density is 1.10g/cm3.Sample detection content of danshinolic acid B in concentration process.
S3. after concentration starts 10min, first time sampling is carried out, it is later primary every 3min samplings, respectively by above-mentioned sample
It is measured by near infrared spectroscopy, and calculates the content of tanshin polyphenolic acid B in sample.
S4. the sample after detecting is sealed under 0 DEG C of environment and preserves for use.
Embodiment 5
Present embodiments provide the method for quality control in a kind of red sage root extract concentration process comprising following steps：
S1. purified water 250L is added into extractor, opens stirring, heats the water to 80 DEG C with steam, is added suitable
Acid maintains the pH value 5.5 of liquid.The 15kg medicinal materials weighed up are put into extraction tank, the persistently stirring extraction at 80 DEG C of temperature
2h, filtering, obtains red sage root extract.
S2. above-mentioned red sage root extract is subjected to single-action concentration, 70 DEG C of thickening temperature, vacuum degree is -0.08MPa.It is concentrated into
Medicinal extract density is 1.20g/cm3.Sample detection content of danshinolic acid B in concentration process.
S3. after concentration starts 10min, first time sampling is carried out, it is later primary every 3min samplings, respectively by above-mentioned sample
It is measured by near infrared spectroscopy, and calculates the content of tanshin polyphenolic acid B in sample.
S4. the sample after detecting is sealed under 0 DEG C of environment and preserves for use.
The testing result of Examples 1 to 3 is as shown in table 1.
1. content of danshinolic acid B monitoring result of table
As can be seen from Table 1, the quality in a kind of red sage root extract concentration process that the embodiment of the present invention 1~3 is provided
Detection of the control method for content of danshinolic acid B can be as accurate as after decimal point 4, and measuring accuracy is higher.Meanwhile measuring number
According to growth at any time, preferable line style growing trend is showed, is illustrated in red sage root extract concentration process, the drop of tanshin polyphenolic acid B
Solution and oxidation have obtained preferable inhibition, and the efficient concentration of tanshin polyphenolic acid B may be implemented, conducive to the tanshin polyphenolic acid B leaching of high-purity is obtained
Cream concentrate.
In conclusion an embodiment of the present invention provides the method for quality control in a kind of red sage root extract concentration process,
Red sage root extract is monitored on-line using near infrared spectrum, to monitor red sage root extract red phenol in concentration process in real time
The situation of change of sour B provides foundation for the further adjustment of concentration protocol, and then improves the quality of final products.Meanwhile the party
Method effectively inhibits the degradation and oxidation of tanshin polyphenolic acid B, reduces by-product as far as possible by being further limited to concentration condition
Interference of the object to the near infrared spectrum of tanshin polyphenolic acid B, improves the accuracy of monitoring result.
The embodiment of the present invention additionally provides a kind of extracting method of tanshin polyphenolic acid B comprising above-mentioned red sage root extract is concentrated
Method of quality control in journey.The extracting method has carried out reality in red sage root extract concentration process, to primary product tanshin polyphenolic acid B
When accurately monitor, accomplished the controllable concentration of tanshin polyphenolic acid B, conducive to the tanshin polyphenolic acid B medicinal extract concentrate of high-quality high-purity is obtained.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. the method for quality control in a kind of red sage root extract concentration process, which is characterized in that including：
By red sage root extract temperature be 50~90 DEG C, vacuum degree be -0.05~-0.08MPa under conditions of concentrated；
In concentration process, the red sage root extract after concentration is sampled, is measured and is calculated by near infrared spectroscopy
The content of tanshin polyphenolic acid B in collected sample.
2. method of quality control according to claim 1, which is characterized in that adopting for the red sage root extract after concentration
Sample includes multiple, and 3~5min is spaced between adjacent double sampling.
3. method of quality control according to claim 2, which is characterized in that when to the sampling for the first time of the red sage root extract
Between for concentration start after 10~20min.
4. method of quality control according to claim 3, which is characterized in that the test temperature of the near infrared spectroscopy is
20~30 DEG C, humidity is 30%~40%.
5. method of quality control according to claim 4, which is characterized in that the scanning range of the near infrared spectroscopy is
10000~4000cm-1, scanning times are 20~50 times, resolution ratio 8cm-1。
6. method of quality control according to claim 1, which is characterized in that the red sage root extract is to use extracts reagent
Red rooted salvia is extracted, the extracts reagent includes at least one of water and ethyl alcohol.
7. method of quality control according to claim 6, which is characterized in that be 70 to the temperature that red rooted salvia extracts
~100 DEG C, pH value is 2.5~5.5,1~2.5h of extraction time.
8. method of quality control according to claim 7, which is characterized in that during being extracted to red rooted salvia,
By adding acid reagent, the pH value of the red sage root extract is controlled 2.5~5.5；The acid reagent includes hydrochloric acid and vinegar
At least one of acid.
9. method of quality control according to claim 1, which is characterized in that the red rooted salvia and the extracts reagent
Mass ratio is 1:10~20.
10. a kind of extracting method of tanshin polyphenolic acid B, which is characterized in that carried including such as claim 1~9 any one of them Radix Salviae Miltiorrhizae
Take the method for quality control in liquid concentration process.
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