CN108218692A - Utilize the method for cape jasmine fruit production crocetin - Google Patents
Utilize the method for cape jasmine fruit production crocetin Download PDFInfo
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- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
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Abstract
The invention discloses a kind of method using cape jasmine fruit production crocetin, step includes that cape jasmine fruit powder is broken, solvent extraction, and supernatant concentration removing organic solvent obtains concentrate A；Concentrate A is concentrated to give concentrate B through removal of impurities；It adds in lye to be cracked, obtains lysate C；Acid solution is added in, must be precipitated；Precipitation acid liquid continues to wash, and separation of solid and liquid obtains sediment；It is crocetin crude product after drying precipitate；Crocetin crude product is dissolved in removal of impurities in organic solvent, filtrate crystallisation, collects crystal, crystal washing and drying, obtains crocetin highly finished product.The production method simple process solves current crocetin raw materials for production price height, it can be achieved that industrialized production, and production stage is complicated, the problems such as seriously polluted.
Description
Technical field
The invention belongs to Biochemical Engineering technical fields, and in particular to a kind of method using cape jasmine fruit production crocetin.
Background technology
Crocetin（Crocetin）Also known as crocetin or bayer acid, it is safflower for red or kermesinus crystal
One of principle active component, exist in madder wort cape jasmine fruit.There is crocetin how unsaturated to be conjugated olefin(e) acid knot
Structure has protection liver, inhibits tumour, is anti-oxidant, improve anoxia endurance, improve a variety of pharmacological functions such as eyesight, belongs to doctor
It treats and is worth high drug, functional food and cosmetic material.
The Absorption And Metabolism result of study of crocetin and crocin in mouse small intestine shows that crocetin can be quickly
Blood circulation is rapidly absorbed into, and is present in blood plasma in the form of free state or glucuronide conjugate, is found simultaneously
Only crocetin and its glucuronide conjugate are detected in its blood plasma and crocin is not detected.This may be because
It is hydrolyzed to the reason of crocetin before intestinal absorption or in absorption process, by the safranine of intestinal absorption in Mice Body
Flower acid moieties are metabolized as single glucuronic acid or double glucuronide conjugates, crocetin and dimethyl crocetin tool
Have it is stronger suppression cancer, anti-cancer ability, mechanism may with crocetin have destroy tumour cell in DNA, RNA synthesis and
Its anti-oxidation function is related.The result shows that demutation early stage can inhibit tumour bad using crocetin treatment after hemorrhagic shock
The expression of necrosis factor (TNF-α and IL-1 β) m RNA, experimental bleeding can simultaneously be improved by improving the recovery of cell ATP after suffering a shock
Property shock survival rate.Crocetin can make in cancer Mice Body LPO and various metabolism enzyme levels restore normal, and can be with
The various pathological changes of cancer mouse is made to restore normal, so as to reduce the incidence of Swiss Albino mice lung cancer.Crocin, Tibetan
Safflower acid can inhibit the proliferation of thymocyte.In the evolution of Atheromatosis, vascular smooth muscle cells
Hyper-proliferative plays an important role, and a large amount of zoopery has proven to crocetin and makees with specific antiatherosclerosis
With.Crocetin can effective ox human arterial smooth muscle cells caused by inhibition angiotensin II proliferation, make cell
Cycle arrest is in the G0/G1 phases.Crocetin can also significantly inhibit extracellular signal-regulated kinase caused by angiotensinⅡ
The activation of ERK1/2, the activity aoxidized and intracellular superoxide dismutase can be improved of intracellular activation particle.Crocetin
It can prevent the apoptosis of the ox vascular endothelial cell (BEC) of angiotensins (AGEs) induction.This may can with crocetin
Reduce using AGEs as the formation of the reactive oxygen species of medium and improve intracellular Ca2+concentration it is related.Crocetin may be used also
To reduce T-CHOL and low-density lipoprotein white level in serum.Myocardial hypertrophy is a kind of overweight adaptability of heart long-term load
Reaction, is increased with cardiac muscle cell protein synthesis and cell volume increase is main feature.Research shows that crocetin can be significantly
The heart coefficient of rat model and left ventricle coefficient are reduced, and cardiac muscle cell's Na-K-A TP enzymes and mitochondria can be significantly improved
Ca2+Mg2 +The activity of ATP enzymes, while cardiac muscle cell's hydroxyprolin levels are reduced, crocetin is prompted to have and inhibits interstitial thin
Born of the same parents' collagen increases, and improves rat model remodeling ventricle.Intracellular energy (ATP and ADP) insufficient supply can cause mitochondria to damage
Wound, so as to cause Apoptosis even necrosis so as to cause hemorrhagic shock.Research shows that crocetin can increase cell
The diffusion of interior oxygen, and the storage of intraor extracellular energy can be improved, so as to reduce Apoptosis and improve depositing for hemorrhagic shock
Motility rate.Active oxygen (ROS) is considered as to cause a variety of nerve dysfunction disease (including Parkinson's disease) neuronal cells dead
The important biochemical reason died.Research in recent years finds that crocetin can protect neuronal cell from damage.It is taken to rat
After crocetin, the increased activity of various antioxidases in big substantia nigra, dopamine and its metabolite content improve, paddy
The sweet peptide of Guang and Thiobarbituric Acid Reactive Substance (TBARS) content reduce, and so as to protect neuronal cell from damage, play
Prevent the effect of Parkinson's disease and nerve dysfunction disease.Crocetin is to H2O2The hydroxy radical of system has stronger clear
Removing solid capacity, and liver homogenate autoxidation and Vc-Fe can be inhibited2+Lipid peroxidation caused by system hydroxy radical.Crocetin also has
There is anticoagulation inhibition thrombosis, and tool is resisted to the diabetes insulin of multiple models and is improved significantly.
From more than effect crocetin is can be seen that with preferable medicine prospect, but how efficiently to prepare crocetin
As key.Containing 10% or so crocetin in safflower, but safflower raw material（Main product it is Iranian）It is expensive, and Cape jasmine
Contain 0.5% or so saffron glucoside in sub- fruit（Crocetin can be converted into）, therefore, become using cape jasmine production crocetin
Research hotspot.
103539657 A data of publication of application 2014.01.29 of application publication number CN disclose a kind of Tibetan in cape jasmine source
The preparation method of safflower acid, includes the following steps：Extract cape jasmine raw material；Above-mentioned obtained powder is digested, adds in mixed enzyme；Alkali carries,
After enzymolysis, reactant hydrogen sodium hydroxide solution, stirring extraction 1h are added in, filtering has crude product precipitation, filters again, obtains content
More than 50% crocetin；Crystallization, the crocetin that will be obtained add in absolute ethyl alcohol, flow back 2 hours, cool crystallization, mistake
Up to the crocetin product of more than 95% content after filter drying.
102432455 A data of publication of application 2012.05.02 of application publication number CN, which are disclosed, a kind of prepares crocetin
With the method for crocin.This method includes preparing cape jasmine fruit extracting solution under Ultrasonic Conditions with ethyl alcohol, and extracting solution is concentrated to give
To medicinal extract.Medicinal extract is molten in polyethylene glycol solution, and then carrying out selective extraction with solvent obtains crocetin and safflower
Element.
Above-mentioned prior art has the following disadvantages：Preparation process is cumbersome, seriously polluted, yield is relatively low.The present invention carries thus
Specific production decision is gone out.
Invention content
The present invention provides a kind of methods using cape jasmine fruit production crocetin, and it is former to solve current crocetin production
Expect that price is high, production stage is complicated, seriously polluted problem.
To achieve the above object, the technical solution adopted by the present invention is：This produces the method for crocetin using cape jasmine fruit,
Include the following steps：
（1）Cape jasmine fruit powder is broken, is extracted added with solvent, separation of solid and liquid, and supernatant concentration removes organic solvent, obtains concentrate A；
（2）Concentrate A crosses macroreticular resin removal of impurities, and eluent is concentrated, and is removed eluant, eluent, is obtained concentrate B；
（3）Concentrate B adds in lye and is cracked, and obtains lysate C；
（4）Lysate C adds in acid solution, must precipitate；Precipitation acid liquid continues to wash, and separation of solid and liquid obtains sediment；
（5）It is crocetin crude product after drying precipitate；
（6）Crocetin crude product is dissolved in organic solvent, and filtered removal of impurities, filtrate crystallisation, collection crystal, crystal washing are dry
It is dry, crocetin highly finished product.
In said program：
Step（1）Middle organic solvent is methanol, ethyl alcohol, at least one of acetone solvent, solid-liquid ratio 1：5~30（Weight kg：
Volume L）；Extracting mode is extracted for heating stirring, any one mode in ultrasonic wave extraction, Microwave Extraction, adverse current extraction；Its
The middle temperature range for using heating extraction for 50~85 DEG C, preferably 60~75 DEG C, more select 70 DEG C, 2~5h of extraction time, preferably
3~4h, more preferable 3.5h；The ultrasonic power of ultrasonic wave extraction is 100~200W/L, preferably 150~180W/L, more preferable 160
W/L, preferably 1~3h of extraction time, 2~2.5h, more preferable 2.5h.
Step（1）Middle condensing mode is concentrated for vacuum-concentrcted or film, and wherein vacuum-concentrcted temperature control is 70
~85 DEG C.
Step（2）Model D101, D201 of middle macroreticular resin, D301, AB-8, NKA, D4020, HPD100,
Any one in HPD400, HPD500, HPD600.
Step（2）Middle eluant, eluent is at least one of water, methanol, ethyl alcohol, acetone solvent, and loading volume is column volume
1/5~1/3, preferably 1/4, eluting agent are 3~5 times, preferably 4 times of column volume.
Step（3）Middle lye is at least one of NaOH, KOH, and tune solution ph is 8~14, preferable ph 13, alkali
Solve 2~18h of time, preferably 6h, 20~95 DEG C of alkaline hydrolysis temperature, preferably 80 DEG C.
Step（4）Middle acid solution is formic acid, acetic acid, hydrochloric acid, lactic acid, phosphoric acid, at least one of, adjust solution ph for 3~
6th, preferable ph 5,1~10h of sedimentation time.
Step（5）Middle drying mode is freeze-drying, blast heating is dry, is spray-dried, ultrasonic wave drying.
The blast heating drying temperature control is at 40~60 DEG C, preferably 55 DEG C.
The spray drying EAT is 120~180 DEG C, preferably 150~170 DEG C, more preferable 165 DEG C；Go out wind-warm syndrome
Spend is 80~110 DEG C, preferably 95 DEG C.
The ultrasonic wave drying temperature is 20~30 DEG C；Ultrasonic intensity is 10~100W/cm2, vacuum impulse interval
Compare 5min：10min.
Step（6）Crocetin crude product is dissolved in organic solvent, wherein organic solvent is pyridine, in DMF, DMSO, methanol
At least one, solid-liquid ratio 1：10~1：50（Weight kg：Volume L）；Crystallization temperature is -5~-20 DEG C.
Crocetin product crude product purity >=50% prepared by said program, fine work purity are >=97.5%, production stage letter
Single, manufacturing cost is low, in production process the problem of non-pollution discharge.
Specific embodiment
Embodiment 1
（1）Cape jasmine fruit 100kg is crushed plus methanol extraction, solid-liquid ratio 1： 30（Weight kg：Volume L）, extracting mode for heating
Stirring extraction, the temperature range of heating extraction is 50~85 DEG C, preferably 60~75 DEG C, 70 DEG C more preferable, 2~5h of extraction time,
It is preferred that 3~4h, more preferable 3.5h；Separation of solid and liquid, supernatant concentration removing organic solvent, condensing mode is vacuum-concentrcted,
Thickening temperature control 70~85 DEG C, concentrate A；
（2）Concentrate A crosses the removal of impurities of D101 macroreticular resins, and loading volume is the 1/5~1/3, preferably 1/4 of column volume, and eluant, eluent is used
3~5 times for column volume, preferably 4 times are measured, eluant, eluent is ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in NaOH lye, and tune solution ph is 14, preferable ph 13, is cracked, alkaline hydrolysis time 6h, alkali
Solve 20~95 DEG C of temperature, preferably 80 DEG C, obtain lysate C；
（4）Lysate C adds in acetic acid acid solution, and it is 6 to adjust solution ph, and sedimentation time 10h must be precipitated；Precipitation acid liquid continues to wash
It washs, separation of solid and liquid obtains sediment；
（5）It is crocetin crude product after pellet frozen drying.Obtain 390 grams of crude product, purity 50%；
（6）Crocetin crude product is dissolved in organic solvent pyridine, solid-liquid ratio 1：10~1：50（Weight kg：Volume L）, cross filter out
Miscellaneous, filtrate crystallisation, crystallization temperature are -5~-20 DEG C, collect crystal, crystal washing and drying, obtain crocetin highly finished product.Obtain fine work
97.5 grams, purity 98%.
Embodiment 2
（1）Cape jasmine fruit 100kg is crushed plus EtOH Sonicate ripple extraction, ultrasonic power 200W/L, extraction time 2.5h, solid-liquid ratio
It is 1：20（Weight kg：Volume L）, separation of solid and liquid, supernatant concentration removing organic solvent, condensing mode is vacuum-concentrcted,
Thickening temperature control 75~85 DEG C, concentrate A；
（2）Concentrate A crosses the removal of impurities of AB-8 macroreticular resins, and loading volume is the 1/4 of column volume, and eluting agent is column volume
3 times, eluant, eluent is ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in KOH lye, and it is 13 to adjust solution ph, is cracked, alkaline hydrolysis time 3h, 85 DEG C of alkaline hydrolysis temperature,
Obtain lysate C；
（4）Lysate C adds in hydrochloric acid, and it is 4 to adjust solution ph, and sedimentation time 5h must be precipitated；Precipitation acid liquid continues to wash, Gu
Liquid detaches to obtain sediment；
（5）It is crocetin crude product after sediment is spray-dried.Spray drying EAT is 160 DEG C.
410 grams of crude product, purity 52%.
（6）Crocetin crude product is dissolved in DMF, solid-liquid ratio 1：50（Weight kg：Volume L）, filtering and impurity removing, filtrate crystallisation,
Crystallization temperature is -5~-20 DEG C, collects crystal, crystal washing and drying, obtains crocetin highly finished product.Obtain 100.5 grams of fine work, purity
It is 98.5%.
Embodiment 3
（1）Cape jasmine fruit 100kg is crushed, and adds acetone extraction, and extracting mode is Microwave Extraction, solid-liquid ratio 1：10（Weight kg：Volume
L）, separation of solid and liquid, supernatant concentration removing organic solvent, condensing mode is vacuum-concentrcted, wherein vacuum-concentrcted temperature
Degree control obtains concentrate A at 75 DEG C；
（2）Concentrate A crosses the removal of impurities of HPD100 macroreticular resins, and loading volume is the 1/5 of column volume, and eluting agent is column volume
5 times, eluant, eluent for water, ethyl alcohol, eluent carry out concentration removing eluant, eluent, obtain concentrate B；
（3）Concentrate B adds in NaOH lye, and it is 8 to adjust solution ph, is cracked, alkaline hydrolysis time 11h, 65 DEG C of alkaline hydrolysis temperature
DEG C, obtain lysate C；
（4）Lysate C adds in lactic acid acid solution, and it is 5 to adjust solution ph, and sedimentation time 6h must be precipitated；Precipitation acid liquid continues to wash
It washs, separation of solid and liquid obtains sediment；
（5）It is crocetin crude product after the drying of sediment ultrasonic wave.Ultrasonic wave drying temperature is 30 DEG C；Ultrasonic intensity is
100W/cm2, vacuum impulse interval compare 5min：10min.Obtain 399 grams of crude product, purity 51%.
（6）Crocetin crude product is dissolved in organic solvent DMSO, solid-liquid ratio 1：30（Weight kg：Volume L）, cross filter out
Miscellaneous, filtrate crystallisation, crystallization temperature are -20 DEG C, collect crystal, crystal washing and drying, obtain crocetin highly finished product.Obtain fine work 95
Gram, purity 97.8%.
Embodiment 4
（1）Cape jasmine fruit 100kg is crushed plus ethyl alcohol extraction, extracting mode are extracted for heating stirring, and the temperature range of heating extraction is
65 DEG C, extraction time 3.5h；Solid-liquid ratio is 1：15（Weight kg：Volume L）, separation of solid and liquid, supernatant concentration removing it is organic molten
Agent, condensing mode are vacuum-concentrcted, obtain concentrate A；
（2）Concentrate A crosses the removal of impurities of HPD400 macroreticular resins, and loading volume is the 1/3 of column volume, and eluting agent is column volume
4 times, eluant, eluent is ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in NaOH lye, and it is 13 to adjust solution ph, is cracked, alkaline hydrolysis time 4h, 55 DEG C of alkaline hydrolysis temperature,
Obtain lysate C；
（4）Lysate C adds in hydrochloric acid solution, and it is 3 to adjust solution ph, and sedimentation time 10h must be precipitated；Precipitation acid liquid continues to wash,
Separation of solid and liquid obtains sediment；
（5）It is crocetin crude product after the drying of sediment blast heating.Drying temperature is controlled at 40 DEG C.408 grams of crude product is obtained, it is pure
Spend is 53%.
（6）Crocetin crude product is dissolved in organic solvent DMF, solid-liquid ratio 1：40（Weight kg：Volume L）, cross filter out
Miscellaneous, filtrate crystallisation, crystallization temperature are -10 DEG C, collect crystal, crystal washing and drying, obtain crocetin highly finished product.Obtain fine work 101
Gram, purity 99.3%.
Embodiment 5
（1）Cape jasmine fruit 100kg is crushed, is added in the extraction of 75% ethyl alcohol, and extracting mode is ultrasonic wave extraction, ultrasonic power 230W/
L, extraction time 2.5h, solid-liquid ratio 1：30（Weight kg：Volume L）, separation of solid and liquid, supernatant concentration removing organic solvent, it is dense
Contracting mode is vacuum-concentrcted, and thickening temperature is 60 DEG C, obtains concentrate A；
（2）Concentrate A crosses the removal of impurities of HPD600 macroreticular resins, and loading volume is the 1/3 of column volume, and eluting agent is cylinder
Long-pending 5 times, eluant, eluent are ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in NaOH lye, and it is 12 to adjust solution ph, is cracked, alkaline hydrolysis time 6h, 75 DEG C of alkaline hydrolysis temperature,
Obtain lysate C；
（4）Lysate C adds in acetic acid acid solution, it is 3.5 to adjust solution ph, and sedimentation time 5h must be precipitated；Precipitate acid liquid after
Continuous washing, separation of solid and liquid obtain sediment；
（5）It is crocetin crude product after sediment spray drying.Spray drying EAT is 160 DEG C, leaving air temp 95
℃.Obtain 419 grams of crude product, purity 55%.
（6）Crocetin crude product is dissolved in organic solvent DMF, solid-liquid ratio 1：10~1：50（Weight kg：Volume L）, mistake
Filter out miscellaneous, filtrate crystallisation, crystallization temperature is -15 DEG C, collect crystal, crystal washing and drying, obtains crocetin highly finished product.It obtains smart
121 grams of product, purity 99.5%.
Embodiment 6
（1）Cape jasmine fruit 100kg is crushed plus the extraction of 50% ethyl alcohol, extracting mode are extracted for heating stirring, the temperature of heating extraction
Ranging from 65 DEG C, extraction time 4h；Solid-liquid ratio is 1：15 （Weight kg：Volume L）, separation of solid and liquid, supernatant concentration removing have
Solvent, condensing mode are vacuum-concentrcted, and the later stage concentrates for film, and wherein vacuum-concentrcted temperature control is 70~85
DEG C, concentrate A；
（2）Concentrate A crosses the removal of impurities of D4020 macroreticular resins, and loading volume is the 1/3 of column volume, and eluting agent is cylinder
Long-pending 3 times, eluant, eluent are ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in KOH lye, and it is 14 to adjust solution ph, is cracked, alkaline hydrolysis time 2h, alkaline hydrolysis temperature 95
DEG C, obtain lysate C；
（4）Lysate C adds in formic acid acid solution, and it is 4 to adjust solution ph, and sedimentation time 10h must be precipitated；Precipitation acid liquid continues to wash
It washs, separation of solid and liquid obtains sediment；
（5）It is crocetin crude product after sediment 100kg dryings.Ultrasonic wave drying temperature is 20 DEG C；Ultrasonic intensity is
50W/cm2, vacuum impulse interval compare 5min：10min.406 grams of crude product, purity 52%.
（6）Crocetin crude product is dissolved in organic solvent DMF, solid-liquid ratio 1：40（Weight kg：Volume L）, cross filter out
Miscellaneous, filtrate crystallisation, crystallization temperature are -5 DEG C, collect crystal, crystal washing and drying, obtain crocetin highly finished product.Obtain fine work 112
Gram, purity 97.5%.
Embodiment 7
（1）Cape jasmine fruit 100kg is crushed plus the extraction of 30% methanol, and extracting mode is ultrasonic wave extraction, ultrasonic power 150W/L,
Extraction time 1h, solid-liquid ratio 1：20（Weight kg：Volume L）, separation of solid and liquid, supernatant concentration removing organic solvent, concentration side
Formula is vacuum-concentrcted, wherein vacuum-concentrcted temperature control 70~85 DEG C, concentrate A；
（2）Concentrate A crosses the removal of impurities of HPD500 macroreticular resins, and loading volume is the 1/4 of column volume, and eluting agent is cylinder
Long-pending 3 times, eluant, eluent are ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in NaOH lye, and it is 8 to adjust solution ph, is cracked, alkaline hydrolysis time 18h, preferably 6h, alkaline hydrolysis temperature
50 DEG C of degree, obtains lysate C；
（4）Lysate C adds in hydrochloric acid acid solution, it is 6 to adjust solution ph, and sedimentation time 10h must be precipitated；Precipitate acid liquid after
Continuous washing, separation of solid and liquid obtain sediment；
（5）It is crocetin crude product after sediment freeze-drying.388 grams of crude product, purity 50%.
（6）Crocetin crude product is dissolved in organic solvent DMF, solid-liquid ratio 1：20（Weight kg：Volume L）, cross filter out
Miscellaneous, filtrate crystallisation, crystallization temperature are -20 DEG C, collect crystal, crystal washing and drying, obtain crocetin highly finished product.Obtain fine work 92
Gram, purity 98.3%.
Embodiment 8
（1）Cape jasmine fruit 100kg is crushed, is taken added with 80% second, and extracting mode is extracted for heating stirring, the temperature of heating extraction
Ranging from 70 DEG C, extraction time 3.5h；Solid-liquid ratio is 1：20（Weight kg：Volume L）, separation of solid and liquid, supernatant concentration removing
Organic solvent, condensing mode are vacuum-concentrcted, are concentrated into concentration of alcohol and are changed to be concentrated with film less than 10%, wherein vacuum subtracts
Press thickening temperature control 70~85 DEG C, concentrate A；
（2）Concentrate A crosses the removal of impurities of D301 macroreticular resins, and loading volume is the 1/3 of column volume, and eluting agent is cylinder
Long-pending 4 times, eluant, eluent are ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in NaOH lye, and it is 12 to adjust solution ph, is cracked, alkaline hydrolysis time 12h, preferably 6h, alkaline hydrolysis temperature
80 DEG C of degree, obtains lysate C；
（4）Lysate C adds in acetic acid acid solution, and it is 6 to adjust solution ph, and sedimentation time 10h must be precipitated；Precipitate acid liquid
Continue to wash, separation of solid and liquid obtains sediment；
（5）It is crocetin crude product after sediment spray drying.Spray drying EAT is 120 DEG C；Leaving air temp is 80
℃ .398 grams of crude product, purity 53%.
（6）Crocetin crude product is dissolved in organic solvent DMF, solid-liquid ratio 1：30 （Weight kg：Volume L）, cross filter out
Miscellaneous, filtrate crystallisation, crystallization temperature are -20 DEG C, collect crystal, crystal washing and drying, obtain crocetin highly finished product.Fine work 99
Gram, purity 98.9%.
Embodiment 9
（1）Cape jasmine fruit 100kg is crushed plus the extraction of 65% ethyl alcohol, extracting mode are extracted for heating stirring, the temperature of heating extraction
Ranging from 50 DEG C, 2 h of extraction time；Solid-liquid ratio is 1：20（Weight kg：Volume L）, separation of solid and liquid, supernatant concentration removing have
Solvent, condensing mode are vacuum-concentrcted, the control of vacuum-concentrcted temperature 70~85 DEG C, concentrate A；
（2）Concentrate A crosses the removal of impurities of HPD100 macroreticular resins, and loading volume is the 1/4 of column volume, and eluting agent is cylinder
Long-pending 4 times, eluant, eluent are ethyl alcohol, and eluent carries out concentration removing eluant, eluent, obtains concentrate B；
（3）Concentrate B adds in KOH lye, and it is 11 to adjust solution ph, is cracked, alkaline hydrolysis time 15h, preferably 6h, alkaline hydrolysis temperature
55 DEG C of degree, obtains lysate C；
（4）Lysate C adds in hydrochloric acid acid solution, and it is 6 to adjust solution ph, and sedimentation time 8h must be precipitated；Acid liquid is precipitated to continue
Washing, separation of solid and liquid obtain sediment；
（5）It is crocetin crude product after the drying of sediment ultrasonic wave.Ultrasonic wave drying temperature is 25 DEG C；Ultrasonic intensity is
80W/cm2, vacuum impulse interval compare 5min：10min.402 grams of crude product, purity 51%.
（6）Crocetin crude product is dissolved in organic solvent DMF methanol, solid-liquid ratio 1：30（Weight kg：Volume L）, mistake
Filter out miscellaneous, filtrate crystallisation, crystallization temperature is -20 DEG C, collect crystal, crystal washing and drying, obtains crocetin highly finished product.Fine work
103 grams, purity 99.5%.
The above, part specific embodiment only of the present invention, but protection scope of the present invention is not limited thereto, and is appointed
In the technical scope disclosed by the present invention, the change or replacement that can be readily occurred in should all be contained what those skilled in the art
Lid is within protection scope of the present invention.
Claims (9)
1. utilize the method for cape jasmine fruit production crocetin, which is characterized in that include the following steps：
（1）Cape jasmine fruit powder is broken, is extracted added with solvent, separation of solid and liquid, and supernatant concentration removes organic solvent, obtains concentrate A；
（2）Concentrate A crosses macroreticular resin removal of impurities, and eluent is concentrated, and is removed eluant, eluent, is obtained concentrate B；
（3）Concentrate B adds in lye and is cracked, and obtains lysate C；
（4）Lysate C adds in acid solution, must precipitate；Precipitation acid liquid continues to wash, and separation of solid and liquid obtains sediment；
（5）It is crocetin crude product after drying precipitate；
（6）Crocetin crude product is dissolved in organic solvent, filtering and impurity removing, filtrate crystallisation, collect crystal, crystal washing and drying,
Obtain crocetin highly finished product.
2. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（1）In have
Solvent is methanol, ethyl alcohol, at least one of acetone solvent, solid-liquid ratio 1：5~30（Weight kg：Volume L）；Extracting mode
Any one mode in being extracted for heating stirring extraction, ultrasonic wave extraction, Microwave Extraction or adverse current；Wherein use heating stirring
The temperature range of extraction is 50~85 DEG C, 2~5h of extraction time；The ultrasonic power of ultrasonic wave extraction is 100~200W/L, is extracted
1~3h of time.
3. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（1）In it is dense
Contracting mode is concentrated for vacuum-concentrcted or film, and wherein vacuum-concentrcted temperature control is at 70~85 DEG C.
4. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（2）In it is big
In model D101, D201, D301, AB-8, NKA, D4020, HPD100, HPD400, HPD500 or HPD600 of hole resin
Any one.
5. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（2）In wash
De- agent is water, at least one of methanol, ethyl alcohol, acetone solvent, and loading volume is the 1/5~1/3 of column volume, eluting agent
3~5 times for column volume.
6. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（3）Middle alkali
Liquid is at least one of NaOH, KOH, and it is 8~14 to adjust solution ph, 2~18h of alkaline hydrolysis time, 20~95 DEG C of alkaline hydrolysis temperature.
7. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（4）Middle acid
Liquid is at least one of formic acid, acetic acid, hydrochloric acid, lactic acid, phosphoric acid, and it is 3~6 to adjust solution ph, 1~10h of sedimentation time.
8. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（5）In do
Dry mode is freeze-drying, blast heating is dry, spray drying or ultrasonic wave are dried；Wherein, when being dried using blast heating, temperature
Degree control is at 40~60 DEG C；During using spray drying, inlet air temperature is 120~180 DEG C；Leaving air temp is 80~110 DEG C；Using
When ultrasonic wave is dried, temperature is 20~30 DEG C, and ultrasonic intensity is 10~100W/cm2, vacuum impulse interval compare 5min：
10min。
9. the method according to claim 1 using cape jasmine fruit production crocetin, which is characterized in that step（6）Middle institute
The organic solvent stated is pyridine, at least one of DMF, DMSO or methanol, solid-liquid ratio 1：10~1：50（Weight kg：Volume L）；
Crystallization temperature is -5~-20 DEG C.
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