CN107793456A - Anthocyanidin of extraction purification and preparation method thereof from perilla leaf - Google Patents
Anthocyanidin of extraction purification and preparation method thereof from perilla leaf Download PDFInfo
- Publication number
- CN107793456A CN107793456A CN201711084195.2A CN201711084195A CN107793456A CN 107793456 A CN107793456 A CN 107793456A CN 201711084195 A CN201711084195 A CN 201711084195A CN 107793456 A CN107793456 A CN 107793456A
- Authority
- CN
- China
- Prior art keywords
- anthocyanidin
- perilla leaf
- extraction
- preparation
- perilla
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H17/00—Compounds containing heterocyclic radicals directly attached to hetero atoms of saccharide radicals
- C07H17/04—Heterocyclic radicals containing only oxygen as ring hetero atoms
- C07H17/06—Benzopyran radicals
- C07H17/065—Benzo[b]pyrans
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
- C07H1/08—Separation; Purification from natural products
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Saccharide Compounds (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
Anthocyanidin of extraction purification and preparation method thereof from perilla leaf, it belongs to plant component extraction technical field of purification.Present invention main component of the anthocyanidin of extraction purification from perilla leaf is the O glucosides of corn flower 3.The present invention includes the processing of perilla leaf, the configuration of extract solution, the extraction of anthocyanidin, the pretreatment of polymeric adsorbent, the intensive treatment of polymeric adsorbent, the purifying of anthocyanidin, the drying of anthocyanidin.The present invention is extracted using food-grade reagent alcohol, acetic acid, macroporous absorbent resin selective purification, and the elution of ethanol water reagent, product recovery rate is high, and anthocyanidin content is high.The macroporous absorbent resin that the present invention uses chooses, and effectively removes other impurities；The extracts reagent of use is safe and environment-friendly to be applicable to food industry.Gained anthocyanidin product color value is high, stability is good, and available for food and field of medicaments, process is simple, cost is cheap, is adapted to scale industrial production.
Description
Technical field
The invention belongs to plant component extraction technical field of purification；A kind of specific anthocyanidin of the extraction purification from perilla leaf
And preparation method thereof.
Background technology
Purple perilla, Labiatae annual herb plant, planted extensively in Asian countries, applied to edible and medicinal applications,
Through there is the long history of centuries.Purple perilla is one of integration of drinking and medicinal herbs kind that the Ministry of Public Health ratifies promulgation in the first batch, has been turned into China
A kind of Special plant resource.It can be divided into two kinds of chemical types of purple perilla and green Soviet Union, purple perilla generally according to the color difference purple perilla in footpath, leaf
The caused chemical type mainly due to antioxidation, anthocyanidin content is big, a kind of natural food colour can be used as to add
Agent, in China, purple perilla plantation is widely distributed.Green Soviet Union is equally containing abundant chemical composition, but Anthocyanins are less, mainly
Applied to field of food.The research of natural pigment is an extensive and active research field, current artificial synthesized food color
The food-safety problem that agent is brought increasingly is valued by people, due to introducing during chemical synthesis pigment production and possibility
A variety of toxic reagents are remained, reduce its edible safety performance.Anthocyanidin is a kind of conventional and safety natural plant pigment, with
Synthetic dyestuff is compared, not only edible safety, and is played in prevention nerve, angiocardiopathy, cancer and diabetes to pass weight
The effect wanted.Therefore, purple perilla anthocyanidin has the great potential of healthy pigment, by more and more in the research of different field
Attention.
At present, China conducts in-depth research for the extraction process of purple perilla anthocyanidin, such as publication number
A kind of perilla leaf extract and its extracting method, publication number CN105801391A are disclosed in CN104069172A Chinese patent
Chinese patent in disclose the method for purple perilla extraction perillaldehyde and anthocyanin, in publication number CN102964866A Chinese patent
The method that Perilla color is extracted from perilla leaf is disclosed, disclosing purple perilla in publication number CN105614446A Chinese patent carries
The preparation method of thing is taken, but the process route of above-mentioned document report is had cumbersome method, complex process, tried using toxic chemical
Agent, production cost is higher, food safety risk is higher, it is difficult to meets the needs of industrialized production.Therefore, based on current purple perilla color
The market demand of element, the manufacturing technique method cheap there is an urgent need to develop a kind of simple method, quality safety, cost.
The content of the invention
It is an object of the invention to provide a kind of anthocyanidin of the extraction purification from perilla leaf and preparation method thereof, this method
Simply, efficiently.
The present invention is achieved through the following technical solutions：
A kind of anthocyanidin of the extraction purification from perilla leaf, the anthocyanidin of the extraction purification from perilla leaf it is main
Composition is C-3-G, and the skeleton symbol of described C-3-G is C21H21ClO11。
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, comprises the following steps：
The processing of step 1, perilla leaf：The purple perilla maturity period gathers in purple perilla blade, and described purple perilla blade is in natural condition
Under dry or low temperature drying, crushing after it is stand-by；
The configuration of step 2, extract solution：Selection concentration is extracts reagent for 1~11% acetic acid, chooses absolute ethyl alcohol to carry
Reagent is taken, by described acetic acid and described ethanol according to volume ratio 1：1 ratio is well mixed, and obtains extract solution, stand-by；
The extraction of step 3, anthocyanidin：Weigh the perilla leaf sample that 1g steps 1 are handled well, be fitted into test tube, backward examination
The extract solution that addition 30mL steps 2 prepare in pipe, ultrasonic extraction, 30~40 DEG C of Extracting temperature of control, ultrasonic time 20~
40min, supersonic frequency 100Hz, being filtered after ultrasonic and complete once to extract, the extract solution renewed after suction filtration extracts 2~3 times again,
Filtrate is collected, it is stand-by；
The pretreatment of step 4, polymeric adsorbent：Macroporous absorbent resin is placed in 95% ethanol solution after soaking 24h, filter
Remove upper strata ethanol, resin washed with 95% ethanol solution, untill the ethanol flowed out occurs without white opacity, then with distillation
Water washs resin repeatedly, until without alcohol taste, it is stand-by；
Step 5, the intensive treatment of polymeric adsorbent：Macroporous absorbent resin after step 4 is handled is 5% in volume fraction
2~3h, filtering, with distilled water flushing resin until efflux is neutral, then by resin in mass fraction are soaked in hydrochloric acid solution
To soak 2~3h in 4% sodium hydroxide solution, filtering is stand-by with distilled water flushing resin until efflux is neutral；
The purifying of step 6, anthocyanidin：Step is added after the anthocyanidin extract solution that step 3 obtains is concentrated under reduced pressure into no alcohol taste
It is rapid 5 processing after macroporous absorbent resin, air concussion 12h, 25 DEG C of temperature, filter, collect macroreticular resin, using volume fraction as
50% ethanol water is eluant, eluent, elutes resin with 1mL/min elution rate, obtains eluent, stand-by；
The drying of step 7, anthocyanidin：After the eluent that step 6 is obtained is concentrated under reduced pressure into no alcohol taste, using cryogenic freezing
Dry or vacuum drying or near-infrared drying or microwave drying, obtain Perilla color powder.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, the perilla leaf after step 1 crushing
A diameter of 0.1~the 1mm of piece.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, the perilla leaf after step 1 crushing
Piece water content ＜ 5%.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, it is 7% that concentration is selected in step 2
Acetic acid be extracts reagent, described acetic acid is with described absolute ethyl alcohol according to volume ratio 1：1 ratio is well mixed, and is carried
Take liquid.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, 1g steps 1 place is weighed in step 3
The perilla leaf sample managed, is fitted into test tube, backward test tube in add the extract solution for preparing of 30mL steps 2, ultrasonic extraction,
35 DEG C, ultrasonic time 30min, supersonic frequency 100Hz of Extracting temperature is controlled, is filtered after ultrasound and completes once to extract, extract 2 again
It is secondary, merge and collect filtrate, obtain anthocyanidin extract solution.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, the macroporous absorption tree in step 4
Fat is one kind in NKA-II, D-101, DN-130, X-5, H-103, XAD16, XAD7HP resin.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, the macroporous absorption tree in step 4
Fat is XAD7HP resins.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, the drying temperature in step 7 is not
More than 40 DEG C.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, cyanine is calculated by PH differential methods
Cellulose content, cubage formula such as formula 1 and formula 2：
A=(A510-A700)PH1.0-(A510-A700)PH4.5
(2) wherein, MW is that the molecular weight 449.2g/mol, DF of anthocyanidin are extension rates, and ε is molar absorption coefficient
26900L/mol " cm, L are light length (1cm).
The preparation of buffer solution：PH1.0 buffer solution：1.49g KCl are weighed, are dissolved with distilled water, and are settled to 100mL,
Obtain the KCl solution that concentration is 0.02mol/L.Accurate 1.7mL concentrated hydrochloric acids of drawing are in 100mL volumetric flasks, and with distilled water constant volume
To graduation mark, the hydrochloric acid solution that concentration is 0.2mol/L is obtained.By 0.02mol/L KCl solution and 0.2mol/L hydrochloric acid solutions, with
Volume ratio is 25:67 ratio mixing, PH 4.5 buffer solution is produced with KCl solution tune PH (1.0 ± 0.1).Weigh 1.64g without
Water acetic acid sodium, is dissolved with distilled water, and is settled to 100mL, and PH (4.5 ± 0.1) is adjusted with hydrochloric acid.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, the content of OPC are
50%, the recovery rate of OPC is 5.3%.The preparation side of the anthocyanidin of the extraction purification of the present invention from perilla leaf
Method, the composition of anthocyanidin show the constituent analysis of C18 chromatographic columns anthocyanidin suitable for perilla leaf by lcms analysis, test,
Mobile phase acetonitrile-water is preferable for the separating effect of anthocyanidin, while shows that anthocyanidin is more stable in acid condition, so plus
Entering 0.05% formic acid improves peak type, and separating degree also improves simultaneously.Through being compared with standard items, the main component of anthocyanidin in perilla leaf
It is C-3-G (C21H21ClO11) (a), C-3-G (C21H21ClO11) (a) quality point
Number is 47%.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, meets natural pigment product
The exploitation of the market demand, particularly Perilla color product needs, and the present invention integrates existing pigment extraction and purification process method at present,
To solve Perilla color extraction purification problem in real work, it is proposed that a kind of simply and efficiently to prepare purple perilla anthocyanidin
Method.Present invention process has the advantages that simple to operate, low toxic and environment-friendly, product yield are high, especially in food coloring field side
Face has very big advantage.
The preparation method of the anthocyanidin of the extraction purification of the present invention from perilla leaf, there is peace compared with other method
Entirely, it is environmentally friendly；Macroporous absorbent resin selective adsorption capacity is strong, and the rate of recovery is high, and product purity is high, and resin is by the repeatable profit of regeneration
With reduction production cost；Isolation and purification method is simple, and environmental pollution is small, is adapted to scale industrial production.
Brief description of the drawings
Fig. 1 is the liquid chromatogram of described Anthocyanins after purification prepared by the method for embodiment one.
Embodiment
Embodiment one：
A kind of anthocyanidin of the extraction purification from perilla leaf, the anthocyanidin of the extraction purification from perilla leaf it is main
Composition is C-3-G, and the skeleton symbol of described C-3-G is C21H21ClO11。
Embodiment two：
The preparation method of the anthocyanidin of extraction purification from perilla leaf according to embodiment one, including it is as follows
Step：
The processing of step 1, perilla leaf：The purple perilla maturity period gathers in purple perilla blade, and described purple perilla blade is in natural condition
Under dry or low temperature drying, crushing after it is stand-by；
The configuration of step 2, extract solution：Selection concentration is extracts reagent for 7% acetic acid, chooses absolute ethyl alcohol and is tried for extraction
Agent, by described acetic acid water and described ethanol according to volume ratio 1：1 ratio is well mixed, and obtains extract solution, stand-by；
The extraction of step 3, anthocyanidin：Weigh the perilla leaf sample that 1g steps 1 are handled well, be fitted into test tube, backward examination
The extract solution that 30mL steps 2 prepare is added in pipe, ultrasonic extraction, controls 35 DEG C, ultrasonic time 30min of Extracting temperature, ultrasound
Frequency 100Hz, being filtered after ultrasonic and complete once to extract, the extract solution renewed after suction filtration extracts 2 times again, merges and collects filtrate,
It is stand-by；
The pretreatment of step 4, polymeric adsorbent：Macroporous absorbent resin is placed in 95% ethanol solution after soaking 24h, filter
Remove upper strata ethanol, resin washed with 95% ethanol solution, untill the ethanol flowed out occurs without white opacity, then with distillation
Water washs resin repeatedly, until without alcohol taste, it is stand-by；
Step 5, the intensive treatment of polymeric adsorbent：Macroporous absorbent resin after step 4 is handled is 5% in volume fraction
2h is soaked in hydrochloric acid solution, is filtered, with distilled water flushing resin until efflux is neutral, then is in mass fraction by resin
2h is soaked in 4% sodium hydroxide solution, is filtered, it is stand-by with distilled water flushing resin until efflux is neutral；
The purifying of step 6, anthocyanidin：Step is added after the anthocyanidin extract solution that step 3 obtains is concentrated under reduced pressure into no alcohol taste
It is rapid 5 processing after macroporous absorbent resin, air concussion 12h, 25 DEG C of temperature, filter, collect macroreticular resin, using volume fraction as
50% ethanol water is eluant, eluent, elutes resin with 1mL/min elution rate, obtains eluent, stand-by；
The drying of step 7, anthocyanidin：After the eluent that step 6 is obtained is concentrated under reduced pressure into no alcohol taste, using cryogenic freezing
Dry, obtain Perilla color powder.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the purple after step 1 crushing
A diameter of 0.1~the 1mm of perilla leaf piece.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the purple after step 1 crushing
Revive leaf water content ＜ 5%.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the macropore in step 4 are inhaled
Attached resin is XAD7HP resins.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, temperature is dried in step 7
Degree is no more than 40 DEG C.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, is calculated by PH differential methods
Anthocyanidin content, cubage formula such as formula 1 and formula 2：
A=(A510-A700)PH1.0-(A510-A700)PH4.5
(2) wherein, MW is that the molecular weight 449.2g/mol, DF of anthocyanidin are extension rates, and ε is molar absorption coefficient
26900L/mol " cm, L are light length (1cm).
The preparation of buffer solution：PH1.0 buffer solution：1.49g KCl are weighed, are dissolved with distilled water, and are settled to 100mL,
Obtain the KCl solution that concentration is 0.02mol/L.Accurate 1.7mL concentrated hydrochloric acids of drawing are in 100mL volumetric flasks, and with distilled water constant volume
To graduation mark, the hydrochloric acid solution that concentration is 0.2mol/L is obtained.By 0.02mol/L KCl solution and 0.2mol/L hydrochloric acid solutions, with
Volume ratio is 25:67 ratio mixing, PH 4.5 buffer solution is produced with KCl solution tune PH (1.0 ± 0.1).Weigh 1.64g without
Water acetic acid sodium, is dissolved with distilled water, and is settled to 100mL, and PH (4.5 ± 0.1) is adjusted with hydrochloric acid.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the content of OPC are
50%, the recovery rate of OPC is 5.3%.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the constituent analysis of anthocyanidin
For liquid-phase chromatographic analysis, analysis of spectra is as shown in Figure 1：Chromatographic condition, chromatographic column:Agilent ZorbaxSB-C18(4.6mm
× 150mm, 5.0 μm), mobile phase：0.05% aqueous formic acid (A)-acetonitrile (B), gradient elution (0-25min, 98%A →
60%A；25-40min, 60%A → 40%A；40-50min, 40%A → 5%A；50-60min, 5%A)；Flow velocity:0.5mL·
min-1；Column temperature:30℃；Sampling volume:20 μ L, wavelength 520nm.C18 chromatographic columns are used for the constituent analysis of anthocyanidin in perilla leaf,
Mobile phase acetonitrile-water is preferable for the separating effect of anthocyanidin, while shows that anthocyanidin is more stable in acid condition, so plus
Entering 0.05% formic acid improves peak type, and separating degree also improves simultaneously.Through being compared with standard items, the main component of anthocyanidin in perilla leaf
It is corn flower -3- p-Coumaric Acid glycoside -5- malonyl glucosides (a), corn flower -3- p-Coumaric Acid glycosides -5-
The mass fraction of malonyl glucoside (a) is 47%.
Embodiment three：
The preparation method of the anthocyanidin of extraction purification from perilla leaf according to embodiment one, including it is as follows
Step：
The processing of step 1, perilla leaf：The purple perilla maturity period gathers in purple perilla blade, and described purple perilla blade is in natural condition
Under dry or low temperature drying, crushing after it is stand-by；
The configuration of step 2, extract solution：Selection concentration is extracts reagent for 11% acetic acid, chooses absolute ethyl alcohol as extraction
Reagent, by described acetic acid water and described ethanol according to volume ratio 1：1 ratio is well mixed, and obtains extract solution, stand-by；
The extraction of step 3, anthocyanidin：Weigh the perilla leaf sample that 1g steps 1 are handled well, be fitted into test tube, backward examination
The extract solution that 30mL steps 2 prepare is added in pipe, ultrasonic extraction, controls 30 DEG C, ultrasonic time 40min of Extracting temperature, ultrasound
Frequency 100Hz, being filtered after ultrasonic and complete once to extract, the extract solution renewed after suction filtration extracts 2 times again, merges and collects filtrate,
It is stand-by；
The pretreatment of step 4, polymeric adsorbent：Macroporous absorbent resin is placed in 95% ethanol solution after soaking 24h, filter
Remove upper strata ethanol, resin washed with 95% ethanol solution, untill the ethanol flowed out occurs without white opacity, then with distillation
Water washs resin repeatedly, until without alcohol taste, it is stand-by；
Step 5, the intensive treatment of polymeric adsorbent：Macroporous absorbent resin after step 4 is handled is 5% in volume fraction
3h is soaked in hydrochloric acid solution, is filtered, with distilled water flushing resin until efflux is neutral, then is in mass fraction by resin
3h is soaked in 4% sodium hydroxide solution, is filtered, it is stand-by with distilled water flushing resin until efflux is neutral；
The purifying of step 6, anthocyanidin：Step is added after the anthocyanidin extract solution that step 3 obtains is concentrated under reduced pressure into no alcohol taste
It is rapid 5 processing after macroporous absorbent resin, air concussion 12h, 25 DEG C of temperature, filter, collect macroreticular resin, using volume fraction as
50% ethanol water is eluant, eluent, elutes resin with 1mL/min elution rate, obtains eluent, stand-by；
The drying of step 7, anthocyanidin：After the eluent that step 6 is obtained is concentrated under reduced pressure into no alcohol taste, using cryogenic freezing
Dry or vacuum drying or near-infrared drying or microwave drying, obtain Perilla color powder.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the purple after step 1 crushing
A diameter of 0.1~the 1mm of perilla leaf piece.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the purple after step 1 crushing
Revive leaf water content ＜ 5%.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, concentration is selected in step 2
Acetic acid for 7% is extracts reagent, and described acetic acid is with described absolute ethyl alcohol according to volume ratio 1：1 ratio is well mixed,
Obtain extract solution.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, 1g steps are weighed in step 3
The rapid 1 perilla leaf sample handled well, is fitted into test tube, backward test tube in add the extract solution for preparing of 30mL steps 2, ultrasound
Extraction, 35 DEG C, ultrasonic time 30min, supersonic frequency 100Hz of Extracting temperature is controlled, is filtered after ultrasound and completes once to extract, filtered
The extract solution renewed afterwards extracts 2 times again, merges and collects filtrate, obtains anthocyanidin extract solution.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the macropore in step 4 are inhaled
Attached resin is XAD7HP resins.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, temperature is dried in step 7
Degree is no more than 40 DEG C.
The preparation method of the anthocyanidin of extraction purification from perilla leaf described in present embodiment, the content of OPC are
47%, the recovery rate of OPC is the preparation of the anthocyanidin of extraction purification from perilla leaf described in 5.3% present embodiment
Method, the main component of anthocyanidin is C-3-G (C in perilla leaf21H21ClO11) (a), corn flower -3-O-
Glucoside (C21H21ClO11) (a) mass fraction be 46.8%.
Claims (9)
- A kind of 1. anthocyanidin of the extraction purification from perilla leaf, it is characterised in that：The described flower of extraction purification from perilla leaf The main component of blue or green element is C-3-G, and the skeleton symbol of described C-3-G is C21H21ClO11。
- A kind of 2. preparation method of the anthocyanidin of extraction purification from perilla leaf described in claim 1, it is characterised in that：Including Following steps：The processing of step 1, perilla leaf：The purple perilla maturity period gathers in purple perilla blade, and described purple perilla blade dries in the air under the conditions of naturally It is stand-by after dry or low temperature drying, crushing；The configuration of step 2, extract solution：Selection concentration is extracts reagent for 1~11% acetic acid, chooses absolute ethyl alcohol and is tried for extraction Agent, by described acetic acid and described ethanol according to volume ratio 1：1 ratio is well mixed, and obtains extract solution, stand-by；The extraction of step 3, anthocyanidin：Weigh the perilla leaf sample that 1g steps 1 are handled well, be fitted into test tube, backward test tube in The extract solution that 30mL steps 2 prepare is added, ultrasonic extraction, controls 30~40 DEG C, 20~40min of ultrasonic time of Extracting temperature, Supersonic frequency 100Hz, filtered after ultrasonic and complete once to extract, the extract solution renewed after suction filtration extracts 2~3 times again, collects filter Liquid, it is stand-by；The pretreatment of step 4, polymeric adsorbent：Macroporous absorbent resin is placed in 95% ethanol solution after soaking 24h, in elimination Layer ethanol, resin is washed with 95% ethanol solution, anti-untill the ethanol flowed out occurs without white opacity, then with distilled water Resin is washed in after backwashing, until without alcohol taste, it is stand-by；Step 5, the intensive treatment of polymeric adsorbent：Macroporous absorbent resin after step 4 is handled is in the hydrochloric acid that volume fraction is 5% Soak 2~3h in solution, filtering, with distilled water flushing resin until efflux is neutral, then by resin in mass fraction be 4% Sodium hydroxide solution in soak 2~3h, filtering is stand-by with distilled water flushing resin until efflux is neutral；The purifying of step 6, anthocyanidin：Step 5 place is added after the anthocyanidin extract solution that step 3 obtains is concentrated under reduced pressure into no alcohol taste Macroporous absorbent resin after reason, air concussion 12h, 25 DEG C of temperature, filter, macroreticular resin is collected, using volume fraction as 50% Ethanol water is eluant, eluent, elutes resin with 1mL/min elution rate, obtains eluent, stand-by；The drying of step 7, anthocyanidin：After the eluent that step 6 is obtained is concentrated under reduced pressure into no alcohol taste, using frozen drying Or vacuum drying or near-infrared drying or microwave drying, obtain Perilla color powder.
- 3. the preparation method of the anthocyanidin of the extraction purification according to claim 2 from perilla leaf, it is characterised in that：Step A diameter of 0.1~the 1mm of purple perilla blade after 1 crushing.
- 4. the preparation method of the anthocyanidin of the extraction purification according to claim 2 from perilla leaf, it is characterised in that：Step Purple perilla leaf water content ＜ 5% after 1 crushing.
- 5. the preparation method of the anthocyanidin of the extraction purification according to claim 2 from perilla leaf, it is characterised in that：Step Selection concentration is extracts reagent for 7% acetic acid in 2, and described acetic acid is with described absolute ethyl alcohol according to volume ratio 1：1 ratio Example is well mixed, obtains extract solution.
- 6. the preparation method of the anthocyanidin of the extraction purification according to claim 2 from perilla leaf, it is characterised in that：Step The perilla leaf sample that 1g steps 1 are handled well weighed in 3, be fitted into test tube, backward test tube in add 30mL steps 2 and prepare Extract solution, ultrasonic extraction, 35 DEG C, ultrasonic time 30min, supersonic frequency 100Hz of Extracting temperature is controlled, is filtered after ultrasound and completes one Secondary extraction, the extract solution renewed after suction filtration extract 2 times again, merge and collect filtrate, obtain anthocyanidin extract solution.
- 7. the preparation method of the anthocyanidin of the extraction purification according to claim 2 from perilla leaf, it is characterised in that：Step Macroporous absorbent resin in 4 is one kind in NKA-II, D-101, DN-130, X-5, H-103, XAD16, XAD7HP resin.
- 8. the preparation method of the anthocyanidin of the extraction purification according to claim 7 from perilla leaf, it is characterised in that：Step Macroporous absorbent resin in 4 is XAD7HP resins.
- 9. the preparation method of the anthocyanidin of the extraction purification according to claim 2 from perilla leaf, it is characterised in that：Step Drying temperature in 7 is no more than 40 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711084195.2A CN107793456A (en) | 2017-11-07 | 2017-11-07 | Anthocyanidin of extraction purification and preparation method thereof from perilla leaf |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711084195.2A CN107793456A (en) | 2017-11-07 | 2017-11-07 | Anthocyanidin of extraction purification and preparation method thereof from perilla leaf |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107793456A true CN107793456A (en) | 2018-03-13 |
Family
ID=61547402
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711084195.2A Pending CN107793456A (en) | 2017-11-07 | 2017-11-07 | Anthocyanidin of extraction purification and preparation method thereof from perilla leaf |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107793456A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108741071A (en) * | 2018-05-24 | 2018-11-06 | 中北大学 | A kind of preparation method of purple perilla anthocyanin microcapsules |
| CN109170886A (en) * | 2018-09-12 | 2019-01-11 | 陈晨 | A method of the extraction anthocyanidin content from purple rice shell can be improved |
| CN109507353A (en) * | 2019-01-04 | 2019-03-22 | 安徽农业大学 | The high-efficiency liquid chromatography method for detecting of anthocyanin in a kind of triticale wheat bran |
| CN110590730A (en) * | 2019-09-26 | 2019-12-20 | 浙江工商大学 | Method for extracting perilla leaf anthocyanin by using ternary eutectic solvent |
| WO2023285970A1 (en) | 2021-07-15 | 2023-01-19 | American Bioprocess Limitada | A process for the purification of anthocyanins and anthocyanidins from natural extracts using adsorption resins and acidified water as desorbent |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101041678A (en) * | 2007-04-27 | 2007-09-26 | 浙江工商大学 | Method for separating preparation of corn-flower pigment-3-amylaceum glycosides from red bayberry |
| CN100400535C (en) * | 2003-03-03 | 2008-07-09 | 三荣源有限公司 | Adiponectin expression promoter |
| CN101353362A (en) * | 2008-04-15 | 2009-01-28 | 天津市尖峰天然产物研究开发有限公司 | Extraction method of cyaniding 3-0-glucoside |
| CN101631836A (en) * | 2007-03-12 | 2010-01-20 | 国立大学法人香川大学 | Method for production of purified anthocyanin |
| CN106478579A (en) * | 2016-08-30 | 2017-03-08 | 浙江工业大学 | A kind of procyanidin extracting from fresh perilla stem and leaves and its application |
-
2017
- 2017-11-07 CN CN201711084195.2A patent/CN107793456A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100400535C (en) * | 2003-03-03 | 2008-07-09 | 三荣源有限公司 | Adiponectin expression promoter |
| CN101631836A (en) * | 2007-03-12 | 2010-01-20 | 国立大学法人香川大学 | Method for production of purified anthocyanin |
| CN101041678A (en) * | 2007-04-27 | 2007-09-26 | 浙江工商大学 | Method for separating preparation of corn-flower pigment-3-amylaceum glycosides from red bayberry |
| CN101353362A (en) * | 2008-04-15 | 2009-01-28 | 天津市尖峰天然产物研究开发有限公司 | Extraction method of cyaniding 3-0-glucoside |
| CN106478579A (en) * | 2016-08-30 | 2017-03-08 | 浙江工业大学 | A kind of procyanidin extracting from fresh perilla stem and leaves and its application |
Non-Patent Citations (4)
| Title |
|---|
| 崔丽霞等: "紫苏花色苷纯化工艺研究", 《食品科技》 * |
| 王金秋: "紫茄皮中花青素的提取、纯化及应用研究", 《中国优秀硕士论文学位论文全文数据库工程科技I辑》 * |
| 胡晓丹等: "紫苏甙的提取、纯化及丙二酰基紫苏宁的稳定性研究", 《食品工业科技》 * |
| 高宝昌等: "不同叶色紫苏花青素含量与成分研究", 《天然产物研究与开发》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108741071A (en) * | 2018-05-24 | 2018-11-06 | 中北大学 | A kind of preparation method of purple perilla anthocyanin microcapsules |
| CN109170886A (en) * | 2018-09-12 | 2019-01-11 | 陈晨 | A method of the extraction anthocyanidin content from purple rice shell can be improved |
| CN109507353A (en) * | 2019-01-04 | 2019-03-22 | 安徽农业大学 | The high-efficiency liquid chromatography method for detecting of anthocyanin in a kind of triticale wheat bran |
| CN110590730A (en) * | 2019-09-26 | 2019-12-20 | 浙江工商大学 | Method for extracting perilla leaf anthocyanin by using ternary eutectic solvent |
| CN110590730B (en) * | 2019-09-26 | 2021-09-03 | 浙江工商大学 | Method for extracting perilla leaf anthocyanin by using ternary eutectic solvent |
| WO2023285970A1 (en) | 2021-07-15 | 2023-01-19 | American Bioprocess Limitada | A process for the purification of anthocyanins and anthocyanidins from natural extracts using adsorption resins and acidified water as desorbent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107793456A (en) | Anthocyanidin of extraction purification and preparation method thereof from perilla leaf | |
| CN102229632B (en) | Preparation method of cyaniding-3-O-glucoside chloride | |
| CN101735646B (en) | Separation and extraction method of anthocyanin from purple sweet potato | |
| Yang et al. | Purification of anthocyanins from extracts of red raspberry using macroporous resin | |
| CN104829486B (en) | A kind of method extracting high-purity tea propylhomoserin from fresh tea leaf | |
| CN107325138A (en) | A kind of method of the main anthocyanin of four kinds of extraction separation and purification in pomace from blackcurrant | |
| CN103450703A (en) | Method for preparing high-purity taste-removing purple sweet potato pigment | |
| CN105418571B (en) | The method that black carrot anthocyanidin is extracted using microwave counter current | |
| CN104744489B (en) | Method for preparing high-purity oridonin by taking rabdosia rubescens as raw material | |
| CN103830306A (en) | Preparation method of honey suckle leaf effective extract product | |
| CN111346118B (en) | Method for subcritical water extraction and separation of ganoderma triterpene extract | |
| CN105153253A (en) | Purple sweet potato anthocyanin extraction process | |
| CN107827939A (en) | A kind of glucoside and preparation method thereof and its purposes | |
| CN104140909B (en) | A kind of rose flower wine and preparation method thereof | |
| CN107213180B (en) | Separation and extraction method of notoginseng flavone | |
| CN105434539A (en) | Composition of lotus flavones | |
| CN109053833A (en) | A method of Cy-3-G being prepared from mulberries using medium pressure liquid chromatography | |
| CN108997359A (en) | A method of chlorophyll is extracted from stevioside production waste residue | |
| CN105693675A (en) | A method of extracting flavonoid compounds from tagetes erecta | |
| CN107353296B (en) | A method of extracting activated protein and eurycomanone from Tongkat Ali | |
| CN107721857A (en) | A kind of method that high-purity chlorogenic acid is prepared from Gynura procumbens (Lour.) Merr | |
| CN104784231B (en) | A kind of method that flavone aglycone is obtained from gen-seng haulms | |
| KR101505311B1 (en) | Method to separate and purify vegetable ascorbic acid-2-glucoside from lycium chinense mill extract by utilizing the characteristics of sugar-binding protein | |
| CN104483431A (en) | Method for separating and purifying anthocyanin from blood-flesh peaches | |
| CN106770768B (en) | Separation and detection method of flavonoid glycoside compounds in fructus aurantii prepared in traditional Chinese medicine decoction pieces |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| WD01 | Invention patent application deemed withdrawn after publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20180313 |