CN111704598A - Method for extracting anthocyanin from Chinese yam root bark - Google Patents
Method for extracting anthocyanin from Chinese yam root bark Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D311/00—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
- C07D311/02—Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
- C07D311/04—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring
- C07D311/58—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4
- C07D311/60—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2
- C07D311/62—Benzo[b]pyrans, not hydrogenated in the carbocyclic ring other than with oxygen or sulphur atoms in position 2 or 4 with aryl radicals attached in position 2 with oxygen atoms directly attached in position 3, e.g. anthocyanidins
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a method for extracting anthocyanin from dioscorea opposita root bark, and belongs to the technical field of preparation of natural anthocyanin from plants. The method for extracting anthocyanin from Chinese yam root bark comprises the following steps: drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb; soaking the Chinese yam rhizome peel powder twice with acidic methanol and carrying out ultrasonic extraction, combining the extracting solutions, concentrating and drying to obtain the Chinese yam rhizome peel anthocyanin. The method for extracting anthocyanin from the dioscorea opposita root bark has the advantages of mild extraction conditions, simple and convenient operation method, easy recovery of solvent, easy large-scale production and the like, and can solve the problem of root bark waste generated in the processing process of dioscorea opposita decoction pieces.
Description
Technical Field
The invention belongs to the technical field of preparation of plant-derived natural anthocyanin, and particularly relates to a method for extracting anthocyanin from root bark of dioscorea opposita.
Background
The anthocyanin is an important flavonoid metabolite of the plant, mainly exists in a cell vacuole in a glycoside form, so that flowers and fruits show different colors, and has important physiological functions of attracting insects to pollinate and spread seeds, preventing the plant from being damaged by ultraviolet light and the like. Meanwhile, the anthocyanin also has the health-care functions of resisting oxidation and mutation, removing free radicals, preventing cancers, inflammations, cardiovascular diseases and the like, and is a well-known chemical component beneficial to human health. There are more than 20 natural anthocyanins currently known, the main 6 of which are cyanidin, pelargonidin, delphinidin, peonidin, morning glory pigment and malvidin. Anthocyanins in their native state are mainly present in the glycoside form, called anthocyanins, and less in the free form. Anthocyanins can be used for coloring food, and can also be used in dye, medicine, and cosmetic.
Cyanidin (cyanidin) has the following chemical structure:
rhizoma Dioscoreae is Dioscoreaceae (Dioscoreaceae)Dioscorea oppositeThunb.) is a medicinal material in the river south, has the effects of tonifying spleen and nourishing stomach, promoting the production of body fluid and benefiting lung, tonifying kidney and arresting seminal emission, and is clinically used for treating spleen deficiency and poor appetite, chronic diarrhea, lung deficiency and cough, kidney deficiency and spermatorrhea, deficiency heat and thirst, neurasthenia and the like. Like other genuine medicinal materials, the production of dioscorea opposita has obvious regionality, and the ancient Huaiqingfu, the modern Henan Jia make one area, and the places including Boai, Wu\38495, Qinyang, Wen county and the like are main producing places. The Chinese yam has excellent quality, is highly popular with doctors and is highly evaluated in the past traditional Chinese medicine book. Modern researches show that the dioscorea opposita thunb has various physiological and pharmacological activities of immunoregulation, tumor resistance, blood sugar reduction, oxidation resistance, aging resistance and the like, and is one of the commonly used tonic medicines in the traditional Chinese medicine formula. Since the Chinese yam is evaluated as 'warm tonification' and 'neutral nature' by doctors and families, the Chinese yam is a model of 'homology of medicine and food', has been developed into a Chinese medicine variety with the largest yield and the highest output value in Henan, and is widely popular in the market. In appearance, the Chinese yam has more hair, the skin color is slightly dark, and the peculiar dark red rust spot can be seen, which is an important apparent characteristic and one of the characteristics of showing the genuine character. Research shows that the Chinese yam root bark contains a large amount of phenols, particularly, the rust spot part of the Chinese yam root bark is rich in anthocyanin substances, and the Chinese yam root bark has multiple functions of resisting oxidation, removing free radicals, resisting inflammation and the like.
The prior art discloses methods for extracting anthocyanin from plant roots. The invention patent with application publication number CN104356107A discloses a method for extracting anthocyanin from purple yam peel, which comprises the following steps: selecting fresh and nontoxic purple yam skins, cleaning, removing impurities, crushing into powder, drying in a drying oven at 50 ℃ for 12 hours, sieving with a 80-100-mesh sieve, and placing in a dark place for later use; accurately weighing purple yam peel powder, adding an ethanol extractant with the concentration of 20-30% according to the material-liquid ratio of 1: 6-1: 8, placing the mixture in a constant-temperature water bath at the temperature of 50-70 ℃ for leaching for 1.3-1.7 h, and filtering to fix the volume; and (3) placing the filtered extract with constant volume in a rotary evaporator for evaporation and concentration to obtain a paste, and drying to obtain the anthocyanin. The method is characterized in that anthocyanin in purple yam peel is extracted, the purple yam is different from the dioscorea opposita and is not a species, and the anthocyanin in the purple yam is different from the anthocyanin in the dioscorea opposita in terms of components. The method adopts ethanol for extraction, and adopts a rotary evaporation method to remove the ethanol after extraction, so that the ethanol is not easy to separate and remove.
Disclosure of Invention
The invention aims to provide a method for extracting anthocyanin from dioscorea opposita root bark, which has the advantages of low cost of raw materials, environmental friendliness, simple and easy operation of a purification method, and high value of the obtained anthocyanin product.
The invention adopts the following technical scheme:
the method for extracting anthocyanin from Chinese yam root bark comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb;
2) soaking the Chinese yam rhizome peel powder twice with acidic methanol and carrying out ultrasonic extraction, combining the extracting solutions, concentrating and drying to obtain the Chinese yam rhizome peel anthocyanin.
Further, the Chinese yam root bark in the step 1) contains Chinese yam root bark and Chinese yam, and the mass ratio of the Chinese yam root bark to the Chinese yam is 1: 40-60.
Further, 8-15 mL of acidic methanol is added to each gram of the Chinese yam rhizome peel powder in the step 2).
Further, the acidic methanol in the step 2) is a mixed solution of hydrochloric acid and methanol, and the ratio of the hydrochloric acid to the methanol is 0.5: 100.
Further, in the step 2), adding acidic methanol into the dry powder of the root and bark of the dioscorea opposita thumb, performing primary soaking for 12 hours at 25 ℃, performing primary ultrasonic extraction for 20 minutes, and filtering to obtain primary extracting solution and primary filter residue; adding acidic methanol into the first-stage filter residue, soaking for 6 hr at 25 deg.C, performing second-stage ultrasonic extraction for 10min, filtering to obtain second-stage extractive solution, and mixing the first-stage extractive solution and the second-stage extractive solution to obtain total extractive solution.
Further, the total extract was concentrated under reduced pressure to recover the solvent.
Further, in the first-stage soaking, 8-15 mL of acidic methanol is added into per gram of the Chinese yam root-bark powder; and performing secondary soaking, wherein the amount of the acidic methanol added into the primary filter residue is 40-60% of the volume of the acidic methanol subjected to primary soaking.
Compared with the prior art, the invention has the beneficial effects that:
the method for extracting anthocyanin from dioscorea opposita root bark can solve the problem of root bark waste generated in dioscorea opposita decoction piece processing industry, anthocyanin substances with high added values are extracted from the dioscorea opposita root bark, the used extraction raw materials are low in cost and easy to obtain, the purification method is simple and convenient to operate, environment-friendly pollution can be reduced, and the method has the advantages of simplicity and convenience in operation, easiness in scale production and the like. In addition, methanol is purified, so that the methanol solvent is convenient to recover.
Drawings
FIG. 1 is a high performance liquid chromatogram of dioscorea root anthocyanin obtained in example 1.
The chromatographic peaks in the figure are all anthocyanin compounds determined by ultraviolet spectrum, wherein the most main chromatographic peak is identified as cyanidin.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1
The method for extracting anthocyanin from dioscorea opposita root bark in the embodiment comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb. The Chinese yam rhizome peel comprises Chinese yam rhizome peel and Chinese yam, and the mass ratio of the Chinese yam rhizome peel to the Chinese yam is 1: 50.
2) Taking 100 g of dioscorea opposita root bark powder, adding 1000 mL of 0.5% methanol hydrochloride, carrying out primary soaking for 12h at 25 ℃, then carrying out primary ultrasonic extraction for 20min, and filtering to obtain primary extracting solution and primary filter residue. And adding 500 mL of 0.5% methanol hydrochloride into the primary filter residue, soaking for 6 h at 25 ℃, performing ultrasonic extraction for 10min, and filtering to obtain a secondary extracting solution and a secondary residue. And mixing the first-stage extract and the second-stage extract to obtain a total extract. And concentrating the total extracting solution under reduced pressure to recover the solvent methanol, and drying to obtain the dioscorea root-bark anthocyanin.
Taking 1 mg of dried dioscorea root-bark anthocyanin, fixing the volume to 5 mL by using methanol, wherein the parameters measured by a high performance liquid chromatography method comprise: the chromatographic column is Waters HSS T3-C18Column (2.1 × 100 mm, 1.8 μm), mobile phase is 0.1% formic acid water and 0.1% formic acid acetonitrile with volume ratio of 85:15, sample amount is 2 μ L, detection wavelength is 530nm, flow rate is 1 mL/min, column temperature is 30 deg.C, and measurement and calculation are carried out, and cyanidin content in the obtained rhizoma Dioscoreae radicicol is about 28.9 mg/kg.
The measurement results are shown in fig. 1, and the chromatographic peaks in the graph are all anthocyanin compounds determined by ultraviolet spectroscopy, wherein the most main chromatographic peak is identified as cyanidin (cyanidin). The content and proportion of the anthocyanin can be changed in different embodiments due to the change of extraction conditions.
Example 2
The method for extracting anthocyanin from dioscorea opposita root bark in the embodiment comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb. The Chinese yam rhizome peel comprises Chinese yam rhizome peel and Chinese yam, and the mass ratio of the Chinese yam rhizome peel to the Chinese yam is 1: 50.
2) Taking 250 g of Chinese yam rhizome peel powder, adding 2000mL of 0.5% methanol hydrochloride, carrying out primary soaking for 12h at 25 ℃, then carrying out primary ultrasonic extraction for 30 min, and filtering to obtain primary extracting solution and primary filter residue. Adding 1500 mL of 0.5% methanol hydrochloride into the first-stage filter residue, soaking at 25 deg.C for 6 h, performing ultrasonic extraction for 15 min, and filtering to obtain second-stage extract and second-stage residue. And mixing the first-stage extract and the second-stage extract to obtain a total extract. And concentrating the total extracting solution under reduced pressure to recover the solvent methanol, and drying to obtain the dioscorea root-bark anthocyanin.
Taking 1 mg of dried dioscorea root-bark anthocyanin, fixing the volume to 5 mL by using methanol, wherein the parameters measured by a high performance liquid chromatography method comprise: the chromatographic column is Waters HSS T3-C18Column (2.1 × 100 mm, 1.8 μm), mobile phase is 0.1% formic acid water and 0.1% formic acid acetonitrile with volume ratio of 85:15, sample amount is 2 μ L, detection wavelength is 530nm, flow rate is 1 mL/min, column temperature is 30 deg.C, and measurement and calculation are carried out, and cyanidin content in the obtained rhizoma Dioscoreae radicicol is about 25.5 mg/kg.
Example 3
The method for extracting anthocyanin from dioscorea opposita root bark in the embodiment comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb. The Chinese yam rhizome peel comprises Chinese yam rhizome peel and Chinese yam, and the mass ratio of the Chinese yam rhizome peel to the Chinese yam is 1: 50.
2) Taking 500 g of dioscorea opposita root bark powder, adding 4500 mL of 0.5% methanol hydrochloride, primary soaking for 12h at 25 ℃, then primary ultrasonic extracting for 30 min, and filtering to obtain primary extracting solution and primary filter residue. Adding 2000mL of 0.5% methanol hydrochloride into the first-stage filter residue, soaking at 25 deg.C for 6 h, performing ultrasonic extraction for 15 min, and filtering to obtain second-stage extract and second-stage residue. And mixing the first-stage extract and the second-stage extract to obtain a total extract. And concentrating the total extracting solution under reduced pressure to recover the solvent methanol, and drying to obtain the dioscorea root-bark anthocyanin.
Taking 1 mg of dried dioscorea root-bark anthocyanin, fixing the volume to 5 mL by using methanol, wherein the parameters measured by a high performance liquid chromatography method comprise: the chromatographic column is Waters HSS T3-C18Column (2.1 × 100 mm, 1.8 μm) with mobile phase of 0.1% formic acid water and 0.1% formic acid acetonitrile at volume ratio of 85:15, sample volume of 2 μ L, and detectingThe measurement wavelength was 530nm, the flow rate was 1 mL/min, and the column temperature was 30 ℃. Through measurement and calculation, the cyanidin content in the obtained dioscorea opposita root anthocyanin is about 24.8 mg/kg.
Example 4
The method for extracting anthocyanin from dioscorea opposita root bark in the embodiment comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb. The Chinese yam rhizome peel comprises Chinese yam rhizome peel and Chinese yam, and the mass ratio of the Chinese yam rhizome peel to the Chinese yam is 1: 50.
2) Taking 1000 g of dioscorea opposita root-bark powder, adding 9000 mL of 0.5% methanol hydrochloride, carrying out primary soaking for 12h at 25 ℃, then carrying out primary ultrasonic extraction for 25 min, and filtering to obtain primary extracting solution and primary filter residue. And adding 5000 mL of 0.5% methanol hydrochloride into the primary filter residue, soaking at 25 ℃ for 6 h, performing ultrasonic extraction for 15 min, and filtering to obtain a secondary extracting solution and a secondary residue. And mixing the first-stage extract and the second-stage extract to obtain a total extract. And concentrating the total extracting solution under reduced pressure to recover the solvent methanol, and drying to obtain the dioscorea root-bark anthocyanin.
Taking 1 mg of dried dioscorea root-bark anthocyanin, fixing the volume to 5 mL by using methanol, wherein the parameters measured by a high performance liquid chromatography method comprise: the chromatographic column is Waters HSS T3-C18Column (2.1 × 100 mm, 1.8 μm), mobile phase is 0.1% formic acid water and 0.1% formic acid acetonitrile with volume ratio of 85:15, sample amount is 2 μ L, detection wavelength is 530nm, flow rate is 1 mL/min, column temperature is 30 deg.C, and measurement and calculation are carried out, and cyanidin content in the obtained rhizoma Dioscoreae radicicol is about 24.9 mg/kg.
Example 5
The method for extracting anthocyanin from dioscorea opposita root bark in the embodiment comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb. The Chinese yam rhizome peel comprises Chinese yam rhizome peel and Chinese yam, and the mass ratio of the Chinese yam rhizome peel to the Chinese yam is 1: 50.
2) Taking 2000 g of dioscorea opposita root bark powder, adding 18000 mL of 0.5% methanol hydrochloride, soaking for 15h at 25 ℃ in a first stage, then carrying out first-stage ultrasonic extraction for 30 min, and filtering to obtain a first-stage extracting solution and first-stage filter residue. And adding 10000 mL of 0.5% methanol hydrochloride into the primary filter residue, soaking for 6 h at 25 ℃, performing ultrasonic extraction for 15 min, and filtering to obtain a secondary extracting solution and a secondary residue. And mixing the first-stage extract and the second-stage extract to obtain a total extract. And concentrating the total extracting solution under reduced pressure to recover the solvent methanol, and drying to obtain the dioscorea root-bark anthocyanin.
Taking 1 mg of dried dioscorea root-bark anthocyanin, fixing the volume to 5 mL by using methanol, wherein the parameters measured by a high performance liquid chromatography method comprise: the chromatographic column is Waters HSS T3-C18Column (2.1 × 100 mm, 1.8 μm), mobile phase is 0.1% formic acid water and 0.1% formic acid acetonitrile with volume ratio of 85:15, sample amount is 2 μ L, detection wavelength is 530nm, flow rate is 1 mL/min, column temperature is 30 deg.C, and measurement and calculation are carried out, and cyanidin content in the obtained rhizoma Dioscoreae radicicol is about 22.4 mg/kg.
Example 6
The method for extracting anthocyanin from dioscorea opposita root bark in the embodiment comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb. The Chinese yam rhizome peel comprises Chinese yam rhizome peel and Chinese yam, and the mass ratio of the Chinese yam rhizome peel to the Chinese yam is 1: 40.
2) Taking 100 g of dioscorea opposita root bark powder, adding 800 mL of 0.5% methanol hydrochloride, carrying out primary soaking for 12h at 25 ℃, then carrying out primary ultrasonic extraction for 20min, and filtering to obtain primary extracting solution and primary filter residue. And adding 320 mL of 0.5% methanol hydrochloride into the primary filter residue, soaking for 6 h at 25 ℃, performing ultrasonic extraction for 10min, and filtering to obtain a secondary extracting solution and a secondary residue. And mixing the first-stage extract and the second-stage extract to obtain a total extract. And concentrating the total extracting solution under reduced pressure to recover the solvent methanol, and drying to obtain the dioscorea root-bark anthocyanin.
Taking 1 mg of dried dioscorea root-bark anthocyanin, fixing the volume to 5 mL by using methanol, wherein the parameters measured by a high performance liquid chromatography method comprise: the chromatographic column is Waters HSS T3-C18Column (2.1 × 100 mm, 1.8 μm), mobile phase of 0.1% formic acid water and 0.1% formic acid acetonitrile at volume ratio of 85:15, sample amount of 2 μ L, detection wavelength of 530nm, and flow rate of 1 mL/min, the column temperature is 30 ℃. Through measurement and calculation, the cyanidin content in the obtained dioscorea opposita root anthocyanin is about 28.8 mg/kg.
Example 7
The method for extracting anthocyanin from dioscorea opposita root bark in the embodiment comprises the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb. The Chinese yam rhizome peel comprises Chinese yam rhizome peel and Chinese yam, and the mass ratio of the Chinese yam rhizome peel to the Chinese yam is 1: 60.
2) Taking 100 g of dioscorea root bark powder, adding 1500 mL of 0.5% methanol hydrochloride, carrying out primary soaking for 12h at 25 ℃, then carrying out primary ultrasonic extraction for 20min, and filtering to obtain primary extracting solution and primary filter residue. And adding 480 mL of 0.5% methanol hydrochloride into the primary filter residue, soaking for 6 h at 25 ℃, performing ultrasonic extraction for 10min, and filtering to obtain a secondary extracting solution and a secondary residue. And mixing the first-stage extract and the second-stage extract to obtain a total extract. And concentrating the total extracting solution under reduced pressure to recover the solvent methanol, and drying to obtain the dioscorea root-bark anthocyanin.
Taking 1 mg of dried dioscorea root-bark anthocyanin, fixing the volume to 5 mL by using methanol, wherein the parameters measured by a high performance liquid chromatography method comprise: the chromatographic column is Waters HSS T3-C18Column (2.1 × 100 mm, 1.8 μm), mobile phase is 0.1% formic acid water and 0.1% formic acid acetonitrile with volume ratio of 85:15, sample amount is 2 μ L, detection wavelength is 530nm, flow rate is 1 mL/min, column temperature is 30 deg.C, and measurement and calculation are carried out, and cyanidin content in the obtained rhizoma Dioscoreae radicicol is about 29.0 mg/kg.
The embodiments of the present invention have been described in detail with reference to the drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the gist of the present invention.
Claims (7)
1. The method for extracting anthocyanin from Chinese yam root bark is characterized by comprising the following steps:
1) drying and crushing the root bark of the dioscorea opposita thumb to obtain the root bark powder of the dioscorea opposita thumb;
2) soaking the Chinese yam rhizome peel powder twice with acidic methanol and carrying out ultrasonic extraction, combining the extracting solutions, concentrating and drying to obtain the Chinese yam rhizome peel anthocyanin.
2. The method for extracting anthocyanin from dioscorea opposita root bark as claimed in claim 1, wherein the dioscorea opposita root bark in the step 1) contains dioscorea opposita root bark and dioscorea opposita, and the mass ratio of the dioscorea opposita root bark to the dioscorea opposita is 1: 40-60.
3. The method for extracting anthocyanin from dioscorea opposita root-bark powder as claimed in claim 1, wherein 8-15 mL of acidic methanol is added to each gram of dioscorea opposita root-bark powder in step 2).
4. The method for extracting anthocyanin from dioscorea opposita root bark as claimed in claim 1, wherein the acidic methanol in step 2) is a mixture of hydrochloric acid and methanol, and the volume ratio of hydrochloric acid to methanol is 0.5: 100.
5. The method for extracting anthocyanin from dioscorea opposita root bark as claimed in any one of claims 1 to 4, wherein in the step 2), dioscorea opposita root bark dry powder is taken, acid methanol is added, primary soaking is carried out for 12h at the temperature of 25 ℃, then primary ultrasonic extraction is carried out for 20min, and filtration is carried out to obtain primary extracting solution and primary filter residue; adding acidic methanol into the first-stage filter residue, soaking at 25 deg.C for 6 hr, performing second-stage ultrasonic extraction for 10min, filtering to obtain second-stage extractive solution, and mixing the first-stage extractive solution and the second-stage extractive solution to obtain total extractive solution.
6. The method for extracting anthocyanin from rhizoma dioscoreae root bark as claimed in claim 5, wherein the total extract is concentrated under reduced pressure to recover solvent.
7. The method for extracting anthocyanin from dioscorea opposita root-bark powder as claimed in claim 5, wherein in the first-stage soaking, 8-15 mL of acidic methanol is added into per gram of dioscorea opposita root-bark powder; and performing secondary soaking, wherein the amount of the acidic methanol added into the primary filter residue is 40-60% of the volume of the acidic methanol subjected to primary soaking.
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