CN115010776A - Method for extracting buckwheat rutin - Google Patents
Method for extracting buckwheat rutin Download PDFInfo
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- CN115010776A CN115010776A CN202210723962.4A CN202210723962A CN115010776A CN 115010776 A CN115010776 A CN 115010776A CN 202210723962 A CN202210723962 A CN 202210723962A CN 115010776 A CN115010776 A CN 115010776A
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- rutin
- tartary buckwheat
- buckwheat
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- extracting
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- JMGZEFIQIZZSBH-UHFFFAOYSA-N Bioquercetin Natural products CC1OC(OCC(O)C2OC(OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5)C(O)C2O)C(O)C(O)C1O JMGZEFIQIZZSBH-UHFFFAOYSA-N 0.000 title claims abstract description 81
- IVTMALDHFAHOGL-UHFFFAOYSA-N eriodictyol 7-O-rutinoside Natural products OC1C(O)C(O)C(C)OC1OCC1C(O)C(O)C(O)C(OC=2C=C3C(C(C(O)=C(O3)C=3C=C(O)C(O)=CC=3)=O)=C(O)C=2)O1 IVTMALDHFAHOGL-UHFFFAOYSA-N 0.000 title claims abstract description 81
- FDRQPMVGJOQVTL-UHFFFAOYSA-N quercetin rutinoside Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 FDRQPMVGJOQVTL-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 235000005493 rutin Nutrition 0.000 title claims abstract description 81
- ALABRVAAKCSLSC-UHFFFAOYSA-N rutin Natural products CC1OC(OCC2OC(O)C(O)C(O)C2O)C(O)C(O)C1OC3=C(Oc4cc(O)cc(O)c4C3=O)c5ccc(O)c(O)c5 ALABRVAAKCSLSC-UHFFFAOYSA-N 0.000 title claims abstract description 81
- IKGXIBQEEMLURG-BKUODXTLSA-N rutin Chemical compound O[C@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@@H]1OC[C@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](OC=2C(C3=C(O)C=C(O)C=C3OC=2C=2C=C(O)C(O)=CC=2)=O)O1 IKGXIBQEEMLURG-BKUODXTLSA-N 0.000 title claims abstract description 81
- 229960004555 rutoside Drugs 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 19
- 241000219051 Fagopyrum Species 0.000 title claims abstract description 17
- 235000009419 Fagopyrum esculentum Nutrition 0.000 title claims abstract description 17
- 244000130270 Fagopyrum tataricum Species 0.000 claims abstract description 64
- 235000014693 Fagopyrum tataricum Nutrition 0.000 claims abstract description 64
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000001816 cooling Methods 0.000 claims abstract description 21
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 19
- 238000007710 freezing Methods 0.000 claims abstract description 16
- 238000009835 boiling Methods 0.000 claims abstract description 10
- 238000000605 extraction Methods 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims description 9
- 230000008025 crystallization Effects 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 3
- 239000005416 organic matter Substances 0.000 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 11
- 238000001514 detection method Methods 0.000 description 8
- 238000010812 external standard method Methods 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 238000004128 high performance liquid chromatography Methods 0.000 description 8
- 238000004140 cleaning Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 5
- 229930003944 flavone Natural products 0.000 description 5
- 235000011949 flavones Nutrition 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 150000002212 flavone derivatives Chemical class 0.000 description 4
- 238000001035 drying Methods 0.000 description 3
- 239000000706 filtrate Substances 0.000 description 3
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 238000000108 ultra-filtration Methods 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 241000219050 Polygonaceae Species 0.000 description 2
- ZVOLCUVKHLEPEV-UHFFFAOYSA-N Quercetagetin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=C(O)C(O)=C(O)C=C2O1 ZVOLCUVKHLEPEV-UHFFFAOYSA-N 0.000 description 2
- HWTZYBCRDDUBJY-UHFFFAOYSA-N Rhynchosin Natural products C1=C(O)C(O)=CC=C1C1=C(O)C(=O)C2=CC(O)=C(O)C=C2O1 HWTZYBCRDDUBJY-UHFFFAOYSA-N 0.000 description 2
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- -1 flavone compounds Chemical class 0.000 description 2
- IYRMWMYZSQPJKC-UHFFFAOYSA-N kaempferol Chemical compound C1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 IYRMWMYZSQPJKC-UHFFFAOYSA-N 0.000 description 2
- 238000002386 leaching Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- UXOUKMQIEVGVLY-UHFFFAOYSA-N morin Natural products OC1=CC(O)=CC(C2=C(C(=O)C3=C(O)C=C(O)C=C3O2)O)=C1 UXOUKMQIEVGVLY-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 235000005875 quercetin Nutrition 0.000 description 2
- 229960001285 quercetin Drugs 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000000967 suction filtration Methods 0.000 description 2
- 206010007191 Capillary fragility Diseases 0.000 description 1
- UBSCDKPKWHYZNX-UHFFFAOYSA-N Demethoxycapillarisin Natural products C1=CC(O)=CC=C1OC1=CC(=O)C2=C(O)C=C(O)C=C2O1 UBSCDKPKWHYZNX-UHFFFAOYSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- YXOLAZRVSSWPPT-UHFFFAOYSA-N Morin Chemical compound OC1=CC(O)=CC=C1C1=C(O)C(=O)C2=C(O)C=C(O)C=C2O1 YXOLAZRVSSWPPT-UHFFFAOYSA-N 0.000 description 1
- LUJAXSNNYBCFEE-UHFFFAOYSA-N Quercetin 3,7-dimethyl ether Natural products C=1C(OC)=CC(O)=C(C(C=2OC)=O)C=1OC=2C1=CC=C(O)C(O)=C1 LUJAXSNNYBCFEE-UHFFFAOYSA-N 0.000 description 1
- PUTDIROJWHRSJW-UHFFFAOYSA-N Quercitrin Natural products CC1OC(Oc2cc(cc(O)c2O)C3=CC(=O)c4c(O)cc(O)cc4O3)C(O)C(O)C1O PUTDIROJWHRSJW-UHFFFAOYSA-N 0.000 description 1
- OXGUCUVFOIWWQJ-XIMSSLRFSA-N acanthophorin B Natural products O[C@H]1[C@H](O)[C@H](O)[C@H](C)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OXGUCUVFOIWWQJ-XIMSSLRFSA-N 0.000 description 1
- 238000009098 adjuvant therapy Methods 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000019658 bitter taste Nutrition 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 210000005069 ears Anatomy 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000010828 elution Methods 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013376 functional food Nutrition 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 235000008777 kaempferol Nutrition 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 239000002075 main ingredient Substances 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 230000004089 microcirculation Effects 0.000 description 1
- 238000000874 microwave-assisted extraction Methods 0.000 description 1
- 235000007708 morin Nutrition 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 210000000056 organ Anatomy 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000005325 percolation Methods 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- OEKUVLQNKPXSOY-UHFFFAOYSA-N quercetin 3-O-beta-D-glucopyranosyl(1->3)-alpha-L-rhamnopyranosyl(1->6)-beta-d-galactopyranoside Natural products OC1C(O)C(C(O)C)OC1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OEKUVLQNKPXSOY-UHFFFAOYSA-N 0.000 description 1
- QPHXPNUXTNHJOF-UHFFFAOYSA-N quercetin-7-O-beta-L-rhamnopyranoside Natural products OC1C(O)C(O)C(C)OC1OC1=CC(O)=C2C(=O)C(O)=C(C=3C=C(O)C(O)=CC=3)OC2=C1 QPHXPNUXTNHJOF-UHFFFAOYSA-N 0.000 description 1
- OXGUCUVFOIWWQJ-HQBVPOQASA-N quercitrin Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1OC1=C(C=2C=C(O)C(O)=CC=2)OC2=CC(O)=CC(O)=C2C1=O OXGUCUVFOIWWQJ-HQBVPOQASA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 210000000582 semen Anatomy 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 150000005846 sugar alcohols Chemical class 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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
- C07H17/07—Benzo[b]pyran-4-ones
-
- 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)
- Medicines Containing Plant Substances (AREA)
- Saccharide Compounds (AREA)
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention belongs to the technical field of extraction of effective components, and relates to a method for extracting buckwheat rutin; the method comprises the following steps: carrying out quick-freezing treatment on the fresh tartary buckwheat grains; carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains at the temperature ranging from-5 ℃ to-18 ℃; the frequency of ultrasonic vibration is 10KHz-20KHz, and the power is 1-3 KW; the ultrasonic vibration time is 10-40 s; adding the tartary buckwheat seeds subjected to ultrasonic treatment into water, and boiling for 30-60 min; then cooling the water decoction to separate out crude rutin; recrystallizing the crude rutin with hot water to obtain a rutin finished product; the invention does not use organic matter or acid-base solution for extraction, avoids subsequent processing steps, reduces the content of other substances in the rutin, effectively improves the purity of the rutin, has simpler and more convenient extraction method, and is beneficial to industrial production.
Description
Technical Field
The invention belongs to the technical field of extraction of effective components, and relates to a method for extracting tartary buckwheat rutin.
Background
Tartary buckwheat (F. tartartartaricum) is also called Pyctanthus genus Polygonaceae (Polygona ceae) buckwheat genus ((FagopyrumGaerth) is a medicinal and edible crop, the records of compendium of materia medica): the tartary buckwheat is bitter, mild and cold in nature, and has the effects of maintaining spirit, benefiting strength, benefiting ears and eyes, descending qi, widening intestines and invigorating stomach, modern researches show that: the distribution research of the tartary buckwheat functional components is that the tartary buckwheat flavone is the largest, the protein is the second, the sugar alcohol is the smallest, the content of the tartary buckwheat flavone is different due to different stages and organs, the tartary buckwheat flavone is a polyphenol natural product existing in flowers, stems, leaves and seeds of the tartary buckwheat, and mainly comprises four main components of rutin, quercetin, kaempferol, morin and the like, wherein the rutin content is the highest and accounts for about 85 percent of the four flavone compounds.
Rutin (rutin), also known as rutin and quercitrin, is 3-0-rutinoside of quercetin, has a molecular formula of C27H30O 16.3H 2O and a relative molecular weight of 610.51, is yellow crystalline powder or amorphous powder, has bitter taste, has a melting point of 177-178 ℃, and can be dissolved in hot water and ethanol. Rutin is a flavonoid compound with a wide source. Rutin, as the main ingredient of flavone, can be used as antioxidant and functional food material, has effects of reducing capillary fragility and improving microcirculation, and is mainly used for clinically adjuvant treatment of diabetes, hypertension, etc.
In the prior art, the method for extracting rutin from tartary buckwheat generally comprises the following steps: ethanol reflux extraction, organic solvent percolation, adsorption column chromatography, ultrasonic microwave extraction and the like, but the methods have low utilization rate of raw materials and low purity of rutin, and are not suitable for industrial production.
Disclosure of Invention
The invention overcomes the defects of the prior art and provides a method for extracting buckwheat rutin. So as to improve the utilization rate of the tartary buckwheat and the purity of the rutin.
In order to achieve the above object, the present invention is achieved by the following technical solutions.
The extraction method of tartary buckwheat rutin is characterized by comprising the following steps:
1) and (4) carrying out quick-freezing treatment on the fresh tartary buckwheat grains.
2) Carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains at the temperature ranging from-5 ℃ to-18 ℃; the frequency of ultrasonic vibration is 10KHz-20KHz, and the power is 1-3 KW; the time of ultrasonic vibration is 10-40 s.
3) Adding the tartary buckwheat seeds subjected to ultrasonic treatment into water, and boiling for 30-60 min; then cooling the water decoction to separate out crude rutin.
4) Recrystallizing the crude rutin with hot water to obtain a rutin finished product.
Preferably, the quick-freezing treatment is to ensure that the central temperature of the fresh tartary buckwheat grains reaches-15 ℃ to-18 ℃ within 10 min.
Preferably, the ultrasonic treatment is to embed a vibrator of an ultrasonic device into the tartary buckwheat seed.
Preferably, the vibrator is first cooled to a temperature of-5 ℃ to-10 ℃.
Preferably, the time of the ultrasonic vibration is 30 s.
Preferably, in the step 3), the temperature of the boiled liquid is reduced to 10-20 ℃, and the boiled liquid is kept stand for 12-24h, so that crude rutin is separated out.
Preferably, in the step 4), the crude rutin is dissolved in hot water at the temperature of 98 ℃, filtered while hot, naturally cooled to room temperature, and kept stand for crystallization to obtain the rutin.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, fresh tartary buckwheat seeds are frozen in a quick-freezing manner, moisture in the tartary buckwheat seeds forms fine ice crystals, ultrasonic low-temperature treatment is adopted in the state, acoustic flow and cavitation effect are generated in the tartary buckwheat seeds, the ice crystals form uniform and fine grains, and tartary buckwheat rutin is released by being separated from the constraint of macromolecular substances easily under the action of the grains; then the rutin component can be effectively extracted through the steps of boiling water extraction and recrystallization.
The invention does not use organic matter or acid-base solution for extraction, avoids subsequent processing steps, reduces the content of other substances in the rutin, effectively improves the purity of the rutin, has simpler and more convenient extraction method, and is beneficial to industrial production.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to examples, but the scope of protection is not limited thereto.
Example 1
A method for extracting buckwheat rutin comprises the following specific steps:
1) cleaning and airing 100g of newly harvested plump fresh tartary buckwheat grains, and then carrying out quick-freezing treatment on the fresh tartary buckwheat grains: the quick-freezing treatment is to make the central temperature of fresh tartary buckwheat grains reach-15 ℃ to-18 ℃ within 10 min.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains at the temperature of-5 ℃; the frequency of ultrasonic vibration is 10KHz, and the power is 3 KW; the time of ultrasonic vibration was 20 seconds. The ultrasonic treatment is carried out by cooling vibrator of ultrasonic device to-5 deg.C, and embedding into fresh semen Fagopyri Esculenti.
3) Directly adding the ultrasonically treated fresh tartary buckwheat seeds into cold water, and boiling for 30 min; then cooling the water decoction to 10 ℃, standing for 24h, and separating out crude rutin.
4) Dissolving the crude rutin in hot water of 98 deg.C, filtering while it is hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin refined product obtained in the embodiment has the mass content of 96.9 percent.
Example 2
A method for extracting buckwheat rutin comprises the following specific steps:
1) cleaning and airing 100g of newly harvested plump fresh tartary buckwheat grains, and then carrying out quick-freezing treatment on the fresh tartary buckwheat grains: the quick-freezing treatment is to make the central temperature of fresh tartary buckwheat grains reach-15 ℃ to-18 ℃ within 10 min.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains at the temperature of-18 ℃; the frequency of ultrasonic vibration is 20KHz, and the power is 2 KW; the time of ultrasonic vibration was 30 seconds. The ultrasonic treatment is carried out by cooling the vibrator of the ultrasonic device to-10 deg.C, and embedding into fresh tartary buckwheat seed for treatment.
3) Directly adding the ultrasonically treated fresh tartary buckwheat seeds into cold water, and boiling for 60 min; then cooling the water decoction to 20 ℃, standing for 24h, and separating out crude rutin.
4) Dissolving the crude rutin in 98 deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin refined product obtained in the embodiment has the mass content of 98.7 percent.
Example 3
A method for extracting buckwheat rutin comprises the following specific steps:
1) cleaning and airing 100g of newly harvested full fresh tartary buckwheat grains, and then carrying out quick-freezing treatment on the fresh tartary buckwheat grains: the quick-freezing treatment is carried out within 10min to ensure that the central temperature of the fresh tartary buckwheat grains reaches-18 ℃.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat seeds at the temperature of-10 ℃; the frequency of ultrasonic vibration is 20KHz, and the power is 1 KW; the time of ultrasonic vibration was 40 s. The ultrasonic treatment is carried out by cooling the vibrator of the ultrasonic device to-10 deg.C, and embedding into fresh tartary buckwheat seed for treatment.
3) Directly adding the fresh tartary buckwheat seeds subjected to ultrasonic treatment into cold water, and boiling for 40 min; then cooling the water decoction to 20 ℃, standing for 24h, and separating out crude rutin.
4) Dissolving the crude rutin in 98 deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin refined product obtained in the embodiment has the mass content of 97.1 percent.
Example 4
A method for extracting buckwheat rutin comprises the following specific steps:
1) cleaning and airing 100g of newly harvested plump fresh tartary buckwheat grains, and then carrying out quick-freezing treatment on the fresh tartary buckwheat grains: the quick-freezing treatment is carried out within 10min to ensure that the central temperature of the fresh tartary buckwheat grains reaches-15 ℃.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains at the temperature of-10 ℃; the frequency of ultrasonic vibration is 10KHz, and the power is 3 KW; the time of ultrasonic vibration was 30 seconds. The ultrasonic treatment is carried out by cooling the vibrator of the ultrasonic device to-10 deg.C, and embedding into fresh tartary buckwheat seed for treatment.
3) Directly adding the ultrasonically treated fresh tartary buckwheat seeds into cold water, and boiling for 40 min; then cooling the water decoction to 20 ℃, standing for 24h, and separating out crude rutin.
4) Dissolving the crude rutin in 98 deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin refined product obtained in the embodiment has the mass content of 98.2 percent.
Example 5
A method for extracting buckwheat rutin comprises the following specific steps:
1) cleaning and airing 100g of newly harvested plump fresh tartary buckwheat grains, and then carrying out quick-freezing treatment on the fresh tartary buckwheat grains: the quick-freezing treatment is carried out within 10min to ensure that the central temperature of the fresh tartary buckwheat grains reaches-15 ℃.
2) Then carrying out ultrasonic treatment on the quick-frozen tartary buckwheat grains at the temperature of-18 ℃; the frequency of ultrasonic vibration is 10KHz, and the power is 2 KW; the time of ultrasonic vibration was 40 s. The ultrasonic treatment is carried out by cooling the vibrator of the ultrasonic device to-10 deg.C, and embedding into fresh tartary buckwheat seed for treatment.
3) Directly adding the fresh tartary buckwheat seeds subjected to ultrasonic treatment into cold water, and boiling for 60 min; then cooling the water decoction to 10 ℃, standing for 24h, and separating out crude rutin.
4) Dissolving the crude rutin in 98 deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin refined product obtained in the embodiment has the mass content of 97.6 percent.
Comparative example 1
Selecting 100g of complete fresh tartary buckwheat seeds, cleaning the fresh tartary buckwheat seeds, putting the cleaned tartary buckwheat seeds into clear water, soaking for 2-24 hours at 10-50 ℃, draining off water from the tartary buckwheat seeds after soaking, then drying the drained tartary buckwheat seeds in an environment with the temperature of 105 ℃, adding lime water with the pH value of 8-9 de, leaching for different times at the constant temperature of 80 ℃ by ultrasonic waves, performing suction filtration, and determining the leaching yield of rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin quality product obtained in the comparative example 1 has the rutin mass content of 85.1%.
Comparative example 2
Pulverizing 100g of tartary buckwheat seeds to a particle size of 2mm, adding 2000g of calcium hydroxide aqueous solution, stirring and extracting for 5h, filtering, adjusting the pH value of the filtrate to 6.0 by using a hydrochloric acid solution with the mass concentration of 5%, and then performing ultrafiltration to obtain an ultrafiltration membrane filtrate; and (3) carrying out elution on the obtained ultrafiltration membrane filtrate by using a chromatographic column, collecting eluent, concentrating and drying to obtain a crude rutin product, dissolving the crude rutin product by using 75g of hot water at 98 ℃, filtering while hot, naturally cooling to room temperature, standing for crystallization for 12 hours, carrying out suction filtration and drying to obtain the rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin refined product obtained in the comparative example 2 has the rutin content of 89.2 percent by mass.
Comparative example 3
Soaking 100g of fresh tartary buckwheat grains in water at 50 ℃ for 24 hours, and then boiling for 40 min; then cooling the water decoction to 20 ℃, standing for 24h, and separating out crude rutin. Dissolving the crude rutin in 98 deg.C hot water, filtering while hot, naturally cooling to room temperature, standing for crystallization to obtain rutin.
Through the detection of a high performance liquid chromatography external standard method, the rutin refined product obtained in the comparative example 3 has the mass content of 70.5 percent.
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (7)
1. The extraction method of tartary buckwheat rutin is characterized by comprising the following steps:
1) carrying out quick-freezing treatment on the fresh tartary buckwheat grains;
2) carrying out ultrasonic treatment on the quick-frozen fresh tartary buckwheat grains at the temperature ranging from-5 ℃ to-18 ℃; the frequency of ultrasonic vibration is 10KHz-20KHz, and the power is 1-3 KW; the ultrasonic vibration time is 10-40 s;
3) adding the ultrasonically treated fresh tartary buckwheat seeds into water, and boiling for 30-60 min; then cooling the water decoction to separate out crude rutin;
4) and recrystallizing the crude rutin with hot water to obtain a rutin finished product.
2. The method for extracting buckwheat rutin of claim 1, wherein the quick freezing treatment is to make the central temperature of fresh buckwheat grains reach-15 ℃ to-18 ℃ within 10 min.
3. The method for extracting buckwheat rutin according to claim 1, wherein the ultrasonic treatment is to embed a vibrator of an ultrasonic device into fresh buckwheat seeds.
4. The method for extracting rutin in Tartary buckwheat according to claim 3, wherein the vibrator is cooled to-5 ℃ to-10 ℃.
5. The method for extracting buckwheat rutin of claim 1, wherein the time of ultrasonic vibration is 30 s.
6. The method for extracting buckwheat rutin in claim 1, wherein in step 3), the temperature of the boiled liquid is reduced to 10-20 ℃, and the boiled liquid is kept stand for 12-24h, so that crude rutin is separated out.
7. The method for extracting buckwheat rutin according to claim 1, wherein in step 4), crude rutin is dissolved in hot water of 98 ℃, filtered while hot, naturally cooled to room temperature, and left to stand for crystallization to obtain rutin.
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