CN110623188A - Method for preparing dogwood alcohol extract particles and corresponding alcohol extract particles - Google Patents
Method for preparing dogwood alcohol extract particles and corresponding alcohol extract particles Download PDFInfo
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 164
- 239000000284 extract Substances 0.000 title claims abstract description 86
- 239000002245 particle Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 49
- 240000006766 Cornus mas Species 0.000 title 1
- 241000209020 Cornus Species 0.000 claims abstract description 78
- WCGUUGGRBIKTOS-GPOJBZKASA-N (3beta)-3-hydroxyurs-12-en-28-oic acid Chemical compound C1C[C@H](O)C(C)(C)[C@@H]2CC[C@@]3(C)[C@]4(C)CC[C@@]5(C(O)=O)CC[C@@H](C)[C@H](C)[C@H]5C4=CC[C@@H]3[C@]21C WCGUUGGRBIKTOS-GPOJBZKASA-N 0.000 claims abstract description 66
- 229940096998 ursolic acid Drugs 0.000 claims abstract description 66
- PLSAJKYPRJGMHO-UHFFFAOYSA-N ursolic acid Natural products CC1CCC2(CCC3(C)C(C=CC4C5(C)CCC(O)C(C)(C)C5CCC34C)C2C1C)C(=O)O PLSAJKYPRJGMHO-UHFFFAOYSA-N 0.000 claims abstract description 66
- 239000011347 resin Substances 0.000 claims abstract description 48
- 229920005989 resin Polymers 0.000 claims abstract description 48
- 239000000706 filtrate Substances 0.000 claims abstract description 41
- 238000000605 extraction Methods 0.000 claims abstract description 30
- 238000000926 separation method Methods 0.000 claims abstract description 26
- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical class CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims abstract description 25
- 239000008187 granular material Substances 0.000 claims abstract description 25
- 238000002137 ultrasound extraction Methods 0.000 claims abstract description 24
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 18
- 229920001450 Alpha-Cyclodextrin Polymers 0.000 claims abstract description 17
- HFHDHCJBZVLPGP-RWMJIURBSA-N alpha-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO HFHDHCJBZVLPGP-RWMJIURBSA-N 0.000 claims abstract description 17
- 229940043377 alpha-cyclodextrin Drugs 0.000 claims abstract description 17
- 239000000843 powder Substances 0.000 claims abstract description 17
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 239000000725 suspension Substances 0.000 claims abstract description 11
- 238000001694 spray drying Methods 0.000 claims abstract description 10
- 239000003480 eluent Substances 0.000 claims description 27
- 238000010828 elution Methods 0.000 claims description 26
- 238000011068 loading method Methods 0.000 claims description 19
- 238000011049 filling Methods 0.000 claims description 11
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000003795 desorption Methods 0.000 claims description 7
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 238000002481 ethanol extraction Methods 0.000 claims description 4
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 4
- 238000003809 water extraction Methods 0.000 claims description 3
- 239000008347 soybean phospholipid Substances 0.000 claims 1
- 238000000746 purification Methods 0.000 abstract description 15
- 238000001179 sorption measurement Methods 0.000 abstract description 6
- 235000013361 beverage Nutrition 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 description 11
- 239000000469 ethanolic extract Substances 0.000 description 9
- 239000008280 blood Substances 0.000 description 6
- 210000004369 blood Anatomy 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- 230000001603 reducing effect Effects 0.000 description 4
- 241000759833 Cornus officinalis Species 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000004587 chromatography analysis Methods 0.000 description 3
- 239000012467 final product Substances 0.000 description 3
- YTZSBJLNMIQROD-SFBCHFHNSA-N Morroniside Chemical compound O([C@@H]1OC=C([C@H]2C[C@H](O)O[C@@H](C)[C@H]21)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O YTZSBJLNMIQROD-SFBCHFHNSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000005070 sampling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- YTZSBJLNMIQROD-UHFFFAOYSA-N (4aS)-1c-beta-D-glucopyranosyloxy-6xi-hydroxy-8t-methyl-(4ar,8ac)-5,6,8,8a-tetrahydro-1H,4aH-pyrano[3,4-c]pyran-4-carboxylic acid methyl ester Natural products C12C(C)OC(O)CC2C(C(=O)OC)=COC1OC1OC(CO)C(O)C(O)C1O YTZSBJLNMIQROD-UHFFFAOYSA-N 0.000 description 1
- 210000002237 B-cell of pancreatic islet Anatomy 0.000 description 1
- 206010022489 Insulin Resistance Diseases 0.000 description 1
- AMBQHHVBBHTQBF-UHFFFAOYSA-N Loganin Natural products C12C(C)C(O)CC2C(C(=O)OC)=COC1OC1OC(CO)C(O)C(O)C1O AMBQHHVBBHTQBF-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 229940095686 granule product Drugs 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- AMBQHHVBBHTQBF-UOUCRYGSSA-N loganin Chemical compound O([C@@H]1OC=C([C@H]2C[C@H](O)[C@H](C)[C@H]21)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O AMBQHHVBBHTQBF-UOUCRYGSSA-N 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- XZWYZXLIPXDOLR-UHFFFAOYSA-N metformin Chemical compound CN(C)C(=N)NC(N)=N XZWYZXLIPXDOLR-UHFFFAOYSA-N 0.000 description 1
- 229960003105 metformin Drugs 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003908 quality control method Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 208000001072 type 2 diabetes mellitus Diseases 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/385—Concentrates of non-alcoholic beverages
- A23L2/39—Dry compositions
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/52—Adding ingredients
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L2/00—Non-alcoholic beverages; Dry compositions or concentrates therefor; Their preparation
- A23L2/70—Clarifying or fining of non-alcoholic beverages; Removing unwanted matter
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention belongs to the technical field of solid beverages, and particularly relates to a method for preparing dogwood alcohol extract particles, which comprises the following steps: (1) uniformly mixing dry dogwood fruit powder with 70-85% (v/v) of water-alcohol solution according to the proportion of 1g (25-40) mL to prepare suspension; (2) carrying out ultrasonic extraction on the suspension, then carrying out residue-liquid separation, and reserving alcohol extraction filtrate; (3) purifying the alcohol extraction filtrate by macroporous resin; (4) adding modified soybean phospholipid and alpha-cyclodextrin into the purified alcohol extraction filtrate, stirring, homogenizing, and spray drying to obtain Corni fructus alcohol extract granule; the dosage ratio of the modified soybean lecithin, the alpha-cyclodextrin, the filter residue or the dogwood dry fruit powder is (0.002-0.005): 0.05-0.09): 1. According to the invention, macroporous resin adsorption and purification are carried out on the alcohol extraction filtrate, so that the content of ursolic acid in the dogwood alcohol extract particles is greatly improved.
Description
Technical Field
The invention belongs to the technical field of solid beverages, and particularly relates to a method for preparing alcohol extract granules of dogwood, and the alcohol extract granules prepared by the method.
Background
The dogwood is a unique traditional precious Chinese medicinal material in China, and the dogwood fruits are rich in various beneficial components such as loganin, ursolic acid, morroniside, monosaccharide, polysaccharide and the like, wherein the ursolic acid is used as one of the dogwood quality control indexes, and the ursolic acid can reduce blood sugar, regulate blood fat, eliminate in-vivo free radicals, protect pancreatic beta cells and relieve insulin resistance of organisms, so that the dogwood has the potential for medicine development. In the existing reported literature, an animal experiment is carried out on ursolic acid, according to a rat experiment, the dosage of 25mg/Kg, 50mg/Kg and 100mg/Kg is set, the blood sugar reducing effect is gradually improved along with the increase of the dosage of the medicine, when the dosage is 50mg/Kg and 100mg/Kg, the blood sugar reducing effect is obvious, and when the dosage reaches the dosage of 100mg/Kg, the medicine effect is close to that of the existing medicine metformin for reducing blood sugar. Therefore, the development of the dogwood alcohol extract particle with the blood sugar reducing effect is of great significance. However, the existing dogwood granule has a very small content of ursolic acid, and cannot achieve a good health-preserving and health-care effect.
Disclosure of Invention
The invention aims to provide a method for preparing dogwood alcohol extract particles so as to improve the content of ursolic acid in the dogwood alcohol extract. It is another object of the present invention to provide a corresponding dogwood alcohol extract granule product.
Based on the purpose, the invention adopts the technical scheme that: a method for preparing dogwood alcohol extract particles comprises the following steps:
(1) uniformly mixing dry dogwood fruit powder with 70-85% (v/v) of a hydroalcoholic solution according to the proportion of 1g (25-40) mL to prepare a suspension, or performing residue-liquid separation after water extraction on the dry dogwood fruit powder, reserving filter residues and drying the filter residues, and uniformly mixing the dried filter residues with 70-85% (v/v) of the hydroalcoholic solution according to the proportion of 1g (20-30) mL to prepare the suspension;
(2) carrying out ultrasonic extraction on the suspension, then carrying out residue-liquid separation, and retaining an alcohol extraction filtrate;
(3) purifying the alcohol extraction filtrate by macroporous resin;
(4) adding modified soybean phospholipid and alpha-cyclodextrin into the purified alcohol extraction filtrate, stirring, homogenizing, and spray drying to obtain Corni fructus alcohol extract granule; the dosage ratio of the modified soybean lecithin, the alpha-cyclodextrin and the filter residue or the dogwood dry fruit powder is as follows: (0.002-0.005): 0.05-0.09): 1.
Further, the specific process of the step (1) is as follows: uniformly mixing dry dogwood fruit powder, citric acid, acetone and water according to the weight ratio of 1 (0.02-0.04) to (10-15) to (20-30), performing ultrasonic extraction at 20-30 ℃ for 10-20 min, performing residue-liquid separation, retaining filter residues, and airing for later use; the ultrasonic power is 200-300W, and the interval is 2s every 3s of ultrasonic.
Further, in the step (2), the ultrasonic temperature is 30-40 ℃, the ultrasonic extraction power is 300-420 w, the total time of ultrasonic extraction is 30-50 min, and the interval is 3s every 3s of ultrasonic extraction; the number of ultrasonic extractions was 1.
Further, the specific process of purifying the alcohol extraction filtrate by macroporous resin is as follows: soaking the macroporous resin in 90% (v/v) ethanol water for 36-42 h, and filling the column, wherein the diameter-height ratio of the filled separation column is 1 (8-10); carrying out wet-process sample loading on the ethanol-extracted filtrate and the soaked macroporous resin according to the proportion of (1-2) ml to 1g, wherein the sample loading flow rate is 4-7 BV/h; then, taking 85-90% (v/v) ethanol solution with the pH of 7.5-8 as eluent for elution to obtain desorption solution, wherein the volume ratio of the eluent to the ethanol extraction filtrate is (1.2-1.5): 1; the elution flow rate is 7-10 BV/h, and the elution times are 1.
Further, the model of the macroporous resin is D101B or XDA-1B; the diameter-height ratio of the column filled with the macroporous resin is 1 (8-10).
Further, the HLB value of the modified soybean phospholipid is 5.11 to 8.96.
Further, the homogenization process is as follows: and stirring and homogenizing the alcohol extraction filtrate added with the modified soybean phospholipid and the alpha-cyclodextrin at 45-50 ℃ for 1.5-2 h.
Further, the drying is spray drying.
The dogwood alcohol extract particles prepared by the method have the ursolic acid content of 21-25% (w/w).
Compared with the prior art, the invention has the beneficial effects that:
1. the extraction solution is 70-85% (v/v) of water-alcohol solution, compared with 100% (v/v) of ethanol, the polarity of the extraction solution is appropriate, fat-soluble substances such as ursolic acid can be effectively extracted, and the best dissolution effect of the ursolic acid is achieved.
2. The invention adopts macroporous resin purification after alcohol extraction, thus greatly improving the content of ursolic acid in the dogwood alcohol extract particles.
3. The modified soybean phospholipid is added into the alcohol extract solution, has a wrapping effect on the ursolic acid, and avoids the loss of biological activity of the ursolic acid due to chemical reaction under the conditions of sunlight irradiation, high temperature, humidity, strong acid and alkali and the like; in addition, after the modified soybean lecithin wraps the ursolic acid, the ursolic acid is slowly released, and the bioavailability of the ursolic acid is improved.
4. The invention adopts the way that the alpha-cyclodextrin is added into the alcohol extraction filtrate to be used as an auxiliary stabilizer of the modified soybean phospholipid, thereby improving the stability of the modified soybean phospholipid in the processes of stirring, homogenizing and spray drying.
5. The content of ursolic acid in the dogwood alcohol extract particles prepared by the method is up to 21-25% (w/w).
Detailed Description
Example 1
A method for preparing dogwood alcohol extract particles comprises the following steps:
(1) water extraction: uniformly mixing dry dogwood fruit powder, citric acid, acetone and deionized water according to the weight ratio of 1:0.02:10:20, carrying out ultrasonic extraction for 10min at the ultrasonic temperature of 20 ℃ and the ultrasonic power of 200W, wherein the ultrasonic extraction is carried out for 2s every 3s, carrying out slag-liquid separation after ultrasonic extraction, retaining filter residues, and airing for later use.
(2) Alcohol extraction: taking a water-alcohol solution as an extracting solution, uniformly mixing the dried filter residue and an extracting solution containing ethanol with a certain volume fraction according to a material-liquid ratio of 1g to 25mL, performing ultrasonic extraction at 35 ℃ for 30min, wherein the ultrasonic power is 300w, and the interval is 3s per 3s of ultrasonic; the ultrasonic extraction frequency is 1, and the residue-liquid separation is carried out after the ultrasonic extraction and the alcohol extraction filtrate is reserved, wherein the water-alcohol solution is the ethanol water solution.
(3) The macroporous resin purification treatment process of the alcohol extraction filtrate comprises the following steps: selecting D101B or XDA-1B macroporous resin as column filling resin in the purification process, soaking the selected macroporous resin in 90% (v/v) ethanol water solution for 36h, filling the column, wherein the filled separation column has a certain diameter-height ratio, uniformly mixing ethanol extract filtrate and the soaked macroporous resin according to the proportion of 1ml:1g, carrying out wet loading, controlling the loading flow rate, then using 85% (v/v) ethanol solution with a certain pH value as eluent, controlling the elution flow rate to carry out elution, and collecting desorption and adsorption solution in the elution process, wherein the volume ratio of the eluent to the ethanol extract filtrate is 1.2: 1; the number of elution was 1.
(4) Adding modified soybean phospholipid and alpha-cyclodextrin into the purified alcohol extraction filtrate, wherein the dosage ratio of the modified soybean phospholipid, the alpha-cyclodextrin and filter residue is as follows: 0.002:0.05:1, the HLB value of the modified soybean phospholipid is 5, stirring and homogenizing, stirring at 45 ℃ for 1.5h, cooling, and spray drying the cooled solution to obtain the dogwood alcohol extract particles.
Example 2 Effect of extracts containing different volume fractions of ethanol on Ursolic acid content in alcohol extract granules of Cornus officinalis
Referring to the method for preparing alcohol extract granules of dogwood as described in example 1, the ratio of the diameter to the height of a fixed separation column is 1:8, the sampling flow rate is 4BV/h, the pH of the eluent is 7.5, the flow rate of the eluent is 7BV/h, the volume fraction of ethanol in the extract is changed, the alcohol extract granules of dogwood are prepared according to the specific value of the volume fraction of ethanol in the extract given in table 1, and the influence of the water-alcohol solutions with different volume fractions on the content of ursolic acid in the alcohol extract granules of dogwood is discussed, and the results are shown in table 1.
TABLE 1 content of ursolic acid in dogwood alcohol extract particles prepared from extracts containing different volume fractions of ethanol
| Ethanol volume fraction (%) | 40 | 50 | 60 | 70 | 75 | 80 | 85 | 90 | 100 |
| Content of Ursolic acid (%) | 10.36 | 13.51 | 16.27 | 21.33 | 23.02 | 24.62 | 22.05 | 15.89 | 12.52 |
The result shows that along with the increase of the volume fraction of the ethanol in the extracting solution, the content of the ursolic acid in the dogwood alcohol extract particles extracted and prepared from the extracting solution tends to increase firstly and then decrease; when the volume fraction of ethanol in the extracting solution is 70-85%, the content of ursolic acid in the prepared dogwood alcohol extract particles is obviously higher than that of ethanol in a water-alcohol solution and is lower than 70% or higher than 85%; when the volume fraction of ethanol in the extracting solution is 80%, the content of ursolic acid in the dogwood alcohol extract particles extracted and prepared by the water-alcohol solution is the highest.
Results show that when the ethanol content in the extracting solution is lower than 70%, the requirements of ursolic acid on the polarity range of the extracting agent during dissolution are not met, and the content of the ursolic acid in the final alcohol extract particles is reduced; when the ethanol concentration in the extracting solution is higher than 85%, the dissolution of other fat-soluble substances in the dogwood is improved, the dissolution of ursolic acid is interfered, and the content of the ursolic acid in the extract is in a descending trend along with the increase of the ethanol content.
Example 3 Effect of macroporous resin purification on Ursolic acid content in alcohol extract granule of Cornus officinalis
Referring to the method for preparing alcohol extract granules of dogwood as described in example 1, the volume fraction of ethanol in the extract in the fixing step (2) is 80%, the diameter-height ratio of the separation column in the step (3) is 1:8, the flow rate of the sample loading is 4BV/h, the pH of the eluent is 7.5, the flow rate of the eluent is 7BV/h, the alcohol extract granules of dogwood prepared according to the steps (1), (2), (3) and (4) of the method as described in example 1 are used as a sample 1, the alcohol extract granules of dogwood prepared according to the steps (1), (2) and (4) of the method as described in example 1 are used as a comparative sample 1, that is, the comparative sample 1 is not purified by macroporous resin adsorption in the preparation process; the content of ursolic acid in sample 1 and comparative sample 1 was tested, and the content of ursolic acid in sample 1 and comparative sample 1 was 25.32% (w/w) and 1.62% (w/w), respectively. The result shows that after the ethanol extraction filtrate is subjected to macroporous resin purification treatment, impurities in the ethanol extraction filtrate are effectively removed, and the percentage content of ursolic acid in the dogwood ethanol extract particles is increased.
Example 4 Effect of different macroporous resin purification conditions on Ursolic acid content in alcohol extract granule of Cornus officinalis
(I) influence of different diameter-height ratios on ursolic acid content in dogwood alcohol extract particles
Referring to the method for preparing dogwood alcohol extract particles in example 1, the volume fraction of ethanol in the extracting solution in the step (2) is fixed to be 80%, the sampling flow rate in the step (3) is 4BV/h, the pH value of the eluent is 7.5, and the flow rate of the eluent is 7BV/h, macroporous resins with different amounts are added into separation columns, so that the chromatography columns filled with the columns have different diameter-height ratios, the influence of the chromatography columns with different diameter-height ratios on the content of ursolic acid in the dogwood alcohol extract particles is analyzed, and the experimental results are shown in table 2.
TABLE 2 influence of chromatographic columns with different diameter-height ratios on the content of ursolic acid in the alcohol extract granules of Corni fructus
| Aspect ratio of the column | 1:5 | 1:6 | 1:7 | 1:8 | 1:9 | 1:10 |
| Content of Ursolic acid (%) | 8.92 | 13.05 | 17.89 | 21.33 | 24.65 | 25.65 |
The result shows that along with the reduction of the diameter-height ratio of the macroporous resin filled in the separation column, namely, when the diameter of the section is kept consistent and the height of the filled macroporous resin is gradually increased, the content of the ursolic acid in the prepared dogwood alcohol extract particles is increased.
And result analysis shows that macroporous resins with different heights are filled in the same separation column, so that the separation effect of the ursolic acid is influenced to a certain extent, and the purification effect of the ursolic acid is more obvious along with the increase of the filling height of the macroporous resins.
(II) influence of different sample loading flow rates on ursolic acid content in dogwood alcohol extract particles
Referring to the method for preparing dogwood alcohol extract particles as described in example 1, the volume fraction of ethanol in the extract in the fixing step (2) is 80%, the diameter-height ratio of the chromatographic column formed by the macroporous resin in the step (3) is 1:10, the pH value of the eluent is 7.5, and the flow rate of the eluent is 7BV/h, and the influence of different sample loading flow rates on the ursolic acid content in the dogwood alcohol extract particles is studied, and the results are shown in table 3.
TABLE 3 Effect of different sample application flow rates on Ursolic acid content in alcohol extract granule of Corni fructus
| Sample flow rate (BV/h) | 4 | 5 | 6 | 7 | 8 | 9 | 10 |
| Content of Ursolic acid (%) | 25.73 | 24.71 | 23.52 | 21.33 | 19.56 | 17.20 | 15.32 |
The result shows that the content of the ursolic acid in the dogwood alcohol extract particles is in a descending trend along with the increase of the sample loading flow rate.
And result analysis shows that the sample loading flow rate is accelerated, so that the adsorption and purification of the ursolic acid by the macroporous resin are not facilitated, the separation efficiency of the chromatographic column on the ursolic acid is reduced, and the content of the ursolic acid in the final product of the dogwood alcohol extract particles is reduced.
(III) influence of different elution flow rates on ursolic acid content in dogwood alcohol extract particles
Referring to the method for preparing dogwood alcohol extract particles in example 1, the volume fraction of ethanol in the extracting solution in the fixing step (2) is 80%, the diameter-height ratio of the chromatographic column formed by the macroporous resin in the step (3) is 1:10, the sample loading flow rate is 4BV/h, the pH value of the eluent is 8, the influence of different elution flow rates on the ursolic acid content in the dogwood alcohol extract particles is researched, and the results are shown in table 4.
TABLE 4 Effect of different elution flow rates on Ursolic acid content in alcohol extract granules of Corni fructus
| Elution flow Rate (BV/h) | 7 | 8 | 9 | 10 | 11 | 12 |
| Content of Ursolic acid (%) | 25.93 | 24.70 | 23.02 | 21.31 | 19.23 | 15.32 |
The result shows that along with the increase of the elution flow rate, the content of the ursolic acid in the dogwood alcohol extract particles is in a descending trend.
The result analysis shows that the elution flow rate is accelerated, so that the desorption of the ursolic acid by the macroporous resin is not facilitated, the separation efficiency of the ursolic acid adsorbed by the macroporous resin is reduced, and the content of the ursolic acid in the final product of the dogwood alcohol extract particles is reduced.
(IV) influence of eluents with different pH values on ursolic acid content in dogwood alcohol extract particles
Referring to the method for preparing dogwood alcohol extract particles as described in example 1, the volume fraction of ethanol in the extraction solution in the fixing step (2) is 80%, the diameter-height ratio of the chromatography column formed by the macroporous resin in the step (3) is 1:10, the sample loading flow rate is 4BV/h, and the elution flow rate is 7BV/h, and the influence of eluents with different pH values on the ursolic acid content in the dogwood alcohol extract particles is studied, and the results are shown in table 5.
TABLE 5 influence of eluents of different pH values on the Ursolic acid content in alcohol extract granules of Corni fructus
| pH value of the eluent | 7.5 | 7.6 | 7.7 | 7.8 | 8 | 9 |
| Content of Ursolic acid (%) | 25.07 | 23.02 | 24.71 | 23.31 | 19.03 | 15.21 |
The result shows that the content of the ursolic acid in the dogwood alcohol extract particles is in a descending trend along with the increase of the pH value of the eluent. As a result, when the pH value of the eluent is increased, elution of other organic salts is caused, and the content of the ursolic acid in the final product is reduced.
Example 5
A method for preparing dogwood alcohol extract particles comprises the following steps:
(1) mixing Corni fructus dry fruit powder with 70% (v/v) water alcohol solution at a ratio of 1g:25mL to obtain suspension, ultrasonic extracting at 30 deg.C for 50min with ultrasonic power of 300w, and intermittent for 3s per 3 s; the ultrasonic extraction frequency is 1, and the residue-liquid separation is carried out after the ultrasonic extraction and the alcohol extraction filtrate is reserved.
(2) The macroporous resin purification treatment process of the alcohol extraction filtrate comprises the following steps: selecting D101B type macroporous resin as column filling resin in the purification process, soaking the selected macroporous resin in 90% (v/v) ethanol for 42h, filling the column, wherein the diameter-height ratio of the filled separation column is 1:5, uniformly mixing ethanol extract filtrate and the soaked macroporous resin according to the proportion of 1ml:1g, carrying out wet-process sample loading, controlling the sample loading flow rate to be 4BV/h, then using 90% (v/v) ethanol solution with the pH value of 8 as eluent, controlling the elution flow rate to be 7BV/h, and collecting desorption adsorption solution in the elution process, wherein the volume ratio of the eluent to the ethanol extract filtrate is 1.2: 1; the number of elution was 1.
(3) Adding modified soybean phospholipid and alpha-cyclodextrin into the purified alcohol extraction filtrate, wherein the dosage ratio of the modified soybean phospholipid to the alpha-cyclodextrin to the dogwood dry fruit powder is 0.002:0.05:1, the HLB value of the modified soybean phospholipid is 5.11, stirring and homogenizing, stirring at 45 ℃ for 1.5h, cooling, and spray drying the cooled solution to obtain the dogwood alcohol extract particles. The content of ursolic acid in the prepared dogwood alcohol extract particles is 21.38% (w/w).
Example 6
A method for preparing dogwood alcohol extract particles comprises the following steps:
(1) mixing Corni fructus dry fruit powder with 85% (v/v) water-alcohol solution at a ratio of 1g:40mL to obtain suspension, ultrasonic extracting at 40 deg.C for 30min with ultrasonic power of 420w, and intermittent for 3s per 3 s; the ultrasonic extraction frequency is 1, and the residue-liquid separation is carried out after the ultrasonic extraction and the alcohol extraction filtrate is reserved.
(2) The macroporous resin purification treatment process of the alcohol extraction filtrate comprises the following steps: selecting XDA-1B type macroporous resin as column filling resin in the purification process, soaking the selected macroporous resin in 90% (v/v) ethanol for 36h, filling the column, wherein the diameter-height ratio of the filled separation column is 1:10, uniformly mixing ethanol extract filtrate and the soaked macroporous resin according to the proportion of 2ml to 1g, carrying out wet-method sample loading, controlling the sample loading flow rate to be 7BV/h, then using 85% (v/v) ethanol solution with the pH value of 7.5 as eluent, controlling the elution flow rate to be 10BV/h, eluting, and collecting desorption and adsorption solution in the elution process, wherein the volume ratio of the eluent to the ethanol extract filtrate is 1.5: 1; the number of elution was 1.
(3) Adding modified soybean phospholipid and alpha-cyclodextrin into the purified alcohol extraction filtrate, wherein the dosage ratio of the modified soybean phospholipid to the alpha-cyclodextrin to the dogwood dry fruit powder is 0.005:0.09:1, the HLB value of the modified soybean phospholipid is 8.96, stirring and homogenizing, stirring at 45 ℃ for 2 hours, cooling, and spray drying the cooled solution to obtain the dogwood alcohol extract particles. The content of ursolic acid in the prepared dogwood alcohol extract particles is 24.37% (w/w).
Example 7
A method for preparing dogwood alcohol extract particles comprises the following steps:
(1) mixing Corni fructus dry fruit powder with 80% (v/v) water alcohol solution at a ratio of 1g:35mL to obtain suspension, ultrasonic extracting at 35 deg.C for 40min with ultrasonic power of 380w, and intermittent for 3s per 3 s; the ultrasonic extraction frequency is 1, and the residue-liquid separation is carried out after the ultrasonic extraction and the alcohol extraction filtrate is reserved.
(2) The macroporous resin purification treatment process of the alcohol extraction filtrate comprises the following steps: selecting D101B type macroporous resin as column filling resin in the purification process, soaking the selected macroporous resin in 90% (v/v) ethanol for 40h, filling the column, wherein the diameter-height ratio of the filled separation column is 1:8, uniformly mixing ethanol extract filtrate and the soaked macroporous resin according to the proportion of 1.5ml:1g, carrying out wet-method sample loading, controlling the sample loading flow rate to be 5.5BV/h, then using 88% (v/v) ethanol solution with the pH value of 7.8 as eluent, controlling the elution flow rate to be 8.5BV/h, and collecting desorption solution in the elution process, wherein the volume ratio of the eluent to the ethanol extract filtrate is 1.3: 1; the number of elution was 1.
(3) Adding modified soybean phospholipid and alpha-cyclodextrin into the purified alcohol extract filtrate, wherein the dosage ratio of the modified soybean phospholipid to the alpha-cyclodextrin to the dogwood dry fruit powder is 0.003:0.07:1, the HLB value of the modified soybean phospholipid is 6.26, stirring and homogenizing, stirring at 48 ℃ for 1.8h, cooling, and spray drying the cooled solution to obtain the dogwood alcohol extract particles. The content of ursolic acid in the obtained Corni fructus alcohol extract granule is 22.65% (w/w).
Claims (8)
1. The method for preparing the dogwood alcohol extract particles is characterized by comprising the following steps of:
(1) uniformly mixing dry dogwood fruit powder with 70-85% (v/v) of a hydroalcoholic solution according to the proportion of 1g (25-40) mL to prepare a suspension, or performing residue-liquid separation after water extraction on the dry dogwood fruit powder, reserving filter residues and drying the filter residues, and uniformly mixing the dried filter residues with 70-85% (v/v) of the hydroalcoholic solution according to the proportion of 1g (20-30) mL to prepare the suspension;
(2) carrying out ultrasonic extraction on the suspension, then carrying out residue-liquid separation, and retaining an alcohol extraction filtrate;
(3) purifying the alcohol extraction filtrate by macroporous resin;
(4) adding modified soybean phospholipid and alpha-cyclodextrin into the purified alcohol extraction filtrate, stirring, homogenizing, and spray drying to obtain Corni fructus alcohol extract granule; the dosage ratio of the modified soybean lecithin, the alpha-cyclodextrin and the filter residue or the dogwood dry fruit powder is as follows: (0.002-0.005): 0.05-0.09): 1.
2. The method for preparing alcohol extract granules of dogwood according to claim 1, wherein the specific process of the step (1) is as follows: uniformly mixing dry dogwood fruit powder, citric acid, acetone and water according to the weight ratio of 1 (0.02-0.04) to (10-15) to (20-30), performing ultrasonic extraction at 20-30 ℃ for 10-20 min, performing residue-liquid separation, retaining filter residues, and airing for later use; the ultrasonic power is 200-300W, and the interval is 2s every 3s of ultrasonic.
3. The method for preparing dogwood alcohol extract particles according to claim 1 or 2, wherein the ultrasonic extraction temperature in the step (2) is 30-40 ℃, the ultrasonic power is 300-420 w, the total time of ultrasonic extraction is 30-50 min, and the interval is 3s per 3s of ultrasonic; the number of ultrasonic extractions was 1.
4. The method for preparing alcohol extract granules of dogwood according to claim 3, wherein the specific process of purifying the alcohol extract filtrate by macroporous resin is as follows: soaking the macroporous resin in 90% (v/v) ethanol water for 36-42 h, and filling the column, wherein the diameter-height ratio of the filled separation column is 1 (8-10); carrying out wet-process sample loading on the ethanol-extracted filtrate and the soaked macroporous resin according to the proportion of (1-2) ml to 1g, wherein the sample loading flow rate is 4-7 BV/h; and then, taking 85-90% (v/v) ethanol solution with the pH of 7.5-8 as eluent for elution to obtain desorption solution, wherein the volume ratio of the eluent to the ethanol extraction filtrate is (1.2-1.5): 1, and the elution flow rate is 7-10 BV/h.
5. The method for preparing alcohol extract granules of fructus corni according to claim 4, wherein the HLB value of the modified soybean phospholipids is 5.11-8.96.
6. The method for preparing alcohol extract granules of fructus corni as claimed in claim 5, wherein the homogenizing process comprises: and stirring and homogenizing the alcohol extraction filtrate added with the modified soybean phospholipid and the alpha-cyclodextrin at 45-50 ℃ for 1.5-2 h.
7. The method for preparing alcohol extract granules of fructus corni according to claim 6, wherein the drying is spray drying.
8. The dogwood alcohol extract particle prepared by the method for preparing the dogwood alcohol extract particle according to any one of claims 1 to 7, wherein the content of ursolic acid in the dogwood alcohol extract particle is 21 to 25% (w/w).
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