CN114246288A - Method for improving preservation efficiency of rosmarinic acid in rosemary material - Google Patents
Method for improving preservation efficiency of rosmarinic acid in rosemary material Download PDFInfo
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- CN114246288A CN114246288A CN202111670672.XA CN202111670672A CN114246288A CN 114246288 A CN114246288 A CN 114246288A CN 202111670672 A CN202111670672 A CN 202111670672A CN 114246288 A CN114246288 A CN 114246288A
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- DOUMFZQKYFQNTF-WUTVXBCWSA-N (R)-rosmarinic acid Chemical compound C([C@H](C(=O)O)OC(=O)\C=C\C=1C=C(O)C(O)=CC=1)C1=CC=C(O)C(O)=C1 DOUMFZQKYFQNTF-WUTVXBCWSA-N 0.000 title claims abstract description 44
- ZZAFFYPNLYCDEP-HNNXBMFYSA-N Rosmarinsaeure Natural products OC(=O)[C@H](Cc1cccc(O)c1O)OC(=O)C=Cc2ccc(O)c(O)c2 ZZAFFYPNLYCDEP-HNNXBMFYSA-N 0.000 title claims abstract description 22
- 238000000034 method Methods 0.000 title claims abstract description 22
- DOUMFZQKYFQNTF-MRXNPFEDSA-N rosemarinic acid Natural products C([C@H](C(=O)O)OC(=O)C=CC=1C=C(O)C(O)=CC=1)C1=CC=C(O)C(O)=C1 DOUMFZQKYFQNTF-MRXNPFEDSA-N 0.000 title claims abstract description 22
- TVHVQJFBWRLYOD-UHFFFAOYSA-N rosmarinic acid Natural products OC(=O)C(Cc1ccc(O)c(O)c1)OC(=Cc2ccc(O)c(O)c2)C=O TVHVQJFBWRLYOD-UHFFFAOYSA-N 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 title claims abstract description 18
- 238000004321 preservation Methods 0.000 title claims abstract description 15
- 241001529742 Rosmarinus Species 0.000 title claims abstract 12
- 238000001035 drying Methods 0.000 claims abstract description 31
- 238000011282 treatment Methods 0.000 claims abstract description 19
- 238000007710 freezing Methods 0.000 claims abstract description 15
- 230000008014 freezing Effects 0.000 claims abstract description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000001291 vacuum drying Methods 0.000 claims abstract description 14
- 238000004108 freeze drying Methods 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 9
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 7
- 238000001514 detection method Methods 0.000 claims abstract description 6
- 238000003306 harvesting Methods 0.000 claims abstract description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- 238000007789 sealing Methods 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000011049 filling Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000005457 ice water Substances 0.000 claims description 3
- 238000004806 packaging method and process Methods 0.000 claims description 3
- 238000005192 partition Methods 0.000 claims description 3
- 239000002002 slurry Substances 0.000 claims description 3
- 239000000126 substance Substances 0.000 claims description 3
- 239000006228 supernatant Substances 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000004366 reverse phase liquid chromatography Methods 0.000 claims 1
- QRYRORQUOLYVBU-VBKZILBWSA-N carnosic acid Chemical compound CC([C@@H]1CC2)(C)CCC[C@]1(C(O)=O)C1=C2C=C(C(C)C)C(O)=C1O QRYRORQUOLYVBU-VBKZILBWSA-N 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000001100 (2S)-5,7-dihydroxy-2-(3-hydroxy-4-methoxyphenyl)chroman-4-one Substances 0.000 abstract description 3
- QUQPHWDTPGMPEX-UHFFFAOYSA-N Hesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(COC4C(C(O)C(O)C(C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-UHFFFAOYSA-N 0.000 abstract description 3
- QUQPHWDTPGMPEX-UTWYECKDSA-N aurantiamarin Natural products COc1ccc(cc1O)[C@H]1CC(=O)c2c(O)cc(O[C@@H]3O[C@H](CO[C@@H]4O[C@@H](C)[C@H](O)[C@@H](O)[C@H]4O)[C@@H](O)[C@H](O)[C@H]3O)cc2O1 QUQPHWDTPGMPEX-UTWYECKDSA-N 0.000 abstract description 3
- APSNPMVGBGZYAJ-GLOOOPAXSA-N clematine Natural products COc1cc(ccc1O)[C@@H]2CC(=O)c3c(O)cc(O[C@@H]4O[C@H](CO[C@H]5O[C@@H](C)[C@H](O)[C@@H](O)[C@H]5O)[C@@H](O)[C@H](O)[C@H]4O)cc3O2 APSNPMVGBGZYAJ-GLOOOPAXSA-N 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- VUYDGVRIQRPHFX-UHFFFAOYSA-N hesperidin Natural products COc1cc(ccc1O)C2CC(=O)c3c(O)cc(OC4OC(COC5OC(O)C(O)C(O)C5O)C(O)C(O)C4O)cc3O2 VUYDGVRIQRPHFX-UHFFFAOYSA-N 0.000 abstract description 3
- QUQPHWDTPGMPEX-QJBIFVCTSA-N hesperidin Chemical compound C1=C(O)C(OC)=CC=C1[C@H]1OC2=CC(O[C@H]3[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]4[C@@H]([C@H](O)[C@@H](O)[C@H](C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-QJBIFVCTSA-N 0.000 abstract description 3
- 229940025878 hesperidin Drugs 0.000 abstract description 3
- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 abstract description 3
- 244000178231 Rosmarinus officinalis Species 0.000 description 28
- 241000196324 Embryophyta Species 0.000 description 2
- 241001072256 Boraginaceae Species 0.000 description 1
- 241000207923 Lamiaceae Species 0.000 description 1
- 244000269722 Thea sinensis Species 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005779 cell damage Effects 0.000 description 1
- 208000037887 cell injury Diseases 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- -1 phenolic acid compound Chemical class 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Images
Classifications
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- 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/40—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
- A23L3/44—Freeze-drying
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F3/00—Tea; Tea substitutes; Preparations thereof
- A23F3/06—Treating tea before extraction; Preparations produced thereby
- A23F3/14—Tea preparations, e.g. using additives
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23F—COFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
- A23F3/00—Tea; Tea substitutes; Preparations thereof
- A23F3/16—Tea extraction; Tea extracts; Treating tea extract; Making instant tea
- A23F3/163—Liquid or semi-liquid tea extract preparations, e.g. gels, liquid extracts in solid capsules
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- 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
- A23L3/00—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
- A23L3/34—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
- A23L3/3409—Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals in the form of gases, e.g. fumigation; Compositions or apparatus therefor
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- 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
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- A61K31/21—Esters, e.g. nitroglycerine, selenocyanates
- A61K31/215—Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids
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- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
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- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Abstract
The invention discloses a method for improving the preservation efficiency of rosmarinic acid in rosemary materials, which comprises the following steps: s1, picking: harvesting fresh rosemary leaves, and removing stems; s2, sample cleaning: cleaning the collected leaves, and drying the leaves by using a drying machine; s3, sample pre-freezing: pre-freezing the cleaned and dried sample in an ultra-low temperature refrigerator or liquid nitrogen; s4, freeze vacuum drying: and (3) putting the sample subjected to the pre-freezing treatment in the step into a freeze dryer for drying treatment, and then performing freeze-drying treatment. By adopting the detection and preservation method designed by the invention, after the fresh rosemary leaves are treated by the freeze vacuum drying technology, the preservation effect of the freeze vacuum drying on the rosmarinic acid which is an effective component in the rosemary is very obvious, after the rosemary is treated by the freeze vacuum drying technology, the content of the rosmarinic acid is 11.26 times of the content after common drying, and the content of the hesperidin and the content of the carnosic acid are respectively 1.64 times and 1.66 times of the content after common drying.
Description
Technical Field
The invention relates to the technical field of rosemary, in particular to a method for improving the storage efficiency of rosmarinic acid in rosemary materials.
Background
Rosmarinic acid is a water-soluble natural phenolic acid compound separated from rosemary, is a natural antioxidant, is helpful for preventing cell damage caused by free radicals, has strong anti-inflammatory activity, is widely applied to the fields of pharmacy, food, cosmetics and the like, at present, rosmarinic acid is mainly extracted from labiatae and Boraginaceae plants, rosemary is more applied to the preparation of herb tea drinks and diet, and the fresh leaves are easy to mildew and pollute due to short preservation time, and are mostly preserved in a drying mode after being picked, but the drying treatment can greatly reduce the loss of the rosmarinic acid serving as an effective component in the rosemary.
Disclosure of Invention
The invention aims to provide a method for improving the preservation efficiency of rosmarinic acid in rosemary materials, which has the advantage of high preservation efficiency and solves the problems in the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a method for improving the preservation efficiency of rosmarinic acid in rosemary materials comprises the following steps:
s1, picking: harvesting fresh rosemary leaves, and removing stems;
s2, sample cleaning: cleaning the collected leaves, and drying the leaves by using a drying machine;
s3, sample pre-freezing: pre-freezing the cleaned and dried sample in an ultra-low temperature refrigerator or liquid nitrogen;
s4, freeze vacuum drying: putting the sample subjected to the pre-freezing treatment in the step into a freeze dryer for drying treatment, then carrying out freeze-drying treatment, and finally taking out the sample after shutdown;
s5, content detection: weighing 0.1g of vacuum freeze-dried/oven-dried herba Rosmarini officinalis sample, adding 10ml of 80% methanol aqueous solution, grinding to slurry, ultrasonic extracting in ice water bath for 50min, centrifuging to extract supernatant, filtering, and determining with chromatograph;
s6, vacuumizing and storing the dried materials: and (4) filling the dried rosemary material into a packaging bag, and pumping air out of the bag by using a vacuum sealing machine for sealing.
Preferably, the temperature of the ultra-low temperature refrigerator in the step S3 is-80 ℃, and the temperature of the liquid nitrogen is-196 ℃.
Preferably, in the step S4, the reference model of the freeze dryer is CHRIST ALPHA 1-2, a Manual → Freezing + Warm-Up VP mode is selected, a Run key is pressed to enter a cold trap pre-cooling and vacuum pump pre-heating stage, after the stage is finished, the pre-frozen rosemary plant sample and the partition plate are placed in a drying chamber of the freeze dryer, a Manual → Main → drying mode is selected to enter a Main freeze-drying stage (vacuum pumping is started in a cavity at this time), and when the vacuum degree reaches a set value, the rosemary material is dried until the weight is constant, generally 24-72 hours are needed, and then a Manual → Final-drying mode is selected to perform post-freeze-drying treatment (the time of the step is not too long).
Preferably, in step S5, the content of rosmarinic acid and other substances under two treatments is calculated by measuring with Agilent1100 high performance liquid chromatograph, wavelength is 284nm, and reverse phase chromatographic column Compass C18(2) (250mm × 4.6mm, 5 μm).
Compared with the prior art, the invention has the following beneficial effects:
1. by adopting the detection and preservation method designed by the invention, after the fresh rosemary leaves are treated by the freeze vacuum drying technology, the preservation effect of the freeze vacuum drying on the rosmarinic acid which is an effective component in the rosemary is very obvious, after the rosemary is treated by the freeze vacuum drying technology, the content of the rosmarinic acid is 11.26 times of the content after common drying, and the content of the hesperidin and the content of the carnosic acid are respectively 1.64 times and 1.66 times of the content after common drying.
2. The method provided by the invention is accurate and effective, and compared with the content of the rosmarinic acid in the rosemary treated by the freeze vacuum drying method and the drying method, the method has obvious advantages for storing the rosmarinic acid in the rosemary material.
Drawings
FIG. 1 is a schematic flow chart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The components of the present invention are all standard components or components known to those skilled in the art, and the structure and principle thereof can be known to those skilled in the art through technical manuals or through routine experimentation.
Referring to fig. 1, a method for improving the preservation efficiency of rosmarinic acid in rosemary material comprises the following steps:
s1, picking: harvesting fresh rosemary leaves, and removing stems;
s2, sample cleaning: cleaning the collected leaves, and drying the leaves by using a drying machine;
s3, sample pre-freezing: pre-freezing the cleaned and dried sample in an ultra-low temperature refrigerator or liquid nitrogen, wherein the temperature of the ultra-low temperature refrigerator is-80 ℃, and the temperature of the liquid nitrogen is-196 ℃;
s4, freeze vacuum drying: putting the sample subjected to the pre-Freezing treatment in a freeze dryer for drying treatment, then performing freeze-drying treatment, finally taking out the sample after shutdown, wherein the reference model of the freeze dryer is CHRIST ALPHA 1-2, selecting a Manual → Freezing + Warm-Up VP mode, entering a cold trap pre-cooling and vacuum pump pre-heating stage by pressing a Run key, placing the pre-frozen rosemary plant sample and a partition plate in a drying chamber of the freeze dryer after the stage is finished, selecting the Manual → Main → drying mode to enter a Main freeze-drying stage (vacuumizing is started in a cavity at the moment), drying until the rosemary material is constant weight under the condition that the vacuum degree reaches a set value, generally requiring 24-72 hours, and then selecting the Manual → Fiil-drying mode for post-freeze-drying treatment (the step is not too long);
s5, content detection: weighing 0.1g of vacuum freeze-dried/dried rosemary sample, adding 10ml of 80% methanol aqueous solution, grinding into slurry, performing ultrasonic extraction in ice-water bath for 50min, centrifuging to extract supernatant, filtering, measuring by using a chromatograph, measuring by using an Agilent1100 high performance liquid chromatograph, measuring by using a reverse phase chromatographic column Compass C18(2) (250mm x 4.6mm, 5 mu m), and comparing and calculating the content of rosmarinic acid and other substances under two treatments;
s6, vacuumizing and storing the dried materials: the method comprises the steps of filling dried rosemary materials into a packaging bag, pumping air out of the bag by using a vacuum sealing machine for sealing, and finding that the freeze vacuum drying has extremely remarkable preservation effect on the active ingredient rosmarinic acid in the rosemary by adopting the detection preservation method designed by the invention after the fresh leaves of the rosemary are treated by the freeze vacuum drying technology, wherein after the rosemary is treated by the freeze vacuum drying technology, the content of the rosmarinic acid is 11.26 times of the content of the rosemary after common drying, and the content of hesperidin and carnosic acid are respectively 1.64 times and 1.66 times of the content of the rosemary after common drying.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (4)
1. A method for improving the preservation efficiency of rosmarinic acid in rosemary materials is characterized by comprising the following steps: the method comprises the following steps:
s1, picking: harvesting fresh rosemary leaves, and removing stems;
s2, sample cleaning: cleaning the collected leaves, and drying the leaves by using a drying machine;
s3, sample pre-freezing: pre-freezing the cleaned and dried sample in an ultra-low temperature refrigerator or liquid nitrogen;
s4, freeze vacuum drying: putting the sample subjected to the pre-freezing treatment in the step into a freeze dryer for drying treatment, then carrying out freeze-drying treatment, and finally taking out the sample after shutdown;
s5, content detection: weighing 0.1g of vacuum freeze-dried/oven-dried herba Rosmarini officinalis sample, adding 10ml of 80% methanol aqueous solution, grinding to slurry, ultrasonic extracting in ice water bath for 50min, centrifuging to extract supernatant, filtering, and determining with chromatograph;
s6, vacuumizing and storing the dried materials: and (4) filling the dried rosemary material into a packaging bag, and pumping air out of the bag by using a vacuum sealing machine for sealing.
2. The method of claim 1, wherein the method comprises the steps of: the temperature of the ultra-low temperature refrigerator in the step S3 is-80 ℃, and the temperature of the liquid nitrogen is-196 ℃.
3. The method of claim 1, wherein the method comprises the steps of: in the step S4, the reference model of the freeze dryer is CHRIST ALPHA 1-2, a Manual → Freezing + Warm-Up VP mode is selected, a Run key is pressed to enter a cold trap pre-cooling and vacuum pump pre-heating stage, after the stage is finished, the pre-frozen rosemary plant sample and a partition plate are placed in a drying chamber of the freeze dryer, the Manual → Main → drying mode is selected to enter a Main freeze-drying stage (vacuum pumping is started in a cavity at this time), when the vacuum degree reaches a set value state, the rosemary plant sample is dried until the weight of the rosemary material is constant, generally 24-72 hours are needed, and then the Manual → Final-drying mode is selected to carry out post-freeze-drying treatment (the time of the step is not too long).
4. The method of claim 1, wherein the method comprises the steps of: in step S5, the content of rosmarinic acid and other substances under two treatments was calculated by measuring with Agilent1100 hplc, wavelength 284nm, reverse phase chromatography column Compass C18(2) (250mm × 4.6mm, 5 μm).
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CN110283226A (en) * | 2019-08-06 | 2019-09-27 | 桂林莱茵生物科技股份有限公司 | A kind of method of antioxidant content in extraction rosemary |
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CN101849536A (en) * | 2010-05-27 | 2010-10-06 | 东北林业大学 | Method for keeping stable contents of carnosic acid and rosmarinic acid in rosemary stems and leaves after picking |
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CN105661404A (en) * | 2016-03-25 | 2016-06-15 | 国家林业局泡桐研究开发中心 | Dried astringent persimmon processing method |
CN110283226A (en) * | 2019-08-06 | 2019-09-27 | 桂林莱茵生物科技股份有限公司 | A kind of method of antioxidant content in extraction rosemary |
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CN115486530A (en) * | 2022-10-21 | 2022-12-20 | 湖南祥民制药有限公司 | Rosemary freeze-drying method |
CN115486530B (en) * | 2022-10-21 | 2024-03-26 | 湖南祥民制药有限公司 | Freeze-drying method of rosemary |
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