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 PDF

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Publication number
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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drying
rosemary
freeze
sample
freezing
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CN114246288B (en
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万晓
田丹青
葛亚英
潘晓韵
谢卢鹏
周媛
潘刚敏
朱强
姚兴达
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Zhejiang Institute Of Landscape Plants And Flowers
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Zhejiang Institute Of Landscape Plants And Flowers
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/40Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by drying or kilning; Subsequent reconstitution
    • A23L3/44Freeze-drying
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/06Treating tea before extraction; Preparations produced thereby
    • A23F3/14Tea preparations, e.g. using additives
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23FCOFFEE; TEA; THEIR SUBSTITUTES; MANUFACTURE, PREPARATION, OR INFUSION THEREOF
    • A23F3/00Tea; Tea substitutes; Preparations thereof
    • A23F3/16Tea extraction; Tea extracts; Treating tea extract; Making instant tea
    • A23F3/163Liquid or semi-liquid tea extract preparations, e.g. gels, liquid extracts in solid capsules
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L3/00Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs
    • A23L3/34Preservation of foods or foodstuffs, in general, e.g. pasteurising, sterilising, specially adapted for foods or foodstuffs by treatment with chemicals
    • A23L3/3409Preservation 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
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L33/00Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K31/00Medicinal preparations containing organic active ingredients
    • A61K31/21Esters, e.g. nitroglycerine, selenocyanates
    • A61K31/215Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids
    • A61K31/216Esters, e.g. nitroglycerine, selenocyanates of carboxylic acids of acids having aromatic rings, e.g. benactizyne, clofibrate
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/37Esters of carboxylic acids
    • A61K8/375Esters of carboxylic acids the alcohol moiety containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P29/00Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P39/00General protective or antinoxious agents
    • A61P39/06Free radical scavengers or antioxidants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • A61Q19/08Anti-ageing preparations
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food 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

Method for improving preservation efficiency of rosmarinic acid in rosemary material
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).
CN202111670672.XA 2021-12-31 2021-12-31 Method for improving preservation efficiency of rosmarinic acid in rosemary material Active CN114246288B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115486530A (en) * 2022-10-21 2022-12-20 湖南祥民制药有限公司 Rosemary freeze-drying method

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102318828A (en) * 2011-08-05 2012-01-18 中国林业科学研究院林产化学工业研究所 Ultrasonic wave assisted extraction method of rosemary anti-oxidant
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN102318828A (en) * 2011-08-05 2012-01-18 中国林业科学研究院林产化学工业研究所 Ultrasonic wave assisted extraction method of rosemary anti-oxidant
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

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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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