CN115282186A - Freeze-drying method of radix fici simplicissimae and dry powder of radix fici simplicissimae - Google Patents
Freeze-drying method of radix fici simplicissimae and dry powder of radix fici simplicissimae Download PDFInfo
- Publication number
- CN115282186A CN115282186A CN202210850574.2A CN202210850574A CN115282186A CN 115282186 A CN115282186 A CN 115282186A CN 202210850574 A CN202210850574 A CN 202210850574A CN 115282186 A CN115282186 A CN 115282186A
- Authority
- CN
- China
- Prior art keywords
- hispid
- freeze
- drying
- fici simplicissimae
- radix fici
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 238000000034 method Methods 0.000 title claims abstract description 43
- 239000000843 powder Substances 0.000 title claims abstract description 42
- 238000004108 freeze drying Methods 0.000 title claims abstract description 28
- 238000009777 vacuum freeze-drying Methods 0.000 claims abstract description 26
- 238000005520 cutting process Methods 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 11
- 238000003892 spreading Methods 0.000 claims abstract description 7
- 230000007480 spreading Effects 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000007710 freezing Methods 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 238000010521 absorption reaction Methods 0.000 claims description 2
- 238000005192 partition Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- ZCCUUQDIBDJBTK-UHFFFAOYSA-N psoralen Chemical compound C1=C2OC(=O)C=CC2=CC2=C1OC=C2 ZCCUUQDIBDJBTK-UHFFFAOYSA-N 0.000 abstract description 102
- VXGRJERITKFWPL-UHFFFAOYSA-N 4',5'-Dihydropsoralen Natural products C1=C2OC(=O)C=CC2=CC2=C1OCC2 VXGRJERITKFWPL-UHFFFAOYSA-N 0.000 abstract description 51
- 229930003944 flavone Natural products 0.000 abstract description 32
- 235000011949 flavones Nutrition 0.000 abstract description 32
- 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 abstract description 31
- 150000002212 flavone derivatives Chemical class 0.000 abstract description 31
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 abstract description 31
- 230000018044 dehydration Effects 0.000 abstract description 16
- 238000006297 dehydration reaction Methods 0.000 abstract description 16
- 238000007602 hot air drying Methods 0.000 abstract description 16
- 150000008442 polyphenolic compounds Chemical class 0.000 abstract description 16
- 235000013824 polyphenols Nutrition 0.000 abstract description 16
- 238000005516 engineering process Methods 0.000 abstract description 6
- 239000004480 active ingredient Substances 0.000 abstract description 5
- 150000004676 glycans Chemical class 0.000 abstract description 5
- 229920001282 polysaccharide Polymers 0.000 abstract description 5
- 239000005017 polysaccharide Substances 0.000 abstract description 5
- 238000011160 research Methods 0.000 abstract description 4
- 230000000717 retained effect Effects 0.000 abstract description 3
- 239000002352 surface water Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 28
- 239000000463 material Substances 0.000 description 15
- 244000173782 Ficus hirta Species 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000012360 testing method Methods 0.000 description 9
- 239000003153 chemical reaction reagent Substances 0.000 description 7
- 230000002829 reductive effect Effects 0.000 description 7
- 238000002835 absorbance Methods 0.000 description 6
- 238000007605 air drying Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 238000005070 sampling Methods 0.000 description 5
- 238000009423 ventilation Methods 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000000605 extraction Methods 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 229930003935 flavonoid Natural products 0.000 description 3
- 150000002215 flavonoids Chemical class 0.000 description 3
- 235000017173 flavonoids Nutrition 0.000 description 3
- 241000411851 herbal medicine Species 0.000 description 3
- 238000004128 high performance liquid chromatography Methods 0.000 description 3
- 238000007619 statistical method Methods 0.000 description 3
- 241000196324 Embryophyta Species 0.000 description 2
- 241000218218 Ficus <angiosperm> Species 0.000 description 2
- 235000011591 Ficus hirta Nutrition 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000706 filtrate Substances 0.000 description 2
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 2
- 150000002989 phenols Chemical class 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 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 description 1
- 206010011224 Cough Diseases 0.000 description 1
- 240000008168 Ficus benjamina Species 0.000 description 1
- 206010061218 Inflammation Diseases 0.000 description 1
- 241000218231 Moraceae Species 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000007865 diluting Methods 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 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 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 230000036039 immunity Effects 0.000 description 1
- 230000004054 inflammatory process Effects 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000000670 limiting effect Effects 0.000 description 1
- 238000012417 linear regression Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000012982 microporous membrane Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 210000003205 muscle Anatomy 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 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 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 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 description 1
- 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 description 1
- 235000005493 rutin Nutrition 0.000 description 1
- 229960004555 rutoside Drugs 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 210000000952 spleen Anatomy 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Images
Classifications
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/60—Moraceae (Mulberry family), e.g. breadfruit or fig
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/14—Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B5/00—Drying solid materials or objects by processes not involving the application of heat
- F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
- F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/15—Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/10—Preparation or pretreatment of starting material
- A61K2236/17—Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/85—Food storage or conservation, e.g. cooling or drying
Landscapes
- Health & Medical Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Pharmacology & Pharmacy (AREA)
- Chemical & Material Sciences (AREA)
- Veterinary Medicine (AREA)
- Public Health (AREA)
- General Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Animal Behavior & Ethology (AREA)
- Epidemiology (AREA)
- Biotechnology (AREA)
- Mycology (AREA)
- Microbiology (AREA)
- Medical Informatics (AREA)
- Botany (AREA)
- Alternative & Traditional Medicine (AREA)
- Bioinformatics & Cheminformatics (AREA)
- Molecular Biology (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Medicines Containing Plant Substances (AREA)
- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention provides a freeze-drying method of radix fici simplicissimae and dry powder of radix fici simplicissimae, comprising the following steps: cleaning fresh radix fici Simplicissimae, sucking surface water, and cutting to obtain radix fici Simplicissimae sample; then spreading the hispid fig sample in an ultra-low temperature refrigerator for precooling to obtain a hispid fig precooled product; and finally, spreading the pre-cooled hispid fig in a tray of a freeze dryer, and carrying out vacuum freeze drying, crushing and sieving to obtain hispid fig dry powder. The method adopts a vacuum freeze drying technology to dry the radix fici simplicissimae, ensures the dehydration rate of the radix fici simplicissimae, reduces the loss of psoralen, flavone and polysaccharide and ensures the dehydration rate of the radix fici simplicissimae. Compared with hot air drying treatment, the dehydration rate of the hispid fig dry powder prepared by the invention and the content of active ingredients such as psoralen, flavone, polyphenol and the like are higher, so that the medicinal value of the hispid fig is retained to the maximum extent, and a foundation is provided for the subsequent application research of the hispid fig.
Description
Technical Field
The invention relates to the technical field of Chinese herbal medicine drying, and particularly relates to a freeze-drying method of radix fici simplicissimae and dry powder of radix fici simplicissimae.
Background
Ficus hirta (Ficus hirta) is a plant of Ficus of Moraceae, is also called Ficus simplicissima lour, ficus benjamina, and Ficus macrocarpa, is usually used as a medicine by root, is mostly distributed in China south China, and is a plant used as both medicine and food. The radix fici simplicissimae has wide functions, mainly strengthens the spleen and tonifies the lung, supplements qi and eliminates dampness, relaxes the muscles and joints and dredges the collaterals, and has various pharmacological effects of resisting aging, resisting oxidation, regulating immunity, relieving cough and asthma, inhibiting bacteria and resisting inflammation and the like.
Drying treatment is an important link in medicinal material processing and is a key step influencing the quality of medicinal materials. The good drying treatment mode can effectively prevent the Chinese herbal medicines from mildewing and polluting, reduce the damage and loss of effective components and keep the drug effect to the maximum extent. The traditional drying method of the Chinese herbal medicine mainly comprises shade drying and sun drying, and has the defects of long time, low efficiency, high labor cost, greater restriction by weather factors, easy pollution, uneven product quality, poor quality and the like. The hot air drying and the cold air drying have the advantages of high drying efficiency and no influence of factors such as weather, environmental temperature and the like, and are suitable for industrial large-scale production. After the root traditional Chinese medicinal materials are treated by different drying modes, the content of the total flavonoids is found to be different, and microwave drying, sun drying and shade drying are sequentially carried out from high to low. However, the above-mentioned drying method still has problems such as incomplete drying and serious loss of active ingredients after drying.
Disclosure of Invention
The invention aims to provide a freeze-drying method of radix fici simplicissimae and dry powder of the radix fici simplicissimae, wherein the dry powder of the radix fici simplicissimae is dried by adopting a vacuum freeze-drying technology, the dehydration rate of the obtained dry powder of the radix fici simplicissimae is high, and the content of active ingredients such as psoralen, flavone, polyphenol and the like is higher than that of the traditional drying method.
The technical problem to be solved by the invention is realized by adopting the following technical scheme.
The invention provides a freeze-drying method of radix fici simplicissimae, which is characterized by comprising the following steps:
s1, taking fresh radix fici simplicissimae, cleaning, sucking surface moisture, and cutting to obtain a radix fici simplicissimae sample;
s2, paving the hispid fig sample in an ultra-low temperature refrigerator for precooling to obtain a hispid fig precooled product;
and S3, spreading the pre-cooled hispid fig in a tray of a freeze dryer, and performing vacuum freeze drying, crushing and sieving to obtain hispid fig dry powder.
The invention provides a hispid fig root dry powder which is prepared according to the freeze drying method.
The freeze-drying method of the radix fici simplicissimae and the dry powder of the radix fici simplicissimae provided by the embodiment of the invention have the beneficial effects that:
the method adopts a vacuum freeze drying technology and improves the process to dry the radix fici simplicissimae, so that the dehydration rate of the radix fici simplicissimae is ensured, the dehydration efficiency is improved, and the loss of psoralen, flavone and polysaccharide is reduced. Compared with the hot air drying method, the dehydration rate and the content of active ingredients such as psoralen, flavone, polyphenol and the like of the hispid fig dry powder prepared by the method are higher than those of the hispid fig dry powder prepared by the hot air drying method, so that the medicinal value of the hispid fig can be retained to the maximum extent. Compared with the traditional freeze drying technology, the freeze drying time is shortened, the dehydration efficiency is improved, the content of psoralen, flavone and polysaccharide in the medicinal materials is ensured, and a foundation is provided for the subsequent application research of the hispid fig.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and those skilled in the art can also obtain other related drawings based on the drawings without inventive efforts.
FIG. 1 is a chromatogram of psoralen standard and extract of radix fici Simplicissimae psoralen;
FIG. 2 is a comparison graph of the content of psoralen in freeze-dried root psoralen extract of Ficus simplicissima lour, dried root psoralen extract of Ficus simplicissima lour and traditional freeze-dried root psoralen extract of Ficus simplicissima lour;
FIG. 3 is a comparison graph of the total flavone content in the freeze-dried root total flavone extract of hispid fig, the dried root total flavone extract of hispid fig and the conventional freeze-dried root total flavone extract of hispid fig;
FIG. 4 is a comparison graph of polyphenol content in freeze-dried root polyphenol extract of hispid fig, dried root polyphenol extract of hispid fig and traditional freeze-dried root polyphenol extract of hispid fig;
fig. 5 is a flow chart of the preparation of the dry powder of hispid fig.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The freeze-drying method of hispid fig root and the dry hispid fig powder according to the embodiment of the present invention will be specifically described below.
Referring to fig. 5, a freeze-drying method for fici root provided by an embodiment of the present invention includes the following steps:
s1, taking fresh radix fici simplicissimae, cleaning, sucking surface moisture, and cutting to obtain a radix fici simplicissimae sample.
Further, in a preferred embodiment of the present invention, the step of washing and drying includes: cleaning the radix fici simplicissimae with clear water, and then sucking the water on the surface of the radix fici simplicissimae with water-absorbing filter paper.
Further, in a preferred embodiment of the present invention, the cutting step includes: when the diameter of the root of the hispid fig is less than 0.3cm, the root of the hispid fig is cut into sections with the length of 1.7-2.2 cm.
Further, in a preferred embodiment of the present invention, the cutting step includes: when the diameter of the root of the hispid fig is more than 0.3cm, the root of the hispid fig is cut into pieces with the thickness of 0.2-0.3 cm.
S2, spreading the hispid fig sample in an ultra-low temperature refrigerator for precooling to obtain the hispid fig precooled product.
Further, in the preferred embodiment of the invention, the pre-freezing temperature of the ultra-low temperature refrigerator is-75 to-80 ℃, and the pre-freezing time is 1.5 to 2 hours.
And S3, spreading the pre-frozen hispid fig in a tray of a freeze dryer, and performing vacuum freeze drying, crushing and sieving to obtain hispid fig dry powder.
Further, in the preferred embodiment of the present invention, the temperature of the vacuum freeze-drying partition is-40 to 35 ℃, and the drying time is 8 to 12 hours.
Further, in a preferred embodiment of the present invention, the temperature of the vacuum freeze-dried cold trap is less than-70 ℃.
Further, in the preferred embodiment of the present invention, the vacuum degree of the vacuum freeze-drying is less than 20Pa.
The invention also provides a hispid fig dry powder which is prepared by the freeze-drying method.
The invention adopts the vacuum freeze drying technology and improves the process to dry the radix fici simplicissimae, thereby improving the dehydration rate of the radix fici simplicissimae and reducing the loss of psoralen, flavone and polysaccharide. Compared with the hot air drying method, the dehydration rate and the content of active ingredients such as psoralen, flavone, polyphenol and the like of the hispid fig dry powder prepared by the method are higher than those of the hispid fig dry powder prepared by the hot air drying method, so that the medicinal value of the hispid fig can be retained to the maximum extent. Compared with the traditional freeze drying technology, the freeze drying time is shortened, the dehydration efficiency is improved, the content of psoralen, flavone and polysaccharide in the medicinal materials is ensured, and a foundation is provided for the subsequent application research of the hispid fig.
The features and properties of the present invention are described in further detail below with reference to examples.
Example 1
The hispid fig dry powder provided by the embodiment is prepared according to the following method:
(1) Cleaning fresh radix fici Simplicissimae with clear water, and air drying in a ventilation chamber. Cutting the root with the diameter less than 0.3cm into a section with the length of 2cm, cutting the root with the diameter more than 0.3cm into a piece with the thickness of 0.2-0.3 cm, sampling and weighing the fresh weight of the sample to be about 5 g.
(2) Spreading the sample in a tray of an ultra-low temperature refrigerator, and precooling for 1.5-2 h at-80 ℃ to obtain the hispid fig precooled product.
(3) The pre-cooled product was spread in the freeze dryer tray, the temperature of the septum was reduced to-40 ℃, the temperature of the cold trap was reduced to below-70 ℃, the vacuum was reduced to below 20Pa, and the freeze drying procedure was run as shown in table 1. And taking out the sample after the drying end point is reached, crushing the sample, and sieving the crushed sample with a 60-mesh sieve to obtain the hispid fig dry powder, wherein the dry weight of the hispid fig dry powder is 0.92g.
TABLE 1 Ficus Simplicissima Freeze-drying procedure
Comparative example 1
In the present comparative example, a hispid fig dry powder was provided, which was prepared according to the following method:
(1) Cleaning fresh radix fici Simplicissimae with clear water, and air drying in a ventilation chamber. Cutting the root with the diameter less than 0.3cm into a section with the length of 2cm, cutting the root with the diameter more than 0.3cm into a piece with the thickness of 0.2-0.3 cm, sampling and weighing the fresh weight of the sample to be about 5 g.
(2) Drying the sample by adopting a hot air drying mode at 70 ℃, and obtaining the hispid fig dry powder with the dry weight of 1.44g after the constant weight of 12 hours. The drying data for each time period is shown in table 2.
TABLE 2 Hot-air drying quality Change of Ficus Simplicissima
Comparative example 2
In the present comparative example, a hispid fig dry powder was provided, which was prepared according to the following method:
(1) Cleaning fresh radix fici Simplicissimae with clear water, and air drying in a ventilation chamber. Cutting the root with the diameter less than 0.3cm into a section with the length of 2cm, cutting the root with the diameter more than 0.3cm into a piece with the thickness of 0.2-0.3 cm, sampling and weighing the fresh weight of the sample to be about 5 g.
(2) Drying the sample in the sun outdoors, and obtaining the hispid fig root dry powder with the dry weight of 1.37g after 4 days. The drying data for each time period are shown in table 3.
TABLE 3 drying quality Change of Ficus Simplicissima
Comparative example 3
In the present comparative example, a hispid fig dry powder was provided, which was prepared according to the following method:
(1) Cleaning fresh radix fici Simplicissimae with clear water, and air drying in a ventilation chamber. Cutting the root with the diameter less than 0.3cm into a section with the length of 2cm, cutting the root with the diameter more than 0.3cm into a piece with the thickness of 0.2-0.3 cm, sampling and weighing the fresh weight of the sample to be about 5 g.
(2) Drying the sample by adopting an indoor drying mode at 25 +/-3 ℃ in the shade, and keeping the weight constant after 6 days to obtain the hispid fig dry powder, wherein the dry weight of the hispid fig dry powder is 1.80g. The drying data for each time period is shown in table 4.
TABLE 4 drying quality changes of Ficus Simplicissima in the shade
Comparative example 4
In the present comparative example, a hispid fig dry powder was provided, which was prepared according to the following method:
(1) Cleaning fresh radix fici Simplicissimae with clear water, and air drying in a ventilation chamber. Cutting the root with the diameter less than 0.3cm into a section with the length of 2cm, cutting the root with the diameter more than 0.3cm into a piece with the thickness of 0.2-0.3 cm, sampling and weighing the fresh weight of the sample to be about 5 g.
(2) The sample is spread in a tray of a freeze dryer for precooling for 3.5 to 4 hours at the temperature of minus 35 to minus 40 ℃, the temperature of a clapboard is reduced to minus 40 ℃, the temperature of a cold trap is reduced to below minus 70 ℃, the vacuum degree is reduced to below 20Pa, and the freeze-drying procedure is operated as shown in table 5. And taking out the sample after reaching the drying end point for 46h, crushing the sample, and sieving the crushed sample with a 60-mesh sieve to obtain the hispid fig dry powder, wherein the dry weight of the hispid fig dry powder is 0.92g.
TABLE 5 Ficus simplicissima lour Freeze-drying procedure
Test example 1
This test example compares the drying effects of different drying methods of hispid fig by studying the drying ratio, dehydration rate and drying speed of the hispid fig dried powders of example 1 and comparative examples 1 to 4. Wherein, the drying ratio represents the ratio of the constant weight of the material to the fresh weight of the material at the end of drying. Calculated according to the following formula:
in the formula, M 0 The fresh weight of the materials; m is a group of t The material weight is constant at the end of drying.
The dehydration rate represents the proportion of water removed from the material when it is dried to constant weight. Calculated according to the following formula:
in the formula, M 0 The fresh weight of the materials; m t The material weight is constant at the end of drying.
The drying rate represents the speed of dehydration of the material and is expressed in g/h. Calculated according to the following formula:
in the formula: m t1 And M t2 Respectively, is a drying time t 1 And t 2 Mass of the material.
The results of the two drying modes are compared as shown in table 6. As can be seen from table 6, when the sample was dried to constant weight, the drying ratio of the vacuum freeze-drying treatment was 51.78%, and the dehydration rate was 48.22%; the drying rate of the hot air drying treatment was 50.31%, and the dehydration rate was 49.69%. The drying ratio of hot air drying is slightly lower than that of vacuum freeze drying.
TABLE 6 results of different drying modes
Test example 2
The experimental example researches the influence of vacuum freeze drying, hot air drying and traditional vacuum freeze drying with high drying rate on the content of psoralen extracted from radix fici simplicissimae, and comprises the following steps:
respectively taking 1g of the dry powder of the hispid fig root of the example 1, the comparative example 1 and the comparative example 4, respectively adding 50mL of 50% methanol solution, carrying out ultrasonic extraction at 30 ℃ for 40min, cooling, shaking up, filtering, then adding 50% methanol for constant volume, and filtering by using a 0.45 mu m microporous filter membrane to respectively obtain a freeze-dried root psoralen extracting solution of the hispid fig root, a dried root psoralen extracting solution of the hispid fig root and a traditional freeze-dried root psoralen extracting solution of the hispid fig root for later use.
Dissolving the psoralen standard substance with methanol to prepare 0.37mg/mL psoralen standard substance solution. 0.02,0.10,0.50,1.00,1.50,2.00mL are respectively sucked to prepare gradient solutions with psoralen concentrations of 0.74 mu g/mL, 3.7 mu g/mL, 18.5 mu g/mL, 37 mu g/mL, 55.5 mu g/mL, 74 mu g/mL. Filtering with 0.45 μm microporous membrane to obtain control solution. And establishing a standard curve by taking the psoralen content as a horizontal coordinate and taking the peak area as a vertical coordinate, and performing linear regression.
Taking a psoralen standard solution with the concentration of 0.037mg/mL, adopting the HPLC condition, carrying out sample injection continuously for 6 times for determination, and recording the result. The RSD of the retention time is calculated and analyzed to be 0.07%, the RSD of the peak area is 0.11% and is lower than 0.5%, and therefore the instrument has good precision and can meet the analysis requirements of the experiment.
The same chromatographic conditions are adopted to respectively detect the content of psoralen in the freeze-dried root psoralen extracting solution of the hispid fig and the dry root psoralen extracting solution of the hispid fig. The psoralen content of the samples was calculated according to the following formula.
In the formula:
x-psoralen content (mg/g);
a-psoralen concentration (mg/mL) in the solution to be tested;
c, metering volume (mL) of psoralen extracting solution;
m-mass (g) of sample used in psoralen extraction.
And (3) carrying out data processing and statistical analysis on the determined psoralen content, and carrying out significance analysis by adopting a T test.
Detecting psoralen standard substance by HPLC method. FIG. 1 shows chromatogram of psoralen standard and fructus fici Simplicissimae extract. As can be seen from fig. 1, a single peak appears in the chromatogram from 6 to 7 min. Therefore, the peak of the extract of the root psoralen of the hispid fig appears in chromatogram of 6 to 7min is considered as the absorption peak of psoralen. Stability detection proves that HPLC conditions can meet the determination requirements of psoralen in hispid fig.
The regression equation for psoralen is Y =88.611x-66.709, R 2 =0.9984. As shown in FIG. 2, the content of psoralen in radix fici Simplicissimae freeze-dried root psoralen extract, radix fici Simplicissimae oven-dried root psoralen extract and radix fici Simplicissimae traditional freeze-dried root psoralen extract is compared with that in radix fici Simplicissimae freeze-dried root psoralen extract. Wherein, represents P<0.05, represents P<0.01. As can be seen from FIG. 2, the psoralen content of the freeze-dried root psoralen extract of Ficus simplicissima lour is 0.48mg/g, the psoralen content of the oven-dried root psoralen extract of Ficus simplicissima lour is 0.44mg/g, and the psoralen content of the traditional freeze-dried root psoralen extract of Ficus simplicissima lour is 0.48mg/g. The content of psoralen in the sample subjected to vacuum freeze drying is greater than that in the sample subjected to hot air drying, and the difference is very obvious (P)<0.01). The content of the psoralen in the sample subjected to vacuum freeze drying is equivalent to that of the psoralen in the sample subjected to traditional vacuum freeze drying, and the difference is not significant (P is more than 0.05).
Test example 3
The experimental example studies the influence of vacuum freeze drying, hot air drying and traditional vacuum freeze drying on the content of flavone extracted from the root of hispid fig. The method comprises the following steps:
weighing 1g of the dry powder of the hispid fig. 1, the dry powder of the hispid fig. 1 and the traditional freeze-dried powder of the hispid fig. 4 respectively, and then respectively mixing the dry powder according to the weight ratio of 1: adding ethanol solution with volume fraction of 60% into 15 material liquid ratio, shaking, sealing, ultrasonic extracting at 70 deg.C for 30min, and centrifuging at 8000r/min for 5min. The filtrate is subjected to constant volume by using 60% ethanol to obtain a hispid fig freeze-dried root total flavone extracting solution and a hispid fig dried root total flavone extracting solution respectively.
Adding the reagent according to table 7, taking 60% ethanol added with the reagent according to table 7 as reference, measuring absorbance at 510nm wavelength, taking rutin standard substance concentration as abscissa, taking absorbance as ordinate, and making standard curve.
TABLE 7 Total Flavonoids Standard Curve reagent addition Table
Adding freeze-dried radix fici simplicissimae total flavone extract obtained by vacuum freeze-drying, freeze-dried radix fici simplicissimae total flavone extract obtained by hot air drying and freeze-dried radix fici simplicissimae total flavone extract obtained by traditional vacuum freeze-drying respectively, adding reagents according to the table 7 for reaction, measuring absorbance, and calculating the total flavone content in the sample according to the following formula.
In the formula:
x-total flavone content (mg/g);
a-measured total flavone concentration (mg/mL);
c, the volume (mL) of the extracting solution is determined;
v-volume of fluid to be measured (mL);
y-volume of extract used (mL);
m-sample mass (g) used in the extraction of flavones.
And (4) carrying out data processing and statistical analysis on the determined total flavone content, and carrying out significance analysis by adopting a T test. The regression equation of the standard curve of the flavone is Y =11.995x-0.012 2 =0.9912。
As shown in FIG. 3, the content of total flavonoids in the freeze-dried radix fici simplicissimae extractive solution, the oven-dried radix fici simplicissimae extractive solution, and the conventional freeze-dried radix fici simplicissimae extractive solution is shown. As can be seen from FIG. 3, the total flavone content extracted from vacuum freeze-dried hispid Fig root is 7.67mg/g; the content of total flavone extracted from radix fici Simplicissimae dried by hot air is 6.90mg/g, and the content of total flavone extracted from radix fici Simplicissimae dried by traditional vacuum freeze drying is 7.63mg/g. The content of the total flavone in the sample subjected to vacuum freeze drying is larger than that of the total flavone in the sample subjected to hot air drying, and the difference is very obvious (P < 0.01). The content of the total flavone in the vacuum freeze-dried sample is higher than that of the total flavone in the traditional vacuum freeze-dried sample, and the difference is not significant (P is more than 0.05).
Test example 4
This test example investigated the effect of vacuum freeze-drying and hot air drying on the polyphenol content extracted from fici hirta root. The method comprises the following steps:
1g of the dry powder of the hispid fig from example 1, comparative example 1 and comparative example 4 is weighed respectively, then 50% volume fraction ethanol solution is added according to the ratio of 1. And (3) diluting the filtrate with 50% ethanol to a constant volume to obtain a hispid fig root polyphenol extracting solution and a hispid fig root polyphenol extracting solution respectively.
The total phenol content was determined by the Folin-ciocalteu method, the reagents were added according to Table 8, 50% ethanol was added according to Table 8 as a reference, the absorbance was determined at 765nm wavelength, the gallic acid concentration was plotted on the abscissa and the absorbance was plotted on the ordinate to create a standard curve.
TABLE 8 Total phenol standard curve reagent addition Table
Adding freeze-dried root polyphenol extracting solution of hispid fig, dried root polyphenol extracting solution of hispid fig and traditional freeze-dried root polyphenol extracting solution of hispid fig respectively, operating according to table 8, detecting absorbance, and calculating the total phenol content in the sample according to the following formula.
In the formula:
x-total phenol content in sample (mg/g);
a is the total phenol concentration (mg/mL) in the solution to be tested;
c-constant volume (mL);
n-dilution factor;
m-sample mass (g) used in the extraction of total phenols.
And (4) carrying out data processing and statistical analysis on the determined total phenol content, and carrying out significance analysis by adopting a T test. The standard curve equation of polyphenol is Y =10.951x +0.0317 2 =0.9902。
Fig. 4 shows the comparison of polyphenol content in freeze-dried radix fici Simplicissimae extract, and conventional freeze-dried radix fici Simplicissimae extract. As can be seen from FIG. 4, the total phenol content of the vacuum freeze-dried root of hispid Fig was 13.00mg/g. The hot air dried radix fici Simplicissimae extract total phenol content is 11.20mg/g. The content of total phenols extracted from traditional vacuum freeze-dried radix fici Simplicissimae is 12.78mg/g. The content of the total phenol in the vacuum freeze-dried sample is larger than that in the hot air dried sample, and the difference is very obvious (P < 0.01). The content of the total phenol in the vacuum freeze-dried sample is larger than that in the traditional vacuum freeze-dried sample, and the difference is not significant (P is larger than 0.05).
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the present invention is not intended to limit the scope of the invention as claimed, but is merely representative of selected embodiments of the invention. 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.
Claims (9)
1. A freeze-drying method of radix fici simplicissimae is characterized by comprising the following steps:
s1, taking fresh radix fici simplicissimae, cleaning, sucking surface moisture, and cutting to obtain a radix fici simplicissimae sample;
s2, flatly paving the hispid fig sample in an ultralow temperature refrigerator for precooling to obtain a hispid fig precooled product;
and S3, spreading the pre-cooled hispid fig in a tray of a freeze dryer, and performing vacuum freeze drying, crushing and sieving to obtain hispid fig dry powder.
2. The freeze-drying method according to claim 1, wherein in step S1, the step of washing and drying comprises: and (3) cleaning the root of the hispid fig with clear water, and then sucking the water on the surface of the root of the hispid fig by using water absorption filter paper.
3. The freeze-drying method according to claim 1, wherein in step S1, the step of cutting comprises: when the diameter of the root of the hispid fig is less than 0.3cm, the root of the hispid fig is cut into sections with the length of 1.7-2.2 cm.
4. The freeze-drying method according to claim 1, wherein in step S1, the step of cutting comprises: when the diameter of the root of the hispid fig is more than 0.3cm, the root of the hispid fig is cut into pieces with the thickness of 0.2-0.3 cm.
5. The freeze-drying method according to claim 1, wherein the pre-freezing temperature of the ultra-low temperature refrigerator is-75 to-85 ℃ and the pre-freezing time is 1.5 to 2 hours in step S2.
6. The freeze-drying method according to claim 1, wherein in the step S3, the temperature of the vacuum freeze-drying partition plate is-40 to 35 ℃, and the drying time is 8 to 12 hours.
7. The freeze-drying method according to claim 1, wherein in step S3, the temperature of the vacuum freeze-dried cold trap is less than-70 ℃.
8. The freeze-drying method according to claim 1, wherein in step S3, the vacuum degree of the vacuum freeze-drying is less than 20Pa.
9. A dry powder of hispid Fig, prepared by the freeze-drying method according to any one of claims 1 to 8.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210850574.2A CN115282186B (en) | 2022-07-20 | 2022-07-20 | Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210850574.2A CN115282186B (en) | 2022-07-20 | 2022-07-20 | Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder |
Publications (2)
Publication Number | Publication Date |
---|---|
CN115282186A true CN115282186A (en) | 2022-11-04 |
CN115282186B CN115282186B (en) | 2023-09-08 |
Family
ID=83824375
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210850574.2A Active CN115282186B (en) | 2022-07-20 | 2022-07-20 | Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN115282186B (en) |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109999079A (en) * | 2019-05-15 | 2019-07-12 | 广东省微生物研究所(广东省微生物分析检测中心) | The preparation method of radix fici simplicissimatis extractive and the application in terms of preparing treatment/prevention high lithemia related disease medicine/health product |
CN114259514A (en) * | 2022-02-18 | 2022-04-01 | 暨南大学附属第一医院(广州华侨医院) | Preparation method of hispid fig extract and application of hispid fig extract in preparation of products for preventing and treating obesity, hyperlipidemia and non-alcoholic steatohepatitis |
-
2022
- 2022-07-20 CN CN202210850574.2A patent/CN115282186B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109999079A (en) * | 2019-05-15 | 2019-07-12 | 广东省微生物研究所(广东省微生物分析检测中心) | The preparation method of radix fici simplicissimatis extractive and the application in terms of preparing treatment/prevention high lithemia related disease medicine/health product |
CN114259514A (en) * | 2022-02-18 | 2022-04-01 | 暨南大学附属第一医院(广州华侨医院) | Preparation method of hispid fig extract and application of hispid fig extract in preparation of products for preventing and treating obesity, hyperlipidemia and non-alcoholic steatohepatitis |
Non-Patent Citations (1)
Title |
---|
叶茂森等: "基于粗糙集法的五指毛桃补骨脂素合成酶基因序列获取与分析", 分子植物育种, vol. 19, no. 22, pages 7398 - 7407 * |
Also Published As
Publication number | Publication date |
---|---|
CN115282186B (en) | 2023-09-08 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN103919712B (en) | Cordyceps militaris extract, and preparation method and application thereof | |
CN115282186A (en) | Freeze-drying method of radix fici simplicissimae and dry powder of radix fici simplicissimae | |
CN114224943A (en) | Aronia melanocarpa extract and preparation method thereof | |
CN111830173B (en) | Internal standard method for detecting content of wild spina gleditsiae doped in spina gleditsiae decoction pieces | |
CN102000133B (en) | Preparation method of traditional Chinese medicine anti-oxidation preparation | |
CN109438545A (en) | A kind of natural antibacterial compound and preparation method thereof and the application in electronic cigarette | |
CN106750429B (en) | Preparation process of onion polysaccharide-gelatin composite membrane | |
CN105131140A (en) | Trigonella foenum-graecum polysaccharide extraction purification method and applications of trigonella foenum-graecum polysaccharide as humectant in cigarettes | |
Innocenti et al. | Investigations of the content of furocoumarins in Apium graveolens and in Petroselinum sativum | |
CN107759710B (en) | Preparation method of ambary hemp extract and application of ambary hemp extract in tobacco | |
CN115406991B (en) | Preparation method and quality control method of pearl garden balsam stem formula granules | |
CN102210728B (en) | Method for processing angelica dahurica in producing area | |
CN108931110A (en) | A kind of bletilla medicine materical crude slice vacuum freeze-drying method | |
CN109200175A (en) | A kind of preparation method of vacuum freeze drying fritillaria thunbergii | |
Wang et al. | Investigation of the impact on the antioxidant capacity and Flavonoids components of different drying methods for Sophora japonica L. | |
CN105902628B (en) | A kind of storage practice of rheum officinale | |
CN111759777A (en) | Anti-allergy whitening moisturizing composition and cosmetic | |
Browning et al. | The Permeability of the Shell of the Egg of Acheta Commodus Walker* (Orthoptera, Gryllidae) | |
CN111323508A (en) | Method for measuring content of 2, 4-dihydroxy-6-methoxyacetophenone | |
CN103417589A (en) | Preparation method and application of patrinia villosa root extractive | |
CN110432262A (en) | A kind of preparation of waxed plant leaves sample and store method | |
CN108409545A (en) | A kind of ether compound, preparation method and application | |
CN115651089B (en) | Gastrodia elata polysaccharide with antioxidant activity | |
CN115089629B (en) | Ficus simplicissima lour freeze-dried fruit flavone extracting solution and preparation method thereof | |
CN115097058B (en) | Thin-layer chromatography identification method for Choerospondias axillaris |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant | ||
TR01 | Transfer of patent right |
Effective date of registration: 20241011 Address after: 365000 No. 6, 21st floor, No. 9, Jinsong Road (building 158, Lvyan New Village), Meilie District, Sanming City, Fujian Province Patentee after: Yisheng vitality health technology (Fujian) Co.,Ltd. Country or region after: China Address before: 365000 No. 25 Jingdong Road, Sanyuan District, Sanming City, Fujian Province Patentee before: SANMING University Country or region before: China |