CN115282186B - Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder - Google Patents

Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder Download PDF

Info

Publication number
CN115282186B
CN115282186B CN202210850574.2A CN202210850574A CN115282186B CN 115282186 B CN115282186 B CN 115282186B CN 202210850574 A CN202210850574 A CN 202210850574A CN 115282186 B CN115282186 B CN 115282186B
Authority
CN
China
Prior art keywords
ficus simplicissima
lour
ficus
drying
simplicissima lour
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.)
Active
Application number
CN202210850574.2A
Other languages
Chinese (zh)
Other versions
CN115282186A (en
Inventor
张君诚
杨琳
张杭颖
陈有先
章立
吴进华
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sanming University
Original Assignee
Sanming University
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by Sanming University filed Critical Sanming University
Priority to CN202210850574.2A priority Critical patent/CN115282186B/en
Publication of CN115282186A publication Critical patent/CN115282186A/en
Application granted granted Critical
Publication of CN115282186B publication Critical patent/CN115282186B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • 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)
    • A61K36/60Moraceae (Mulberry family), e.g. breadfruit or fig
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/14Particulate form, e.g. powders, Processes for size reducing of pure drugs or the resulting products, Pure drug nanoparticles
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26DRYING
    • F26BDRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04Drying 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
    • F26B5/06Drying 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
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/15Preparation or pretreatment of starting material involving mechanical treatment, e.g. chopping up, cutting or grinding
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation 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
    • A61K2236/10Preparation or pretreatment of starting material
    • A61K2236/17Preparation or pretreatment of starting material involving drying, e.g. sun-drying or wilting
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P60/00Technologies relating to agriculture, livestock or agroalimentary industries
    • Y02P60/80Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
    • Y02P60/85Food 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 Ficus simplicissima lour roots and Ficus simplicissima lour dried powder, which comprises the following steps: taking fresh radix fici simplicissimae, cleaning, sucking surface moisture, and cutting to obtain radix fici simplicissimae sample; then spreading the Ficus simplicissima lour sample on an ultralow temperature refrigerator for precooling to obtain a Ficus simplicissima lour precooled product; and finally, spreading the pre-cooled Ficus simplicissima lour product in a tray of a freeze dryer, and performing vacuum freeze drying, crushing and sieving to obtain the Ficus simplicissima lour dry powder. The invention adopts the vacuum freeze drying technology to dry the Ficus simplicissima lour roots, ensures the colleague of the dehydration rate of Ficus simplicissima lour, reduces the loss of psoralen, flavone and polysaccharide. Compared with hot air drying treatment, the dehydration rate of the prepared Ficus simplicissima lour dry powder and the content of active ingredients such as psoralen, flavone and polyphenol are high, so that the medicinal value of Ficus simplicissima lour is retained to the maximum extent, and a foundation is provided for the subsequent application research of Ficus simplicissima lour.

Description

Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder
Technical Field
The invention relates to the technical field of Chinese herbal medicine drying, in particular to a freeze-drying method of Ficus simplicissima lour roots and Ficus simplicissima lour dried powder.
Background
Ficus hirta (Ficus hirta), which is a plant of Ficus genus of Moraceae family, is commonly used as root and is mostly distributed in south China, and is a plant for both medicine and food. The five-finger wild peach has wide functions, mainly has the functions of strengthening spleen and tonifying lung, tonifying qi and resolving dampness, relaxing tendons and dredging 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.
The drying treatment is an important link of medicinal material processing and is a key step affecting the quality of medicinal materials. The good drying treatment mode can effectively prevent the Chinese herbal medicines from mildew and pollution, reduce the damage and loss of the effective components and ensure that the medicine effect is maintained to the greatest extent. The traditional drying method of the Chinese herbal medicine mainly comprises drying in the shade and sun, and has the defects of long time, low efficiency, high labor cost, great restriction by weather factors, easiness in pollution, good quality, poor quality and the like. The hot air drying and the cold air drying have the advantages of high drying efficiency, no influence of factors such as weather, ambient temperature and the like, and are suitable for industrial large-scale production. The difference of the total flavone content of the rhizome traditional Chinese medicinal materials is found after the rhizome traditional Chinese medicinal materials are treated by different drying modes, and the drying in the shade is 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 ingredient after drying.
Disclosure of Invention
The invention aims to provide a freeze-drying method and powder for radix fici simplicissimae, which are used for drying radix fici simplicissimae by adopting a vacuum freeze-drying technology, and the obtained powder has high dehydration rate and higher content of active ingredients such as psoralen, flavone, polyphenol and the like than the traditional drying method.
The invention solves the technical problems by adopting the following technical scheme.
The invention provides a freeze-drying method of a five-finger wild peach root, which is characterized by comprising the following steps of:
s1, taking fresh Ficus simplicissima lour roots, cleaning, sucking surface moisture, and cutting to obtain Ficus simplicissima lour samples;
s2, spreading the Ficus simplicissima lour sample in an ultralow temperature refrigerator for precooling to obtain a Ficus simplicissima lour precooled product;
and S3, spreading the pre-cooled Ficus simplicissima lour product in a tray of a freeze dryer, and performing vacuum freeze drying, crushing and sieving to obtain the Ficus simplicissima lour dry powder.
The invention provides a Ficus simplicissima lour dry powder, which is prepared according to the freeze-drying method.
The freeze-drying method of the Ficus simplicissima lour roots and the Ficus simplicissima lour dry powder have the beneficial effects that:
the invention adopts the vacuum freeze drying technology and improves the flow thereof to dry the root of the Ficus simplicissima lour, improves the dehydration efficiency and reduces the loss of psoralen, flavone and polysaccharide while guaranteeing the dehydration rate of the Ficus simplicissima lour. Compared with hot air drying, the dehydration rate of the prepared Ficus simplicissima lour dried powder is higher than that of the prepared Ficus simplicissima lour dried powder treated by the hot air drying method, so that the medicinal value of Ficus simplicissima lour can be furthest reserved. Compared with the traditional freeze-drying technology, the method shortens the freeze-drying time, improves the dehydration efficiency, ensures the content of psoralen, flavone and polysaccharide in the medicinal materials, and provides a basis for the subsequent application research of the five-finger wild peach.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the embodiments will be briefly described below, it being understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and other related drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a chromatogram of a psoralen standard and a psoralen extract from Ficus simplicissima root;
FIG. 2 is a graph showing a comparison of psoralen content in a freeze-dried root psoralen extract of Ficus simplicissima lour, a dried root psoralen extract of Ficus simplicissima lour, and a conventional freeze-dried root psoralen extract of Ficus simplicissima lour;
FIG. 3 is a graph showing the comparison of total flavonoids in the lyophilized root total flavonoids extract of Ficus simplicissima lour, the dried root total flavonoids extract of Ficus simplicissima lour and the conventional lyophilized root total flavonoids extract of Ficus simplicissima lour;
FIG. 4 is a graph showing the comparison of the polyphenol content of the lyophilized root polyphenol extract of Ficus simplicissima lour and the polyphenol content of the conventional lyophilized root polyphenol extract of Ficus simplicissima lour;
fig. 5 is a flow chart of the preparation of the Ficus simplicissima lour dry powder of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The freeze-drying method of the Ficus simplicissima lour root and the Ficus simplicissima lour dry powder according to the embodiment of the invention are specifically described below.
Referring to fig. 5, the freeze-drying method for the root of the hispid fig provided by the embodiment of the invention comprises the following steps:
s1, taking fresh Ficus simplicissima lour roots, cleaning, sucking surface moisture, and cutting to obtain Ficus simplicissima lour samples.
Further, in a preferred embodiment of the present invention, the steps of washing and drying include: and cleaning the root of the Ficus simplicissima lour with clear water, and then sucking the surface water by using water-absorbing filter paper.
Further, in a preferred embodiment of the present invention, the step of cutting includes: when the diameter of the Ficus simplicissima is smaller than 0.3cm, cutting the Ficus simplicissima into segments with the length of 1.7-2.2 cm.
Further, in a preferred embodiment of the present invention, the step of cutting includes: when the diameter of the Ficus simplicissima lour root is larger than 0.3cm, cutting the Ficus simplicissima lour root into pieces with the thickness of 0.2-0.3 cm.
And S2, spreading the Ficus simplicissima lour sample on an ultralow temperature refrigerator for precooling to obtain a Ficus simplicissima lour precooled product.
Further, in the preferred embodiment of the invention, the pre-freezing temperature of the ultra-low temperature refrigerator is between 75 ℃ below zero and 80 ℃ below zero, and the pre-freezing time is between 1.5 and 2 hours.
And S3, spreading the pre-frozen product of the Ficus simplicissima lour in a tray of a freeze dryer, and performing vacuum freeze drying, crushing and sieving to obtain the dried powder of the Ficus simplicissima lour.
Further, in the preferred embodiment of the invention, the temperature of the vacuum freeze-dried separator is-40-35 ℃ and the drying time is 8-12 h.
Further, in a preferred embodiment of the present invention, the cold trap temperature of the vacuum freeze drying is less than-70 ℃.
Further, in a preferred embodiment of the present invention, the vacuum degree of the vacuum freeze-drying is less than 20Pa.
The invention also provides the Ficus simplicissima lour dry powder, which is prepared according to the freeze-drying method.
The invention adopts the vacuum freeze drying technology and improves the flow thereof to dry the Ficus simplicissima lour root, thereby improving the dehydration rate of the Ficus simplicissima lour root and reducing the loss of psoralen, flavone and polysaccharide. Compared with hot air drying, the dehydration rate of the prepared Ficus simplicissima lour dried powder is higher than that of the prepared Ficus simplicissima lour dried powder treated by the hot air drying method, so that the medicinal value of Ficus simplicissima lour can be furthest reserved. Compared with the traditional freeze-drying technology, the method shortens the freeze-drying time, improves the dehydration efficiency, ensures the content of psoralen, flavone and polysaccharide in the medicinal materials, and provides a basis for the subsequent application research of the five-finger wild peach.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The five-finger wild peach dry powder provided by the embodiment is prepared according to the following method:
(1) Taking the root of fresh Ficus simplicissima lour, cleaning with clear water, and airing the surface water in a ventilation chamber. Root with diameter smaller than 0.3cm is cut into sections with length of 2cm, root with diameter larger than 0.3cm is cut into pieces with thickness of 0.2-0.3 cm, and fresh weight of the sample is about 5 g.
(2) Spreading the sample in an ultralow temperature refrigerator tray, and pre-cooling at-80 ℃ for 1.5-2 hours to obtain the pre-cooled five-finger wild peach product.
(3) The pre-cooled product was spread in a freeze dryer tray, the temperature of the separator was reduced to-40 ℃, the temperature of the cold trap was reduced to below-70 ℃, the vacuum was reduced to below 20Pa, and the lyophilization procedure was run as shown in Table 1. And taking out the sample after reaching the drying end point, crushing, and sieving with a 60-mesh sieve to obtain the Ficus simplicissima lour dried powder, wherein the dry weight of the Ficus simplicissima lour dried powder is 0.92g.
Table 1 Ficus simplicissima freeze-drying procedure
Comparative example 1
In this comparative example, there is provided a Ficus simplicissima lour dried powder prepared according to the following method:
(1) Taking the root of fresh Ficus simplicissima lour, cleaning with clear water, and airing the surface water in a ventilation chamber. Root with diameter smaller than 0.3cm is cut into sections with length of 2cm, root with diameter larger than 0.3cm is cut into pieces with thickness of 0.2-0.3 cm, and fresh weight of the sample is about 5 g.
(2) And drying the sample by adopting a hot air drying mode at 70 ℃ for 12 hours, and then keeping the weight constant to obtain the Ficus simplicissima lour dried powder, wherein the dry weight of the Ficus simplicissima lour dried powder is 1.44g. The drying data for each period are shown in table 2.
Table 2 changes in hot air drying quality of five-finger nectarines
Comparative example 2
In this comparative example, there is provided a Ficus simplicissima lour dried powder prepared according to the following method:
(1) Taking the root of fresh Ficus simplicissima lour, cleaning with clear water, and airing the surface water in a ventilation chamber. Root with diameter smaller than 0.3cm is cut into sections with length of 2cm, root with diameter larger than 0.3cm is cut into pieces with thickness of 0.2-0.3 cm, and fresh weight of the sample is about 5 g.
(2) And (3) drying the sample in an outdoor sun-drying mode, wherein the weight is constant after 4 days, and the dried powder of the Ficus simplicissima lour is obtained, and the dry weight of the dried powder is 1.37g. The drying data for each period are shown in table 3.
Table 3 changes in sun-dried quality of Ficus simplicissima
Comparative example 3
In this comparative example, there is provided a Ficus simplicissima lour dried powder prepared according to the following method:
(1) Taking the root of fresh Ficus simplicissima lour, cleaning with clear water, and airing the surface water in a ventilation chamber. Root with diameter smaller than 0.3cm is cut into sections with length of 2cm, root with diameter larger than 0.3cm is cut into pieces with thickness of 0.2-0.3 cm, and fresh weight of the sample is about 5 g.
(2) Drying the sample in the shade at 25+ -3deg.C for 6d to obtain Ficus simplicissima lour dry powder with dry weight of 1.80g. The drying data for each period are shown in table 4.
Table 4 changes in the quality of drying Ficus simplicissima
Comparative example 4
In this comparative example, there is provided a Ficus simplicissima lour dried powder prepared according to the following method:
(1) Taking the root of fresh Ficus simplicissima lour, cleaning with clear water, and airing the surface water in a ventilation chamber. Root with diameter smaller than 0.3cm is cut into sections with length of 2cm, root with diameter larger than 0.3cm is cut into pieces with thickness of 0.2-0.3 cm, and fresh weight of the sample is about 5 g.
(2) The samples were spread in a freeze dryer tray, pre-cooled at-35 to-40 ℃ for 3.5 to 4 hours, the temperature of the separator 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 5. And after 46 hours from the drying end point, taking out the sample, crushing the sample, and sieving the crushed sample by a 60-mesh sieve to obtain the Ficus simplicissima lour dried powder, wherein the dry weight of the Ficus simplicissima lour dried powder is 0.92g.
Table 5 Ficus simplicissima freeze-drying procedure
Test example 1
This test example compares the drying effect of different drying modes of Ficus simplicissima lour by studying the drying ratio, dehydration rate and drying speed of the Ficus simplicissima lour dried powder 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. The calculation is carried out according to the following formula:
wherein M is 0 The fresh weight of the material; m is M t The weight of the material at the end of drying is constant.
The dehydration rate represents the proportion of water removed from the material when it is dried to a constant weight. The calculation is carried out according to the following formula:
wherein M is 0 The fresh weight of the material; m is M t The weight of the material at the end of drying is constant.
The drying rate represents the speed of dehydration of the material in g/h. The calculation is carried out according to the following formula:
wherein: m is M t1 And M t2 Respectively the drying time t 1 And t 2 The 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 samples were dried to a 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 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 higher drying rate on the content of psoralen extracted from the root of Ficus hirta, and comprises the following steps:
taking 1g of each of the dry powders of the Ficus simplicissima lour of example 1, comparative example 1 and comparative example 4, respectively, then adding 50mL of 50% methanol solution, carrying out ultrasonic extraction at 30 ℃ for 40min, cooling, shaking uniformly, filtering, then adding 50% methanol to fix volume, and filtering by using a 0.45 mu m microporous filter membrane to obtain a Ficus simplicissima lour freeze-dried root psoralen extract, a Ficus simplicissima lour dry root psoralen extract and a Ficus sima lour traditional freeze-dried root psoralen extract for standby.
The psoralen standard substance is dissolved by methanol to prepare 0.37mg/mL psoralen standard substance solution. The concentration of psoralen was 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 by pipetting 0.02,0.10,0.50,1.00,1.50,2.00mL, respectively. Filtering with 0.45 μm microporous membrane to obtain reference solution. And establishing a standard curve by taking the psoralen content as an abscissa and the peak area as an ordinate, and carrying out linear regression.
Taking psoralen standard substance solution with concentration of 0.037mg/mL, adopting the HPLC condition, continuously sampling for 6 times for measurement, and recording the result. The RSD of the retention time obtained by calculation and analysis is 0.07%, the RSD of the peak area is 0.11%, and is lower than 0.5%, which shows that the instrument has good precision and can meet the analysis requirement of the experiment.
The psoralen content in the freeze-dried root psoralen extract of the Ficus simplicissima lour and the dried root psoralen extract of the Ficus simplicissima lour are detected respectively by adopting the same chromatographic conditions. The psoralen content in the sample was calculated according to the following formula.
Wherein:
x-psoralen content (mg/g);
a-concentration of psoralen in the solution to be measured (mg/mL);
c-psoralen extract constant volume (mL);
m-mass of sample used in extraction of psoralen (g).
And carrying out data processing and statistical analysis on the measured psoralen content, and carrying out significance analysis by adopting T test.
And detecting the psoralen standard by adopting an HPLC method. The chromatograms of the psoralen standard and the psoralen extract of the root of Ficus hirta are shown in figure 1. As can be seen from fig. 1, a single peak appears in the chromatogram at 6 to 7 min. Thus, the peak of the extract of psoralen from Ficus simplicissima at a chromatogram of 6 to 7min was considered as the absorption peak of psoralen. Stability detection proves that the HPLC condition can meet the measurement requirement of psoralen in Ficus simplicissima lour.
The regression equation of psoralen is y= 88.611x-66.709, r 2 =0.9984. Fig. 2 is a graph showing the comparison of psoralen content in the freeze-dried root psoralen extract of Ficus simplicissima lour, the dried root psoralen extract of Ficus simplicissima lour and the traditional freeze-dried root psoralen extract of Ficus simplicissima lour. Wherein, is 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 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 dryingThe psoralen content in the samples was very different (P<0.01). The psoralen content in the sample subjected to vacuum freeze drying is equivalent to that in the sample subjected to traditional vacuum freeze drying, and the difference is not obvious (P is more than 0.05).
Test example 3
The experimental example researches the influence of vacuum freeze drying, hot air drying and traditional vacuum freeze drying on the flavone content extracted from the root of Ficus simplicissima. The method comprises the following steps:
1g of the Ficus simplicissima lour dry powder of example 1, and the Ficus simplicissima lour dry powder of comparative example 1 and the Ficus simplicissima lour conventional freeze-dried powder of comparative example 4 were weighed separately, and then 1: adding ethanol solution with volume fraction of 60% into the mixture at 15 feed liquid ratio, shaking, sealing, performing ultrasonic extraction at 70deg.C for 30min, and centrifuging at 8000r/min for 5min. The filtrate is fixed with 60 percent ethanol to obtain the total flavone extract of the freeze-dried root of the Ficus simplicissima lour and the total flavone extract of the dried root of the Ficus simplicissima lour respectively.
The reagent was added as shown in Table 7, and the absorbance was measured at a wavelength of 510nm with 60% ethanol as a reference, and the rutin standard concentration was plotted on the abscissa and the absorbance was plotted on the ordinate, to prepare a standard curve.
TABLE 7 Total flavone Standard Curve reagent addition Table
Adding the total flavone extract of the freeze-dried roots of the Ficus simplicissima lour obtained by vacuum freeze-drying treatment, the total flavone extract of the dried roots of the Ficus simplicissima lour obtained by hot air drying treatment and the total flavone extract of the freeze-dried roots of the Ficus simplicissima lour obtained by traditional vacuum freeze-drying treatment respectively, adding reagents for reaction, measuring absorbance, and calculating the total flavone content in the sample according to the following formula.
Wherein:
x-total flavone content (mg/g);
a-total flavone concentration (mg/mL) measured;
c, the volume of the extracting solution is fixed (mL);
v-volume of liquid to be measured (mL);
y-volume of extract used (mL);
m-the mass of sample used in extracting flavone (g).
And carrying out data processing and statistical analysis on the measured total flavone content, and carrying out significance analysis by adopting T test. The regression equation of the standard curve of the flavone is Y= 11.995x-0.012, R 2 =0.9912。
Fig. 3 is a graph showing the comparison of total flavone content of the total flavone extract of the freeze-dried root of the Ficus simplicissima lour and the total flavone extract of the traditional freeze-dried root of the Ficus simplicissima lour. As can be seen from FIG. 3, the total flavone content extracted from the root of Ficus simplicissima lour which is freeze-dried in vacuum is 7.67mg/g; the total flavone content extracted from the hot air dried Ficus simplicissima lour root is 6.90mg/g, and the total flavone content extracted from the traditional vacuum freeze-dried Ficus simplicissima lour root is 7.63mg/g. The total flavone content in the samples subjected to vacuum freeze drying is greater than that in the samples subjected to hot air drying, and the difference is very remarkable (P < 0.01). The total flavone content in the vacuum freeze-dried sample is higher than that in the traditional vacuum freeze-dried sample, and the difference is not obvious (P is more than 0.05).
Test example 4
The experimental example researches the influence of vacuum freeze drying and hot air drying on the polyphenol content extracted from the root of the Ficus simplicissima. The method comprises the following steps:
1g of the Ficus simplicissima lour dry powder of example 1, comparative example 1 and comparative example 4 are respectively weighed, 50% ethanol solution with volume fraction is added according to the feed liquid ratio of 1:30 respectively, shaking is carried out uniformly, sealing is carried out, ultrasonic extraction is carried out for 44min at 60 ℃, and centrifugation is carried out for 3min at 8000 r/min. The filtrate is fixed with 50% ethanol to obtain the lyophilized root polyphenol extract of Ficus simplicissima lour and the dried root polyphenol extract of Ficus simplicissima lour respectively.
The total phenol content was determined by Folin-ciocalteu method, the reagents were added according to Table 8, and 50% ethanol was added according to Table 8 as reference, absorbance was measured at 765nm wavelength, gallic acid concentration was on the abscissa, and absorbance was on the ordinate to establish a standard curve.
TABLE 8 Total phenol Standard Curve reagent addition Table
And respectively adding the radix fici simplicissimae lyophilized root polyphenol extract, the radix fici simplicissimae dried root polyphenol extract and the radix fici simplicissimae traditional lyophilized root polyphenol extract, operating with reference to table 8, detecting absorbance, and calculating the total phenol content in the sample according to the following formula.
Wherein:
x-total phenol content in sample (mg/g);
a-the total phenol concentration (mg/mL) in the liquid to be measured;
c-constant volume (mL);
n-dilution factor;
m-the mass of sample (g) used in the extraction of total phenol.
And carrying out data processing and statistical analysis on the measured total phenol content, and carrying out significance analysis by adopting T test. The standard curve equation of the polyphenol is Y=10.95dx+0.0317, R 2 =0.9902。
Fig. 4 is a graph showing the comparison of the polyphenol contents of the freeze-dried root polyphenol extract of Ficus simplicissima lour and the conventional freeze-dried root polyphenol extract of Ficus simplicissima lour. As can be seen from FIG. 4, the total phenol content of the extract of the root of Ficus simplicissima was 13.00mg/g. The total phenol content extracted from the hot air dried Ficus simplicissima lour root is 11.20mg/g. The total phenol content extracted from the roots of the Chinese Ficus simplicissima lour which is freeze-dried in a traditional vacuum is 12.78mg/g. The total phenol content in the vacuum freeze-dried samples was greater than that in the hot air dried samples, with a very significant difference (P < 0.01). The total phenol content in the vacuum freeze-dried samples was greater than that in the conventional vacuum freeze-dried samples, with insignificant differences (P > 0.05).
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the 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 made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.

Claims (3)

1. The freeze-drying method of the radix fici simplicissimae root is characterized by comprising the following steps of:
s1, taking fresh Ficus simplicissima lour roots, cleaning, sucking surface moisture, and cutting to obtain Ficus simplicissima lour samples;
s2, spreading the Ficus simplicissima lour sample in an ultralow temperature refrigerator for precooling to obtain a Ficus simplicissima lour precooled product;
s3, spreading the pre-cooled Ficus simplicissima lour product in a tray of a freeze dryer, and performing vacuum freeze drying, crushing and sieving to obtain dried Ficus simplicissima lour powder;
in step S1, the step of cutting includes: when the diameter of the root of the Ficus simplicissima is smaller than 0.3cm, cutting the root of the Ficus simplicissima into segments with the length of 1.7-2.2 cm;
in step S1, the step of cutting includes: when the diameter of the root of the Ficus simplicissima is larger than 0.3cm, cutting the root of the Ficus simplicissima into pieces with the thickness of 0.2-0.3 cm;
in the step S2, the pre-freezing temperature of the ultralow temperature refrigerator is-75 to-85 ℃, and the pre-freezing time is 1.5 to 2 hours;
in the step S3, the temperature of the vacuum freeze-dried separator is-40-35 ℃ and the drying time is 8-12 h;
in the step S3, the cold trap temperature of the vacuum freeze drying is less than-70 ℃;
in the step S3, the vacuum degree of the vacuum freeze drying is less than 20Pa.
2. The method according to claim 1, wherein in step S1, the washing and drying steps include: and cleaning the root of the Ficus simplicissima lour with clear water, and then sucking the surface water by using water-absorbing filter paper.
3. A dried powder of hispid fig. prepared according to the freeze-drying process according to any one of claims 1 to 2.
CN202210850574.2A 2022-07-20 2022-07-20 Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder Active CN115282186B (en)

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 CN115282186A (en) 2022-11-04
CN115282186B true 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)

* Cited by examiner, † Cited by third party
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Title
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;叶茂森等;分子植物育种;第19卷(第22期);7398-7407 *

Also Published As

Publication number Publication date
CN115282186A (en) 2022-11-04

Similar Documents

Publication Publication Date Title
CN111494449B (en) Vacuum freeze-drying process for honeysuckle
CN103919712B (en) Cordyceps militaris extract, and preparation method and application thereof
CN112964804B (en) Method for preparing 5 anthocyanin standard products from blueberry anthocyanin extract
CN115282186B (en) Freeze-drying method for radix fici simplicissimae and radix fici simplicissimae dry powder
Fairbairn et al. The extraction and estimation of the cannabinoids in Cannabis sativa L. and its products
CN114224943A (en) Aronia melanocarpa extract and preparation method thereof
CN102274270B (en) Processing process for emblic leafflower fruit serving as Chinese medicine
CN107759710B (en) Preparation method of ambary hemp extract and application of ambary hemp extract in tobacco
CN101612177A (en) The construction method of Radix Cyathulae medicinal materials fingerprint and standard finger-print thereof
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
CN107362198B (en) Process for extracting scutellaria flavone, scutellaria flavone extract and its application
CN109200175A (en) A kind of preparation method of vacuum freeze drying fritillaria thunbergii
CN111505192A (en) Method for rapidly detecting content of picroside and hydroxytyrosol in olive leaves
CN115645446B (en) High-activity rhizoma panacis majoris decoction pieces and preparation method thereof
Wang et al. Investigation of the impact on the antioxidant capacity and Flavonoids components of different drying methods for Sophora japonica L.
CN115089629B (en) Ficus simplicissima lour freeze-dried fruit flavone extracting solution and preparation method thereof
Stanojević et al. The effect of the operation conditions and the extraction techniques on the yield, kinetics and composition of methanol extracts of Hieracium pilosella L.
CN111297919A (en) Abelmoschus manihot flower extract and preparation method thereof
CN108409545A (en) A kind of ether compound, preparation method and application
CN115651089B (en) Gastrodia elata polysaccharide with antioxidant activity
CN115097058B (en) Thin-layer chromatography identification method for Choerospondias axillaris
CN110075149B (en) Blumea balsamifera extract and preparation method thereof
Och et al. Screening various Juniperus species for the occurrence of umbelliferone by means of bivariate multiple development thin-layer chromatography
CN117630213A (en) Method for simultaneously measuring multiple chemical components in dracocephalum heterophyllum

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