CN107854550B - Preparation method of processing auxiliary material fructus evodiae juice - Google Patents
Preparation method of processing auxiliary material fructus evodiae juice Download PDFInfo
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- CN107854550B CN107854550B CN201711432659.4A CN201711432659A CN107854550B CN 107854550 B CN107854550 B CN 107854550B CN 201711432659 A CN201711432659 A CN 201711432659A CN 107854550 B CN107854550 B CN 107854550B
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- 235000011389 fruit/vegetable juice Nutrition 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000000463 material Substances 0.000 title abstract description 11
- 238000012545 processing Methods 0.000 title abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 44
- 241001078983 Tetradium ruticarpum Species 0.000 claims abstract description 35
- 238000002791 soaking Methods 0.000 claims abstract description 11
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 81
- 238000001914 filtration Methods 0.000 claims description 19
- 239000002904 solvent Substances 0.000 claims description 17
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 238000001816 cooling Methods 0.000 claims description 9
- 239000000706 filtrate Substances 0.000 claims description 9
- 239000003960 organic solvent Substances 0.000 claims description 9
- 239000006228 supernatant Substances 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 6
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 4
- 239000012982 microporous membrane Substances 0.000 claims 1
- ACVGWSKVRYFWRP-UHFFFAOYSA-N Rutecarpine Chemical compound C1=CC=C2C(=O)N(CCC=3C4=CC=CC=C4NC=33)C3=NC2=C1 ACVGWSKVRYFWRP-UHFFFAOYSA-N 0.000 abstract description 28
- HMXRXBIGGYUEAX-SFHVURJKSA-N Evodiamine Natural products CN1[C@H]2N(CCc3[nH]c4ccccc4c23)C(=O)c5ccccc15 HMXRXBIGGYUEAX-SFHVURJKSA-N 0.000 abstract description 22
- TXDUTHBFYKGSAH-SFHVURJKSA-N Evodiamine Chemical compound C1=CC=C2N(C)[C@@H]3C(NC=4C5=CC=CC=4)=C5CCN3C(=O)C2=C1 TXDUTHBFYKGSAH-SFHVURJKSA-N 0.000 abstract description 20
- BCPAKGGXGLGKIO-UHFFFAOYSA-N Pseudorutaecarpin Natural products C1=CC=C2C(=O)N(CCC3=C4C5=CC=CC=C5N3)C4=NC2=C1 BCPAKGGXGLGKIO-UHFFFAOYSA-N 0.000 abstract description 14
- 238000000605 extraction Methods 0.000 abstract description 14
- 238000002137 ultrasound extraction Methods 0.000 abstract description 3
- 238000001514 detection method Methods 0.000 description 9
- 241000037740 Coptis chinensis Species 0.000 description 6
- -1 evodia fruit lactone Chemical class 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000005303 weighing Methods 0.000 description 5
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 150000002596 lactones Chemical class 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 239000012085 test solution Substances 0.000 description 4
- KBDSLGBFQAGHBE-MSGMIQHVSA-N limonin Chemical compound C=1([C@H]2[C@]3(C)CC[C@H]4[C@@]([C@@]53O[C@@H]5C(=O)O2)(C)C(=O)C[C@@H]2[C@]34COC(=O)C[C@@H]3OC2(C)C)C=COC=1 KBDSLGBFQAGHBE-MSGMIQHVSA-N 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000012088 reference solution Substances 0.000 description 3
- 239000013558 reference substance Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 239000006071 cream Substances 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000002401 inhibitory effect Effects 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 238000010992 reflux Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 1
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 1
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 208000007536 Thrombosis Diseases 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000036760 body temperature Effects 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 238000004440 column chromatography Methods 0.000 description 1
- 239000013068 control sample Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007872 degassing Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000035622 drinking Effects 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 235000015203 fruit juice Nutrition 0.000 description 1
- 210000000232 gallbladder Anatomy 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 235000008216 herbs Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000013074 reference sample Substances 0.000 description 1
- 238000013077 scoring method Methods 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 229910021642 ultra pure water Inorganic materials 0.000 description 1
- 239000012498 ultrapure water Substances 0.000 description 1
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- 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)
- A61K36/75—Rutaceae (Rue family)
- A61K36/754—Evodia
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K47/00—Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
- A61K47/46—Ingredients of undetermined constitution or reaction products thereof, e.g. skin, bone, milk, cotton fibre, eggshell, oxgall or plant extracts
-
- 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
-
- 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
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation or decoction
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- 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
- A61K2236/30—Extraction of the material
- A61K2236/39—Complex extraction schemes, e.g. fractionation or repeated extraction steps
-
- 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
- A61K2236/50—Methods involving additional extraction steps
- A61K2236/53—Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization
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- Life Sciences & Earth Sciences (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Veterinary Medicine (AREA)
- Medicinal Chemistry (AREA)
- Pharmacology & Pharmacy (AREA)
- Epidemiology (AREA)
- Animal Behavior & Ethology (AREA)
- General Health & Medical Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Alternative & Traditional Medicine (AREA)
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Abstract
The invention provides a preparation method of a processing auxiliary material evodia rutaecarpa juice, which is characterized in that a series of links such as water addition amount, soaking time, decoction times, decoction time and ultrasonic extraction are controlled, so that the evodia rutaecarpa juice containing evodiamine, evodiamine and rutaecarpine is obtained. The extraction method is simple, does not use special instruments, is simple and convenient to operate, does not use extreme conditions such as temperature, pressure and the like, has short extraction time, and is very suitable for industrial operation.
Description
Technical Field
The invention belongs to the technical field of medicines, and particularly relates to a preparation method of a processing auxiliary material fructus evodiae juice.
Background
Wu Zhu Yu was recorded in Shen nong Ben Cao Jing (Shen nong's herbal) listed in the Shang Pin and the past generation. Evodia rutaecarpa is one of the commonly used Chinese herbs, and has the effects of dispelling cold, relieving pain, soothing liver, descending qi, and drying dampness. Evodia rutaecarpa is a medicine and an auxiliary material, and is commonly used for processing coptis chinensis, namely, coptis chinensis. After being processed by the evodia rutaecarpa juice, the coptis chinensis has changed nature, taste and function indications, is different from evodia rutaecarpa and is also different from coptis chinensis, has the effects of inhibiting the cold property of coptis chinensis and keeping coptis chinensis cold without stagnation, and is mainly used for clearing qi, dispersing damp and heat and dispersing stagnated fire of liver and gallbladder. However, at present, most drinking tablet factories in China have no strict specifications and standards for processing and using the evodia rutaecarpa juice, particularly for the preparation process parameters and the quality of the evodia rutaecarpa juice. Processing auxiliary materials, especially liquid auxiliary materials, as an additive in the processing of decoction pieces directly affect the quality of the decoction pieces, and high attention should be paid.
Researches show that the evodia rutaecarpa juice used as a processing auxiliary material contains chemical components such as evodiamine, rutaecarpine, evodia fruit lactone and the like, and the researches also show that the chemical substances play important roles in resisting experimental gastric ulcer, easing pain, inhibiting body temperature rise, resisting thrombosis, resisting tumors and the like. However, the existing preparation method of the processing auxiliary material evodia rutaecarpa juice mainly has the defects of low content of evodiamine and rutaecarpine or/and evodiamine, long process time and the like.
Disclosure of Invention
In order to solve the problems in the prior art, the invention aims to provide a method for preparing evodia rutaecarpa juice, the evodia rutaecarpa juice prepared by the method has high content of evodiamine, rutaecarpine and evodia rutaecarpa lactone, the process time is short, and the method has obvious industrial prospect.
Except for special description, the parts are parts by weight, and the percentages are mass percentages.
The purpose of the invention is realized as follows:
the preparation method of the evodia rutaecarpa juice is characterized by comprising the following steps: decocting fructus evodiae in water to obtain fructus evodiae decoction, wherein the amount of water is 8-12 times of the amount of water, soaking for 30-60min, and decocting for 1-3 times, each for 30-90 min; then recovering the solvent from the prepared fructus evodiae decoction by using a rotary evaporator, adding an organic solvent for dissolving, ultrasonically extracting for 30-60min, cooling, adding the organic solvent for complementing the weight, filtering, centrifuging the filtrate for 8-12min at 15000-; the organic solvent is methanol or a mixed solution of acetonitrile-water.
In the preparation method of the evodia rutaecarpa juice, preferably, the evodia rutaecarpa is decocted in water to prepare a evodia rutaecarpa water decoction, the water addition amount is 12 times of water, the soaking time is 30min, the decoction is carried out for 3 times, and each time of the decoction is 30 min.
In the preparation method of the evodia rutaecarpa juice, the volume ratio of acetonitrile to water in the acetonitrile-water mixed solution is 6: 4.
In the preparation method of the evodia rutaecarpa juice, preferably, the organic solvent is methanol; more preferably 100% methanol. The preparation method of the evodia rutaecarpa juice further comprises the steps of recovering the solvent of the prepared evodia rutaecarpa water decoction by using a rotary evaporator, adding 100 percent of methanol for dissolving, ultrasonically extracting for 30min, cooling, adding 100 percent of methanol for complementing the weight, filtering, centrifuging the filtrate for 10min at 16000r/min, and filtering the obtained supernatant by using a microporous filter membrane to obtain the evodia rutaecarpa juice.
Specifically, the preparation method of the evodia rutaecarpa juice is characterized by comprising the following steps: decocting fructus evodiae in water to obtain fructus evodiae decoction, wherein the amount of water added is 12 times of water, soaking time is 30min, and decocting for 30min for 3 times; then recovering solvent from the prepared fructus evodiae decoction by using a rotary evaporator, adding 100% methanol for dissolving, ultrasonically extracting for 30min, cooling, adding 100% methanol for complementing weight, filtering, centrifuging the filtrate for 10min at 16000r/min, and filtering the obtained supernatant by using a 0.45-micrometer microporous filter membrane to obtain the fructus evodiae juice.
Has the advantages that:
the invention provides a preparation method of evodia rutaecarpa juice, which is characterized in that a series of links such as water addition amount, soaking time, decoction times, decoction time and ultrasonic extraction are controlled, so that the evodia rutaecarpa juice containing evodiamine, evodiamine and rutaecarpine is obtained. The extraction method is simple, does not use special instruments (such as low-temperature equipment and the like), is simple and convenient to operate, does not use extreme conditions such as temperature, pressure and the like, has short extraction time, and is very suitable for industrial operation.
Detailed Description
The present invention is described in detail below with reference to specific examples, which are given for the purpose of further illustrating the invention and are not to be construed as limiting the scope of the invention, and the invention may be modified and adapted by those skilled in the art in light of the above disclosure. All the raw materials and reagents of the invention are commercial products.
Experimental Material
Raw materials: the evodia rutaecarpa is purchased from the market of Ducheng lotus Chinese medicinal materials. Reagent and reagent testing: the evodiamine reference substance (lot No. 141029), the rutaecarpine reference substance (lot No. 150407), and the evodiamine reference substance (lot No.) were purchased from Kyoto BioPhilide technologies, Inc.; chromatographically pure acetonitrile (Fisher corporation, USA), chromatographic grade methanol, water as ultrapure water, and the rest of the reagents were analytically pure. An experimental instrument: agilent1260 high performance liquid chromatograph (with quaternary gradient pump unit, ChemStation chromatography workstation, automatic temperature control sample introduction unit, automatic degassing unit, DAD diode array detector unit, Agilent technologies, usa), DL-720D model digital controlled ultrasonic cleaner (shanghai news instrument ltd), TGL-16G high speed desktop centrifuge (shanghai ann pavilion scientific instrument factory), BT125D electronic analytical balance (one hundred thousandth, sydow instruments ltd), RE-2000B model rotary evaporator (shanghai subsun biochemical instrument factory).
Example 1
Decocting fructus evodiae in water to obtain fructus evodiae decoction, wherein the amount of water added is 12 times of water, soaking time is 30min, and decocting for 30min for 3 times; then recovering solvent from the prepared fructus evodiae decoction by using a rotary evaporator, adding 100% methanol for dissolving, ultrasonically extracting for 30min, cooling, adding 100% methanol for complementing weight, filtering, centrifuging the filtrate for 10min at 16000r/min, and filtering the supernatant by using a 0.45-micrometer microporous filter membrane to obtain the fructus evodiae juice extracting solution.
Example 2
Referring to the preparation method of example 1, the influence of the decoction process on the extraction results was examined, and the main examination indexes include water addition amount, soaking time, decoction times and the like, and the examination indexes are shown in tables 1 and 2 below.
TABLE 1 horizontal table of technological factors for decoction of fructus evodiae juice
TABLE 2 decocte process test table
Filtering with 200 mesh gauze after decocting, adding distilled water to constant volume to the filtrate, and using as decoction for standby. The volume is shown in table 3.
TABLE 3 constant volume of water decoction
Determination of cream yield
Precisely measuring 25ml of the decoction, putting the decoction in an evaporation dish with constant weight, heating in water bath for volatilizing, drying in an oven at 105 ℃ to constant weight, weighing, calculating the paste yield, and calculating the average value of 2 parts in parallel of each group. The cream yield results are shown in table 4.
The dry extract rate (dry extract weight 1000ml/25 ml)/raw material weight 100g 100%
TABLE 4 determination of Dry paste Rate
EXAMPLE 3 measurement of Components
Preparation of a test solution: decocting fructus evodiae in water to obtain fructus evodiae decoction, wherein the amount of water added is 12 times of water, soaking time is 30min, and decocting for 30min for 3 times; then recovering solvent from the prepared fructus evodiae decoction by using a rotary evaporator, adding 100% methanol for dissolving, ultrasonically extracting for 30min, cooling, adding 100% methanol for complementing the weight, filtering, centrifuging the filtrate for 10min at 16000r/min, and filtering the supernatant by using a 0.45-micrometer microporous filter membrane to obtain a test solution.
Preparation of control solutions: precisely weighing evodiamine control 2mg (0.00244g), rutaecarpine control 1mg (0.00127g) and evodiamine control 2mg (0.00255g), adding 100% methanol solution to desired volume of 25ml, centrifuging at 16000r/min for 15min, and collecting supernatant. Wherein the concentration of the evodia rutaecarpa reference solution is 97.6 μ g/ml, the concentration of the rutaecarpine reference solution is 50.8 μ g/ml, and the concentration of the evodia rutaecarpa lactone reference solution is 0.102 mg/ml.
Sample detection: a Kromasil C18 column chromatography was used, with acetonitrile (A) -0.01% phosphoric acid water (B) (51: 49) as the mobile phase, at a flow rate of 1.0ml/min, at a sample rate of 10. mu.l, at a column temperature of 25 ℃ and a detection wavelength of 215 nm. The retention time of the chromatographic peaks of the evodiamine, the rutaecarpine and the evodia lactone in the test sample is basically consistent with that of the reference sample, the chromatographic peaks of the components can be well separated, and the methanol solvent has no interference to the content measurement. The contents of evodiamine, rutaecarpine and evodia fruit lactone in the evodia fruit juice are calculated according to the following formula:
yevodiamine＝10853xEvodiamine-59.248, correlation coefficient γ being 1.0000;
yrutaecarpine＝5199.7xRutaecarpine14.244, correlation coefficient R2＝0.9999；
yEvodiamine derivative＝524.77xEvodiamine derivative3.4308, correlation coefficient R2＝0.9999；
Wherein, XEvodiamineIs the mass concentration of evodiamine, the unit is mg/ml, YEvodiaminePeak area detected by a high performance liquid chromatograph; xRutaecarpineThe unit is mg/ml and Y is the quality concentration of the rutaecarpineRutaecarpinePeak area detected by a high performance liquid chromatograph; xEvodiamine derivativeIs the mass concentration of the evodia fruit lactone, the unit is mg/ml, YEvodiamine derivativeThe peak area is detected by a high performance liquid chromatograph.
Example 4
The influence of the extraction solvent on the detection results was examined with reference to the detection method of example 3. Taking 10ml of each of 4 parts of fructus evodiae water decoction, recovering the solvent by using a rotary evaporator, adding 20ml of 100% methanol into two parts, adding 20ml of acetonitrile-water (6: 4) into the other two parts, precisely weighing, performing reflux extraction for 1h, taking out, adding the extraction solvent to complement the weight, filtering, sucking 2ml, centrifuging at 16000r/min for 10min, and taking the supernatant to obtain the fructus evodiae water decoction. The contents of three components in the solution are measured, and the detection results are shown in Table 5.
TABLE 5 comparison of different extraction solvents for the main effective components in the test solutions
The results show that the extraction efficiency is superior to other solvents when 100% methanol is used as the extraction solvent.
Example 5
The influence of the preparation method on the detection results was examined with reference to the detection method of example 3. Taking 10ml of each of 4 parts of fructus evodiae water decoction, recovering the solvent by using a rotary evaporator, respectively adding 20ml of 100% methanol, precisely weighing the weight, refluxing and extracting two parts for 1h, ultrasonically extracting the other two parts for 30min, taking out, adding 100% methanol to complement the weight, filtering, sucking 2ml, centrifuging at 16000r/min for 10min, and taking the supernatant to obtain the fructus evodiae decoction. The contents of three components in the solution were measured, and the results are shown in Table 6.
TABLE 6 examination results of the extraction method
The result shows that the total content of the evodiamine, the rutaecarpine and the evodiamine lactone in the obtained evodia rutaecarpa juice is highest and the extraction is most complete after the ultrasonic extraction is carried out for 0.5 h.
Example 6
With reference to the detection method in example 3, test solutions prepared from the 9 groups of fructus evodiae water decoctions in table 2 above were measured, and the contents of evodiamine, rutaecarpine, and evodiamine lactone in each test sample were calculated. The results are shown in Table 7.
Table 7 results of content measurement (n ═ 9)
According to the detection result, the medicinal evodia fruit powder is added with 12 times of water, soaked for 30min and then decocted for 3 times, 30min of decoction is carried out each time to prepare the medicinal evodia fruit water decoction, and the overall level of the contents of the evodiamine, the rutaecarpine and the evodiamine is the highest.
Example 7
The optimal decoction process of the evodia rutaecarpa juice is selected by adopting a comprehensive scoring method, the standard of the evodia rutaecarpa lactone and the evodiamine is 30 minutes, the standard of the rutaecarpine is 20 minutes, the standard of the dry extract rate is 20 minutes, and the scoring result is shown in table 8.
TABLE 8 comprehensive scoring table
According to the scoring result, the highest scoring score is 88.8 points, namely the test number is 8, so the best extraction method of the effective components of the fructus evodiae comprises the following steps: soaking fructus evodiae in 12 times of water for 30min, and decocting for 3 times (each time for 30 min) to obtain fructus evodiae decoction; then taking 10ml of fructus evodiae water decoction, recovering the solvent by using a rotary evaporator, adding 20ml of 100% methanol for dissolving, precisely weighing, ultrasonically extracting for 0.5h, cooling, adding methanol for supplementing the weight, filtering by using filter paper, sucking 2ml, centrifuging for 10min at 16000r/min, and taking supernate and filtering by using a 0.45 mu m microporous filter membrane to obtain the fructus evodiae water decoction.
Claims (5)
1. A preparation method of fructus evodiae juice is characterized by comprising the following steps: decocting fructus evodiae in water to obtain fructus evodiae decoction, wherein the amount of water added is 12 times of water, soaking time is 30min, and decocting for 30min for 3 times; then recovering the solvent from the prepared fructus evodiae decoction by using a rotary evaporator, adding an organic solvent for dissolving, ultrasonically extracting for 30-60min, cooling, adding the organic solvent for complementing the weight, filtering, centrifuging the filtrate for 8-12min at 15000-; the organic solvent is methanol or a mixed solution of acetonitrile-water; the volume ratio of acetonitrile to water of the acetonitrile-water mixed solution is 6: 4.
2. The method for preparing evodia rutaecarpa juice as claimed in claim 1, wherein: the organic solvent is methanol.
3. The method for preparing evodia rutaecarpa juice as claimed in claim 1, wherein: the organic solvent is 100% methanol.
4. The method for preparing evodia rutaecarpa juice as claimed in claim 1, wherein: recovering solvent from the fructus evodiae decoction by rotary evaporator, dissolving in 100% methanol, ultrasonic extracting for 30min, cooling, adding 100% methanol to make up the weight, filtering, centrifuging the filtrate at 16000r/min for 10min, and filtering the supernatant with microporous membrane.
5. A preparation method of fructus evodiae juice is characterized by comprising the following steps: decocting fructus evodiae in water to obtain fructus evodiae decoction, wherein the amount of water added is 12 times of water, soaking time is 30min, and decocting for 30min for 3 times; and then recovering the solvent from the prepared fructus evodiae water decoction by using a rotary evaporator, adding 100% methanol for dissolving, ultrasonically extracting for 30min, cooling, adding 100% methanol for complementing the weight, filtering, centrifuging the filtrate for 10min at 16000r/min, and filtering the supernatant by using a 0.45 mu m microporous filter membrane to obtain the fructus evodiae water decoction.
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| CN1931271A (en) * | 2006-09-27 | 2007-03-21 | 贵州师范大学 | Evodia extract and its prepn process, medicine composition and use |
| CN102141555A (en) * | 2010-12-27 | 2011-08-03 | 贵阳中医学院 | Method for establishing high-pressure liquid-phase fingerprinting of evodia and extractives thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1931271A (en) * | 2006-09-27 | 2007-03-21 | 贵州师范大学 | Evodia extract and its prepn process, medicine composition and use |
| CN102141555A (en) * | 2010-12-27 | 2011-08-03 | 贵阳中医学院 | Method for establishing high-pressure liquid-phase fingerprinting of evodia and extractives thereof |
Non-Patent Citations (1)
| Title |
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| 左金丸血清药物化学研究;龚梦鹃等;《中国民族民间医药》;20170630;第26卷(第11期);第56-62页 * |
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