CN114984119A - Saffron fluid extract and preparation process thereof - Google Patents

Saffron fluid extract and preparation process thereof Download PDF

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CN114984119A
CN114984119A CN202210895340.XA CN202210895340A CN114984119A CN 114984119 A CN114984119 A CN 114984119A CN 202210895340 A CN202210895340 A CN 202210895340A CN 114984119 A CN114984119 A CN 114984119A
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saffron
ethanol
fluid extract
solvent
preparation process
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王初
李繁荣
陈启宏
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Zhejiang Changdian Pharmaceutical Technology Development Co ltd
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    • 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)
    • A61K36/88Liliopsida (monocotyledons)
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0215Solid material in other stationary receptacles
    • B01D11/0219Fixed bed of solid material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/028Flow sheets
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D11/00Solvent extraction
    • B01D11/02Solvent extraction of solids
    • B01D11/0288Applications, solvents
    • 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
    • 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
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • 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
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A50/00TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
    • Y02A50/30Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change

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Abstract

The invention relates to the technical field of medicine preparation, in particular to a saffron fluid extract and a preparation process thereof, and provides the following scheme aiming at the problems that medicinal materials are difficult to store due to moisture, effective components are lost, the storage time is short, the medicinal materials cannot be effectively absorbed by human bodies and the like in the prior art, wherein the preparation method comprises the following steps: s1: selecting a saffron raw material, precisely weighing, drying at 105 ℃ for 6 hours until the weight loss is not more than 12%, determining the absorbance by using an ultraviolet-visible spectrophotometry, detecting whether the raw material is qualified, and entering the next link if the product is qualified; the invention aims to concentrate effective components by carrying out percolation and impregnation treatment on medicinal materials, wherein the medicinal materials do not contain leaching solvents, so that the effective components are stable, avoid being oxidized and volatilized by being affected with damp and can be stored for a long time; the liquid extract has small dosage, rapid absorption, short acting time, convenient carrying and administration, and good taste.

Description

Saffron fluid extract and preparation process thereof
Technical Field
The invention relates to the technical field of medicine preparation, in particular to a saffron fluid extract and a preparation process thereof.
Background
The fluid extract is a liquid extract preparation prepared by leaching the active ingredients of the medicinal materials with a proper solvent, evaporating part of the solvent, and adjusting the concentration to a specified standard. Each 1ml of the fluid extract is equivalent to the standard of 1g of the raw medicinal material, and ethanol is used as a preservative for facilitating storage. The application of the fluid nutrient is generally used as a raw material for preparing tincture, mixture, syrup or other preparations, and a few varieties can be directly used for medicine.
The extracts can be classified into thick extract and dry extract according to their drying degree. The thick extract is a finished product which is obtained by concentrating the leaching solution at low temperature into thick paste and has the water content of about 15-20%. The dry extract is obtained by concentrating the leachate to obtain soft extract, evaporating to dryness, measuring content, diluting with starch, lactose, etc. to specified standard, and making into dried powder product with water content of about 5%. The extract has the advantages of high content of effective components, small volume, no solvent, long storage time, and stable effective components.
Stigma croci Sativi has effects of promoting blood circulation for removing blood stasis, cooling blood, removing toxic substance, resolving stagnation and tranquilizing. The saffron fluid extract is used for treating amenorrhea, obstruction in the abdomen, postpartum stasis, toxic-heat spots, melancholy, stuffiness, palpitation and mania, is not easy to store saffron, easily causes the loss of effective components, has short storage time and can not be effectively absorbed by human bodies, so the saffron fluid extract and the preparation process thereof are provided.
Disclosure of Invention
The invention aims to solve the defects that medicinal materials are not easy to store due to moisture, active ingredients are lost, the storage time is short, and the medicinal materials cannot be effectively absorbed by a human body in the prior art, and provides a saffron fluid extract and a preparation process thereof.
In order to achieve the purpose, the invention adopts the following technical scheme:
a saffron fluid extract comprises the following raw materials in percentage by weight: 25-45% of saffron and 15-45% of ethanol; the balance of carrageenan;
preferably, the traditional Chinese medicine composition comprises, by weight, 25-35% of saffron and 20-45% of ethanol; the balance of carrageenan;
preferably, the beverage comprises the following raw materials, by weight, 25-30% of saffron and 20-40% of ethanol; the balance of carrageenan;
the preparation method comprises the following steps:
s1: selecting a saffron raw material, precisely weighing, drying at 105 ℃ for 6 hours until the weight loss is not more than 12%, determining the absorbance by using an ultraviolet-visible spectrophotometry, detecting whether the raw material is qualified or not, if the product is qualified, entering the next link, and if the product is not qualified, re-screening the raw material;
s2: pulverizing stigma croci Sativi according with specification, adding specified solvent, wetting, standing in sealed condition for a certain time, and percolating in a percolating tube;
s3: covering the powder surface with stainless steel pore plate, pressing tightly, opening the discharge valve below the percolating tube, placing into a container, slowly adding ethanol solution until the effluent reaches a specified amount, standing, and filtering;
s4: detecting whether the effective components reach the standard, adding carrageenan, heating and stirring until the liquid is colloidal, cooling, and standing;
s5: and detecting the microbial limit and ethanol content of the prepared fluid extract to determine whether the microbial limit and ethanol content are within the specified range.
Preferably, in S2, the product is taken and placed in a silica gel dryer, dried under reduced pressure for 24 hours, ground into fine powder, precisely weighed to 30mg, placed in a soxhlet extractor, added with 75ml of ethanol, heated and refluxed until the extract is colorless, cooled, moved to a 100ml measuring flask, washed with ethanol in several times, the washing liquid is merged into the same measuring flask, added with ethanol to the scale, and shaken up; precisely measuring 5ml, placing in a 50ml measuring flask, adding ethanol to scale, shaking, and measuring at 432nm wavelength by ultraviolet-visible spectrophotometry to obtain absorbance not lower than 0.50.
Preferably, in the S2, the granularity of the medicinal materials is proper; the medicinal powder is wetted by an extraction solvent before being filled into the percolation barrel, so that blockage caused by expansion in the percolation barrel is avoided, and the percolation operation is not influenced; adding a solvent in an amount which is 1 time of the medicinal powder, stirring uniformly, then placing for 15 min-6 h in a closed manner according to the quality of the medicinal materials, and stopping stirring when the medicinal powder is fully and uniformly wetted and expanded.
Preferably, in S3, the herbs should be uniformly loaded into the percolator with consistent tightness, air in gaps between the herbs should be removed as much as possible when the solvent is added, the solvent should be higher than the herbs surface, and percolation is performed after soaking for a proper time; collecting primary percolate with concentration of 85% during percolation, and storing in another container; mixing the secondary percolate and the primary percolate, and stirring.
Preferably, in the step S3, the amount of the solvent used for preparing the fluid extract is 4-8 times of the amount of the traditional Chinese medicine, and after all percolates are concentrated under normal pressure or reduced pressure, ethanol is added as a preservative.
Preferably, in S4, if it is determined whether the effective component meets the standard, content determination and ethanol content determination are required; the method comprises determining ethanol content, diluting the concentrated extractive solution with appropriate amount of solvent according to the determination result, standing for over 24 hr, and filtering.
The invention aims to concentrate effective components by carrying out percolation and impregnation treatment on medicinal materials, wherein the medicinal materials do not contain leaching solvents, so that the effective components are stable, avoid being oxidized and volatilized by being affected with damp and can be stored for a long time; the liquid extract has small dosage, rapid absorption, short acting time, convenient carrying and administration, and good taste.
Drawings
Fig. 1 is a flow diagram of a saffron fluid extract and a preparation process thereof provided by the invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments.
Example one
Referring to fig. 1, a saffron fluid extract comprises the following raw materials, by weight, 25% of saffron and 15% of ethanol; the balance of carrageenan;
the preparation method comprises the following steps:
s1: selecting saffron raw materials, accurately weighing, drying at 105 ℃ for 6 hours, reducing weight loss not to exceed 12%, measuring absorbance by using an ultraviolet-visible spectrophotometry, detecting whether the raw materials are qualified or not, entering the next link if the products are qualified, re-screening the raw materials if the products are not qualified, taking the products, placing the products in a silica gel dryer, drying under reduced pressure for 24 hours, grinding into fine powder, accurately weighing 30mg, placing the fine powder in a Soxhlet extractor, adding 75ml of ethanol, heating and refluxing until the extract is colorless, cooling, transferring the extract to a 100ml measuring flask, washing the extractor with ethanol in times, merging the washing liquid into the same measuring flask, adding the ethanol to the scale, and shaking uniformly; precisely measuring 5ml, placing in a 50ml measuring flask, adding ethanol to scale, shaking, and measuring at 432nm wavelength by ultraviolet-visible spectrophotometry until the absorbance is not lower than 0.50;
s2: pulverizing stigma croci Sativi according with specification, adding specified solvent, wetting, sealing, standing for a certain time, and percolating in a percolating tube with proper granularity; the medicinal powder is wetted by an extraction solvent before being filled into the percolation barrel, so that blockage caused by expansion in the percolation barrel is avoided, and the percolation operation is not influenced; adding solvent 1 times of the medicinal powder, stirring, sealing and standing for 15min according to the quality of the medicinal materials, and stopping stirring when the medicinal powder is fully and uniformly wetted and expanded;
s3: covering the powder surface with a stainless steel pore plate, pressing tightly, opening a discharge valve below a percolation cylinder, placing in a container, slowly adding ethanol solution until the effluent reaches a specified amount, standing, filtering, uniformly and uniformly loading the medicinal materials into the percolation apparatus, adding solvent while removing air in gaps between the medicinal materials, and percolating after soaking for a proper time; collecting primary percolate with concentration of 85% during percolating, and storing in another container; mixing the secondary percolate and the primary percolate, stirring, concentrating the percolate at normal pressure or under reduced pressure, and adding ethanol as antiseptic, wherein the amount of solvent is 4 times of the amount of the primary percolate;
s4: detecting whether the effective components reach the standard, adding carrageenan, heating and stirring until the liquid is colloidal, cooling, standing, detecting whether the effective components reach the standard, and if the effective components are clear, performing content determination and ethanol content determination; only determining the ethanol content of the undefined active ingredient, then diluting the concentrated extract with appropriate amount of solvent according to the determination result, keeping standing for more than 24 hr, and filtering;
s5: and detecting the microbial limit and ethanol content of the prepared fluid extract to determine whether the microbial limit and ethanol content are within the specified range.
Example two
Referring to fig. 1, a saffron fluid extract comprises the following raw materials, by weight, 45% of saffron and 45% of ethanol; the balance of carrageenan;
the preparation method comprises the following steps:
s1: selecting saffron raw materials, accurately weighing, drying at 105 ℃ for 6 hours, reducing weight loss not to exceed 12%, measuring absorbance by using an ultraviolet-visible spectrophotometry, detecting whether the raw materials are qualified or not, entering the next link if the products are qualified, re-screening the raw materials if the products are not qualified, taking the products, placing the products in a silica gel dryer, drying under reduced pressure for 24 hours, grinding into fine powder, accurately weighing 30mg, placing the fine powder in a Soxhlet extractor, adding 75ml of ethanol, heating and refluxing until the extract is colorless, cooling, transferring the extract to a 100ml measuring flask, washing the extractor with ethanol in times, merging the washing liquid into the same measuring flask, adding the ethanol to the scale, and shaking uniformly; precisely measuring 5ml, placing in a 50ml measuring flask, adding ethanol to scale, shaking, and measuring at 432nm wavelength by ultraviolet-visible spectrophotometry until the absorbance is not lower than 0.50;
s2: pulverizing stigma croci Sativi according with specification, adding specified solvent, wetting, sealing, standing for a certain time, and percolating in a percolating tube with proper granularity; the medicinal powder is wetted by a leaching solvent before being filled in a percolation barrel, so that the phenomenon that the percolation operation is influenced due to blockage caused by expansion in the percolation barrel is avoided; adding solvent 1 times of the powder, stirring, sealing and standing for 4 hr according to the quality of the medicinal materials, and stopping stirring when the powder is fully and uniformly wetted and expanded;
s3: covering the powder surface with a stainless steel pore plate, pressing tightly, opening a discharge valve below a percolation cylinder, placing in a container, slowly adding ethanol solution until the effluent reaches a specified amount, standing, filtering, uniformly and uniformly loading the medicinal materials into the percolation apparatus, adding solvent while removing air in gaps between the medicinal materials, and percolating after soaking for a proper time; collecting primary percolate with concentration of 85% during percolation, and storing in another container; mixing the secondary percolate and the primary percolate, stirring, concentrating all percolates under normal pressure or reduced pressure with solvent amount 6 times of the amount of the Chinese medicinal materials, and adding ethanol as antiseptic;
s4: detecting whether the effective components reach the standard, adding carrageenan, heating and stirring until the liquid is colloidal, cooling, standing, and detecting whether the effective components reach the standard, if the effective components are clear, performing content determination and ethanol content determination; determining ethanol content, diluting the concentrated extractive solution with appropriate amount of solvent according to determination result, standing for over 24 hr, and filtering;
s5: and detecting the microbial limit and ethanol content of the prepared fluid extract to determine whether the microbial limit and ethanol content are within the specified range.
EXAMPLE III
Referring to fig. 1, a saffron fluid extract comprises the following raw materials, by weight, 30% of saffron and 40% of ethanol; the balance of carrageenan;
the preparation method comprises the following steps:
s1: selecting saffron raw materials, accurately weighing, drying at 105 ℃ for 6 hours, reducing weight loss not to exceed 12%, measuring absorbance by using an ultraviolet-visible spectrophotometry, detecting whether the raw materials are qualified or not, entering the next link if the products are qualified, re-screening the raw materials if the products are not qualified, taking the products, placing the products in a silica gel dryer, drying under reduced pressure for 24 hours, grinding into fine powder, accurately weighing 30mg, placing the fine powder in a Soxhlet extractor, adding 75ml of ethanol, heating and refluxing until the extract is colorless, cooling, transferring the extract to a 100ml measuring flask, washing the extractor with ethanol in times, merging the washing liquid into the same measuring flask, adding the ethanol to the scale, and shaking uniformly; precisely measuring 5ml, placing in a 50ml measuring flask, adding ethanol to scale, shaking, and measuring at 432nm wavelength by ultraviolet-visible spectrophotometry until the absorbance is not lower than 0.50;
s2: pulverizing stigma croci Sativi according with specification, adding specified solvent, wetting, sealing, standing for a certain time, and percolating in a percolating tube with proper granularity; the medicinal powder is wetted by a leaching solvent before being filled in a percolation barrel, so that the phenomenon that the percolation operation is influenced due to blockage caused by expansion in the percolation barrel is avoided; adding solvent 1 times of the medicinal powder, stirring, sealing and standing for 6 hr according to medicinal material quality, and stopping stirring when the medicinal powder is fully and uniformly wetted and expanded;
s3: covering the powder surface with a stainless steel pore plate, pressing tightly, opening a discharge valve below a percolation cylinder, placing in a container, slowly adding ethanol solution until the effluent reaches a specified amount, standing, filtering, uniformly and uniformly loading the medicinal materials into the percolation apparatus, adding solvent while removing air in gaps between the medicinal materials, and percolating after soaking for a proper time; collecting primary percolate with concentration of 85% during percolation, and storing in another container; mixing the secondary percolate and the primary percolate, stirring, using solvent 8 times of the Chinese medicinal materials when preparing fluid extract, concentrating all percolates under normal pressure or reduced pressure, and adding ethanol as antiseptic;
s4: detecting whether the effective components reach the standard, adding carrageenan, heating and stirring until the liquid is colloidal, cooling, standing, detecting whether the effective components reach the standard, and if the effective components are clear, performing content determination and ethanol content determination; only determining the ethanol content of the undefined active ingredient, then diluting the concentrated extract with appropriate amount of solvent according to the determination result, keeping standing for more than 24 hr, and filtering;
s5: and detecting the microbial limit and ethanol content of the prepared fluid extract to determine whether the microbial limit and ethanol content are within the specified range.
Comparative example 1
The difference from the first embodiment is that, S1: selecting stigma croci Sativi raw material, accurately weighing until total ash content is no more than 7.5%, measuring absorbance by ultraviolet-visible spectrophotometry, drying the product in a silica gel drier under reduced pressure for 24 hr, grinding into fine powder, accurately weighing 30mg, placing in a Soxhlet extractor, adding 75ml ethanol, heating and refluxing until the extractive solution is colorless, cooling, transferring the extractive solution into a 100ml measuring flask, washing the extractor with ethanol, mixing the washing solution with the same measuring flask, adding ethanol to scale, and shaking; measured by UV-visible spectrophotometry at 432nm, the absorbance should not be less than 0.50.
Comparative example No. two
The difference from the first embodiment is that, S2: after the crocus sativus medicinal material which meets the specification is properly crushed, a specified solvent is added for uniform wetting, the granularity of the medicinal material is proper, the medicinal material is too fine and is easy to block, the adsorbability is enhanced, and the leaching effect is poor; the medicine is too coarse and is not easy to compress, and the contact surface of the solvent and the medicinal materials is small, so that the leaching effect is influenced; the medicinal powder is wetted by a leaching solvent before being filled in a percolation barrel, so that the phenomenon that the percolation operation is influenced due to blockage caused by expansion in the percolation barrel is avoided; after being mixed evenly, the mixture is placed for 4 hours in a sealed way according to the texture of the medicinal materials, and the stirring is stopped when the medicinal powder is fully and evenly wetted and expanded.
Comparative example No. three
The difference from the first embodiment is that, S3: covering the powder surface with stainless steel pore plate, pressing tightly, opening discharge valve below the percolation barrel, placing into a container, slowly adding ethanol solution until the effluent reaches a specified amount, standing, filtering, adding solvent while removing air from gaps between the medicinal materials, soaking for a proper time, and percolating; collecting primary percolate with concentration of 85% during percolating, and storing in another container; mixing the secondary percolate and the primary percolate, stirring, concentrating all percolates under normal pressure or reduced pressure with solvent amount 8 times of the Chinese medicinal materials, and adding ethanol as antiseptic.
Examples of the experiments
The saffron fluid extract of the first, second and third examples was tested to obtain the following results:
example one Example two EXAMPLE III The existing stigma croci fluid extract
Preparation ofPeriod of time 2.5h 6.5h 6h 7h
Retention rate of effective component 85% 45% 35% 54%
The saffron fluid extracts prepared in the first embodiment, the second embodiment and the third embodiment have the advantages that the retention rate of active ingredients of the saffron fluid extracts is remarkably improved, the preparation period is remarkably reduced, and the first embodiment is the best embodiment.
Detection reporting
The invention aims to concentrate effective components by carrying out percolation and impregnation treatment on medicinal materials, wherein the medicinal materials do not contain leaching solvents, so that the effective components are stable, avoid being oxidized and volatilized by being affected with damp and can be stored for a long time; the liquid extract has small dosage, rapid absorption, short acting time, convenient carrying and administration, and good taste.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.

Claims (9)

1. A saffron fluid extract is characterized by comprising the following raw materials, by weight, 25-45% of saffron and 15-45% of ethanol; the balance of carrageenan.
2. The saffron fluid extract according to claim 1, which comprises 25-35 wt% of saffron and 20-45 wt% of ethanol; the balance of carrageenan.
3. The saffron fluid extract according to claim 1, which comprises 25-30% by weight of saffron and 20-40% by weight of ethanol; the balance of carrageenan.
4. The preparation process of saffron fluid extract according to claim 1, comprising the steps of:
s1: selecting a saffron raw material, wherein the total ash content is not more than 7.5%, precisely weighing, drying at 105 ℃ for 6 hours, reducing the weight loss to not more than 12%, measuring the absorbance by using an ultraviolet-visible spectrophotometry, detecting whether the raw material is qualified or not, if the product is qualified, entering the next link, and if the product is not qualified, re-screening the raw material;
s2: pulverizing stigma croci Sativi according with specification, adding specified solvent, wetting, standing in sealed condition for a certain time, and percolating in a percolating tube;
s3: covering the powder surface with stainless steel pore plate, pressing tightly, opening the discharge valve below the percolating tube, placing into a container, slowly adding ethanol solution until the effluent reaches a specified amount, standing, and filtering;
s4: detecting whether the effective components reach the standard, adding carrageenan, heating and stirring until the liquid is colloidal, cooling, and standing;
s5: and detecting the microbial limit and ethanol content of the prepared fluid extract to determine whether the microbial limit and ethanol content are within the specified range.
5. The preparation process of saffron fluid extract according to claim 4, wherein in S1, the saffron fluid extract is prepared by drying the product in a silica gel dryer under reduced pressure for 24 hours, grinding into fine powder, precisely weighing 30mg, placing in a Soxhlet extractor, adding 75ml ethanol, heating and refluxing until the extract is colorless, cooling, transferring the extract to a 100ml measuring flask, washing the extractor with ethanol in several times, merging the washing solution into the same measuring flask, adding ethanol to the scale, and shaking up; precisely measuring 5ml, placing in a 50ml measuring flask, adding ethanol to scale, shaking, and measuring at 432nm wavelength by ultraviolet-visible spectrophotometry to obtain absorbance not lower than 0.50.
6. The preparation process of saffron fluid extract according to claim 4, wherein in S2, the particle size of the herbs should be suitable; the medicinal powder is wetted by a leaching solvent before being filled in a percolation barrel, so that the phenomenon that the percolation operation is influenced due to blockage caused by expansion in the percolation barrel is avoided; adding a solvent in an amount which is 1 time of the medicinal powder, stirring uniformly, then placing for 15 min-6 h in a closed manner according to the quality of the medicinal materials, and stopping stirring when the medicinal powder is fully and uniformly wetted and expanded.
7. The preparation process of saffron fluid extract according to claim 4, wherein in step S3, the herbs are uniformly and uniformly loaded into the percolator, and the air in the gaps between the herbs is removed when the solvent is added, and the solvent is higher than the herbs surface, and the percolation is performed after the herbs are soaked for a proper time; collecting primary percolate with concentration of 85% during percolation, and storing in another container; mixing the secondary percolate and the primary percolate, and stirring.
8. The preparation process of saffron fluid extract according to claim 4, wherein in S3, the amount of solvent used in the preparation of the fluid extract is 4-8 times of the amount of the traditional Chinese medicine, and ethanol is added as preservative after all percolates are concentrated under normal pressure or reduced pressure.
9. The preparation process of saffron fluid extract according to claim 4, wherein in step S4, if the effective components are determined, the content determination and ethanol content determination are required when the effective components are determined to be up to standard; the method comprises determining ethanol content, diluting the concentrated extractive solution with appropriate amount of solvent according to the determination result, standing for over 24 hr, and filtering.
CN202210895340.XA 2022-07-28 2022-07-28 Saffron fluid extract and preparation process thereof Pending CN114984119A (en)

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CN113144057A (en) * 2021-06-03 2021-07-23 上海瀛洲西红花种植专业合作社 Stigma croci extract and preparation method and application thereof

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