CN113018332A - Cistanche tubulosa extract and preparation method thereof - Google Patents
Cistanche tubulosa extract and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a cistanche tubulosa extract and a preparation method thereof, wherein the preparation method comprises the following steps: mixing pretreated cistanche tubulosa with deionized water, performing multi-stage countercurrent ultrasonic extraction, filtering, and mixing filtrates to obtain filter residue and an extract I; mixing the filter residue with ethanol solution, extracting for 2-3 times by flash extraction equipment, filtering, and mixing filtrates to obtain extract II; mixing the first extractive solution and the second extractive solution, concentrating under reduced pressure, eluting with deionized water and ethanol solution for 2-4 times respectively, concentrating the eluate under reduced pressure, and drying, pulverizing and sterilizing to obtain Cistanchis herba extract. The invention also comprises the cistanche tubulosa extract prepared by the method. The preparation method disclosed by the invention is simple in process flow, can be used for rapidly extracting the effective components in the cistanche tubulosa, and effectively solves the problems of long extraction period, low content of the effective components, low extraction efficiency and the like in the prior art.
Description
Technical Field
The invention relates to the technical field of cistanche extraction, in particular to a cistanche tubulosa extract and a preparation method thereof.
Background
Cistanche tubulosa (Schenk) Wight, a scientific name, is a perennial parasitic herbaceous plant of Cistanche genus of Orobanchaceae, the plant height can reach 100 cm, the stem does not branch, the leaves are milky white, the leaves become brown after being dried, the shape of triangle, spike-shaped inflorescence, bract prolate needle-shaped cape or ovate cape-shaped, the edge is molified, and both sides have no hair; the small bract is in the shape of a needle or a spoon and has no hair. Calyx barrel shape, flower crown milky white, long egg shape triangle or wrapping needle shape, flower crown barrel shape funnel shape, the splinters are purple in flower bud, nearly circular, anther egg shape, ovary long egg shape, capsule long circular, most seeds, nearly circular, blooming in 5-6 months, and fruiting in 7-8 months. The water is more abundant in the monster willow cluster and sand dune land which grow at the elevation of 1200 m; are often parasitic on the roots of tamarix plants.
The chemical components of cistanche deserticola are very complex, mainly comprise phenylethanoid glycosides, iridoid and glycosides thereof, lignan glycosides, polysaccharides, oligosaccharides, betaine and the like, and the active ingredients for improving sexual function, learning and memory ability, resisting aging and fatigue, treating senile dementia, Parkinson's disease and myocardial ischemia, protecting liver and the like are the phenylethanoid glycosides; the effective components for improving immunity comprise phenylethanoid glycosides and polysaccharides; the effective component for relaxing bowels is galactitol or total oligosaccharide. However, the existing cistanche tubulosa extraction method is complex in process, inconvenient to operate and high in extraction cost, particularly reflects the problems of long extraction period, low efficiency, low content of effective components in the extract and the like, and only can obtain the active components with low content, so that the cistanche tubulosa is not effectively and fully utilized, the resource waste condition is very serious, and the existing extraction requirements are difficult to meet.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the cistanche tubulosa extract and the preparation method thereof, the preparation method has simple process flow, can quickly extract the effective components in the cistanche tubulosa, and effectively solves the problems of longer extraction period, lower content of the effective components, low extraction efficiency and the like in the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the cistanche tubulosa extract comprises the following steps:
(1) mixing pretreated cistanche tubulosa with deionized water, performing multi-stage countercurrent ultrasonic extraction, filtering, and mixing filtrates to obtain filter residue and an extract I;
(2) mixing the filter residue obtained in the step (1) with 60-80 vt% ethanol solution, extracting for 2-3 times (30-90 s each time) by flash extraction equipment, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure until the relative density is 1.1-1.3, eluting for 2-4 times by respectively passing through 2-4 times of volume of deionized water and 2-5 times of volume of ethanol solution by using a macroporous adsorption resin column, concentrating the eluent under reduced pressure until the relative density is 1.1-1.2, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Further, in the step (1), the pretreatment specifically comprises the following steps: washing cistanche tubulosa with deionized water for 2-4 times, drying at 40-60 deg.C, pulverizing, and sieving with 70-80 mesh sieve to obtain pretreated cistanche tubulosa.
Further, in the step (1), during the ultrasonic countercurrent extraction, the ultrasonic power is 50-90KHz, and the extraction time is 0.4-2h each time.
Further, in the step (1), at least two stages of countercurrent ultrasonic extraction are carried out, and the power of the next stage of countercurrent ultrasonic extraction is 5-10KHz more than that of the previous stage.
Further, in the step (1), when the cistanche tubulosa is mixed with the deionized water, the material-liquid ratio is 1: 5-10.
Further, in the step (2), when the filter residue is mixed with the ethanol solution, the material-liquid ratio is 1: 10-20.
Further, in the step (2), the rotation speed of the flash extraction equipment is 3000-.
Further, in the step (3), the mixture is concentrated under reduced pressure at 40-60 ℃ and under the vacuum degree of 0.7-1 MPa.
Further, in the step (3), instantaneous sterilization is carried out at a temperature of 130 ℃ and 140 ℃.
The cistanche tubulosa extract is prepared by the preparation method of the cistanche tubulosa extract.
Furthermore, the content of echinacoside in the cistanche tubulosa extract is more than or equal to 40%, the content of verbascoside is more than or equal to 16%, and the content of phenylethanol total glycosides is more than or equal to 85%.
In summary, the invention has the following advantages:
1. the preparation method disclosed by the invention is simple in process flow and simple and convenient to operate, can quickly extract a large amount of effective components in cistanche tubulosa so as to effectively and fully utilize the cistanche tubulosa, reduce resource waste, and effectively solve the problems of long extraction period, low content of effective components, low extraction efficiency and the like in the prior art because the obtained extract contains a large amount of echinacoside, verbascoside, phenylethanol total glycoside and the like, and is convenient to popularize and use.
2. When in extraction, the cistanche tubulosa is firstly pretreated by cleaning, drying, crushing and the like, and the aim is to remove impurities on the surface of the cistanche tubulosa and crush the cistanche tubulosa for later use. Then mixing the extract with deionized water, and then carrying out multistage countercurrent ultrasonic extraction, and carrying out at least three stages of countercurrent ultrasonic extraction, wherein the next stage of countercurrent ultrasonic extraction is carried out by using the filter residue after the last stage of extraction, and the power of the next stage of countercurrent ultrasonic extraction is 10KHz more than that of the last stage, so that the water-soluble components in the cistanche tubulosa are fully extracted, the content of the water-soluble effective components in the extract is improved, and the waste is avoided; compared with other extraction modes, the countercurrent ultrasonic extraction has the advantages that the extraction speed is higher, the extraction time can be greatly shortened, the extraction rate of effective components can be improved, the efficiency is higher, the outflow of ineffective components can be reduced, the obtained extract has fewer impurities, the required temperature for the countercurrent ultrasonic extraction is not high, even extra heating is not needed, thermosensitive substances in the extract can be protected from being damaged, the efficient countercurrent extraction and the ultrasonic extraction are superposed and enhanced, the strong cavitation effect of the ultrasound is utilized, and a plurality of small cavities are formed in the cistanche, so that the pressure of thousands of atmospheric pressure is generated by the instant closure of the small cavities, the wall breaking of plant cell tissues can be promoted, the dissolution and diffusion of the effective components of the medicine are accelerated, and the extraction rate of the effective components is remarkably improved.
3. And then adding ethanol into the filter residue obtained after the countercurrent ultrasonic extraction for flash extraction for multiple times to extract the alcohol-soluble components of the filter residue, so that the effective components of the plant can be retained to the maximum extent, the thermosensitive components can not be damaged by heat, the extraction time is very short, the efficiency is high, the solvent consumption is small, the ethanol is adopted for flash extraction for multiple times, the alcohol-soluble components can be extracted as far as possible, and the content of the effective components in the obtained extract is improved. And finally, combining the first extract and the second extract, respectively eluting for multiple times through deionized water and ethanol by adopting a macroporous adsorption resin column, adsorbing organic substances in the extracts, separating and purifying the extracts, improving the purity of effective substances in the cistanche tubulosa extracts, and keeping effective components in the extracts.
4. According to the invention, in the extraction process, the countercurrent ultrasonic extraction of deionized water and the flash extraction of ethanol solution are successively adopted for multiple times, so that the effective components in the extract can be extracted as much as possible, the content of the effective components is increased, the purity of the substance is improved, and the waste of the effective components is avoided; the time required by each step of the whole extraction process is short, the extraction period of the cistanche tubulosa is obviously shortened, and the extraction efficiency is also improved; the obtained total glycosides of echinacoside, verbascoside and phenethyl alcohol in Cistanchis herba respectively reach 40%, 16% and 85%; meanwhile, the active substances are completely extracted, the cistanche tubulosa extract has higher purity, and the residual inactive substances are less.
Detailed Description
Example 1
A cistanche tubulosa extract is prepared by the following steps:
(1) washing cistanche tubulosa with deionized water for 2 times, drying at 40 deg.C, pulverizing, and sieving with 70 mesh sieve to obtain pretreated cistanche tubulosa; mixing pretreated cistanche tubulosa with deionized water according to a material-liquid ratio of 1:5, performing multi-stage countercurrent ultrasonic extraction, filtering, and combining filtrates to obtain filter residue and an extract I; performing two-stage countercurrent ultrasonic extraction, wherein the power of the first-stage countercurrent ultrasonic extraction is 52KHz, and the power of the second-stage countercurrent ultrasonic extraction is 62 KHz; the extraction time is 0.5h each time;
(2) mixing the filter residue obtained in the step (1) with 60 vt% ethanol solution according to a material-liquid ratio of 1:10, extracting for 2 times by flash extraction equipment, each time for 30-90s, at a rotating speed of 3000r/min, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure at 40 ℃ under the vacuum degree of 0.7MPa until the relative density is 1.1, eluting for 2 times by using a macroporous adsorption resin column through 2 times of volume of deionized water and 2 times of volume of ethanol solution respectively, concentrating the eluent under reduced pressure at 40 ℃ under the vacuum degree of 0.7MPa until the relative density is 1.1, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Example 2
A cistanche tubulosa extract is prepared by the following steps:
(1) washing cistanche tubulosa with deionized water for 3 times, drying at 50 ℃, crushing and sieving with a 70-mesh sieve to obtain pretreated cistanche tubulosa; mixing pretreated cistanche tubulosa with deionized water according to a material-liquid ratio of 1:6, performing multi-stage countercurrent ultrasonic extraction, filtering, and combining filtrates to obtain filter residue and an extract I; performing three-stage countercurrent ultrasonic extraction, wherein the power of the first-stage countercurrent ultrasonic extraction is 60KHz, the power of the second-stage countercurrent ultrasonic extraction is 70KHz, and the power of the third-stage countercurrent ultrasonic extraction is 80 KHz; the extraction time is 1h each time;
(2) mixing the filter residue obtained in the step (1) with 70 vt% ethanol solution according to a material-liquid ratio of 1:13, extracting for 2 times by flash extraction equipment, 40s each time, at a rotating speed of 4000r/min, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure at 45 ℃ under the vacuum degree of 0.8MPa until the relative density is 1.2, eluting for 3 times by using a macroporous adsorption resin column through 3 times of volume of deionized water and 3 times of volume of ethanol solution respectively, concentrating the eluent under reduced pressure at 45 ℃ under the vacuum degree of 0.8MPa until the relative density is 1.1, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Example 3
A cistanche tubulosa extract is prepared by the following steps:
(1) washing cistanche tubulosa with deionized water for 3 times, drying at 50 deg.C, pulverizing, and sieving with 70-mesh sieve to obtain pretreated cistanche tubulosa; mixing pretreated cistanche tubulosa with deionized water according to a material-liquid ratio of 1:8, performing multi-stage countercurrent ultrasonic extraction, filtering, and combining filtrates to obtain filter residue and an extract I; carrying out three-stage countercurrent ultrasonic extraction, wherein the power of the first-stage countercurrent ultrasonic extraction is 65KHz, the power of the second-stage countercurrent ultrasonic extraction is 73KHz, and the power of the third-stage countercurrent ultrasonic extraction is 81 KHz; the extraction time is 1.5h each time;
(2) mixing the filter residue obtained in the step (1) with 75 vt% ethanol solution according to a material-liquid ratio of 1:15, extracting for 3 times by flash extraction equipment, 60s each time, at a rotation speed of 5000r/min, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure at 50 ℃ and under the vacuum degree of 0.9MPa until the relative density is 1.3, eluting for 3 times by using a macroporous adsorption resin column through 3 times of volume of deionized water and 3 times of volume of ethanol solution respectively, concentrating the eluent under reduced pressure at 50 ℃ and under the vacuum degree of 0.9MPa until the relative density is 1.2, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Example 4
A cistanche tubulosa extract is prepared by the following steps:
(1) washing cistanche tubulosa with deionized water for 4 times, drying at 60 ℃, crushing and sieving with a 80-mesh sieve to obtain pretreated cistanche tubulosa; mixing pretreated cistanche tubulosa with deionized water according to a material-liquid ratio of 1:10, performing multi-stage countercurrent ultrasonic extraction, filtering, and combining filtrates to obtain filter residue and an extract I; performing three-stage countercurrent ultrasonic extraction with a first-stage countercurrent ultrasonic extraction power of 70KHz, a second-stage countercurrent ultrasonic extraction power of 80KHz, and a third-stage countercurrent ultrasonic extraction power of 90 KH; the extraction time is 2h each time;
(2) mixing the filter residue obtained in the step (1) with 75 vt% ethanol solution according to a material-liquid ratio of 1:20, extracting for 3 times by flash extraction equipment, each time for 70s, at a rotating speed of 4500r/min, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure at 60 ℃ under 1MPa of vacuum degree until the relative density is 1.3, eluting for 2-4 times by using a macroporous adsorption resin column through 4 times of volume of deionized water and 4 times of volume of ethanol solution respectively, concentrating the eluent under reduced pressure at 60 ℃ under 1MPa of vacuum degree until the relative density is 1.2, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Comparative example 1
A cistanche tubulosa extract is prepared by the following steps:
(1) washing cistanche tubulosa with deionized water for 3 times, drying at 50 ℃, crushing and sieving with a 70-mesh sieve to obtain pretreated cistanche tubulosa; mixing pretreated cistanche tubulosa with deionized water according to a material-liquid ratio of 1:6, performing ultrasonic extraction for 3 times, filtering, and mixing filtrates to obtain filter residue and an extract I; ultrasonic extraction power is 80 KHz; the extraction time is 1h each time;
(2) mixing the filter residue obtained in the step (1) with 70 vt% ethanol solution according to a material-liquid ratio of 1:13, extracting for 2 times by flash extraction equipment, 40s each time, at a rotating speed of 4000r/min, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure at 45 ℃ under the vacuum degree of 0.8MPa until the relative density is 1.2, eluting for 3 times by using a macroporous adsorption resin column through 3 times of volume of deionized water and 3 times of volume of ethanol solution respectively, concentrating the eluent under reduced pressure at 45 ℃ under the vacuum degree of 0.8MPa until the relative density is 1.1, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Comparative example 2
A cistanche tubulosa extract is prepared by the following steps:
(1) washing cistanche tubulosa with deionized water for 3 times, drying at 50 ℃, crushing and sieving with a 70-mesh sieve to obtain pretreated cistanche tubulosa; mixing pretreated cistanche tubulosa with deionized water according to a material-liquid ratio of 1:6, performing multi-stage countercurrent ultrasonic extraction, filtering, and combining filtrates to obtain filter residue and an extract I; performing three-stage countercurrent ultrasonic extraction, wherein the power of the first-stage countercurrent ultrasonic extraction is 60KHz, the power of the second-stage countercurrent ultrasonic extraction is 70KHz, and the power of the third-stage countercurrent ultrasonic extraction is 80 KHz; the extraction time is 1h each time;
(2) mixing the filter residue obtained in the step (1) with 70 vt% ethanol solution according to a material-liquid ratio of 1:13, heating to 50 ℃, extracting for 2 times, 40s each time, at a rotating speed of 4000r/min, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure at 45 ℃ under the vacuum degree of 0.8MPa until the relative density is 1.2, eluting for 3 times by using a macroporous adsorption resin column through 3 times of volume of deionized water and 3 times of volume of ethanol solution respectively, concentrating the eluent under reduced pressure at 45 ℃ under the vacuum degree of 0.8MPa until the relative density is 1.1, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Comparative example 3
A cistanche tubulosa extract is prepared by the following steps:
(1) washing cistanche tubulosa with deionized water for 3 times, drying at 50 ℃, crushing and sieving with a 70-mesh sieve to obtain pretreated cistanche tubulosa; mixing pretreated cistanche tubulosa with deionized water according to a material-liquid ratio of 1:6, performing multi-stage countercurrent ultrasonic extraction, filtering, and combining filtrates to obtain filter residue and an extract I; performing three-stage countercurrent ultrasonic extraction, wherein the power of the first-stage countercurrent ultrasonic extraction is 60KHz, the power of the second-stage countercurrent ultrasonic extraction is 70KHz, and the power of the third-stage countercurrent ultrasonic extraction is 80 KHz; the extraction time is 1h each time;
(2) mixing the filter residue obtained in the step (1) with 70 vt% ethanol solution according to a material-liquid ratio of 1:13, extracting for 2 times by flash extraction equipment, 40s each time, at a rotating speed of 4000r/min, filtering, and combining the filtrates to obtain an extract II;
(3) and (3) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure at 45 ℃ and under the vacuum degree of 0.8MPa until the relative density is 1.2, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
Examples of the experiments
The components of cistanche tubulosa extract were detected by the following method.
1. HLC determination of echinacoside and verbascoside
1.1 instruments and appliances: high performance liquid chromatograph, volumetric flask 100m1, analytical balance, pipette, ultrasonic instrument.
1.2 reagent and test solution: 50% methanol and pure methanol, wherein the pure methanol is used as a mobile phase A, the 0.1% formic acid solution is used as a mobile phase B, and the echinacoside standard substance and the verbascoside standard substance are adopted.
1.3 chromatographic conditions and System suitability test:
octadecylsilane chemically bonded silica is used as a filling agent; pure alcohol was used as mobile phase A, and 0.1% formic acid solution was used as mobile phase B (34.5:65.5), and the detection wavelength was 330 mm. The number of theoretical plates is not less than 3000 calculated according to echinacoside peak.
1.4 preparation of Standard solutions
Taking appropriate amount of echinacoside standard product and acteoside standard product, precisely weighing, respectively placing into brown bottle, adding 50% methanol to obtain solutions containing 0.2mg and 0.2mg per 1m 1.
1.5 preparation of test solutions
Taking about 0.05g of cistanche tubulosa extract (screened by a sieve with the number four), precisely weighing, placing in a 100ml brown volumetric flask, precisely adding a proper amount of 50% methanol, carrying out ultrasonic treatment for 10 minutes (power 250W, frequency 35kHz), dissolving, adding 50% methanol for diluting to a scale, and shaking up to obtain the cistanche tubulosa extract.
1.6 assay method
Precisely sucking the standard solution and the sample solution respectively by 10 μ 1, injecting into liquid chromatograph, and measuring.
1.7 recording the concentration of the standard substance, the area S of the main peak of the standard solution, the area S of the main peak of the test solution, the sample weighing amount and the calculation and the result of the content.
2. UV determination of Total glycosides of phenethyl alcohol
2.1 preparation of Standard solutions
Precisely weighing 10mg of echinacoside standard substance, placing into a 50ml brown volumetric flask, adding 50% methanol for dissolving, and diluting to scale.
2.2 Standard Curve preparation
Precisely measuring standard solutions 0.2ml, 0.4ml, 0.6ml, 0.8ml and 1.0ml, respectively placing in 10ml volumetric flasks, diluting with 50% methanol to scale, and shaking. The absorbance was measured at a wavelength of 30mm by an ultraviolet-visible spectrophotometry (appendix VA of 2015 edition of Chinese pharmacopoeia) with the corresponding reagent as a blank, and a standard curve was drawn with the absorbance as the ordinate and the concentration as the abscissa.
2.3 preparation and measurement of test solutions
Precisely weighing 30mg of test powder in a 50ml volumetric flask, adding a proper amount of 50% methanol for ultrasonic dissolution, standing to room temperature, adding 50% methanol to scale, and shaking up. Precisely measuring the solution with the concentration of 1.0m1, placing the solution into a 25ml volumetric flask, diluting the solution to a scale with 50% methanol, measuring the absorbance according to the method under the preparation item of a standard curve from the point that corresponding reagents are used as blanks, reading the amount of the phenethyl alcohol total glycosides in the test solution from the standard curve, and calculating to obtain the phenethyl alcohol total glycosides.
The results of the tests of examples 1 to 4 and comparative examples 1 to 3 are shown in Table 1.
3. Yield of cistanche tubulosa extract
The yield calculation formula is as follows:
the yield is equal to the mass of the cistanche tubulosa extract/the mass of the cistanche tubulosa is multiplied by 100 percent
The yields of examples 1 to 4 and comparative examples 1 to 3 were calculated according to the above formulas, respectively, and the results are shown in Table 1.
TABLE 1 examination results of examples 1 to 4 and comparative examples 1 to 3
As can be seen from Table 1, the cistanche tubulosa extract obtained by the method has complete extraction of effective substances, wherein the contents of echinacoside, verbascoside and phenethyl alcohol total glycoside respectively reach more than 40%, 16% and 85%, and the residual substances are less; meanwhile, the extraction rate of the cistanche tubulosa obtained by the method is high, and the method has positive significance for effective utilization and popularization and use of the cistanche tubulosa. The method is characterized in that deionized water countercurrent ultrasonic extraction and ethanol solution flash extraction are sequentially adopted for multiple times in the extraction process, so that the effective components in the extract can be extracted as much as possible, the content of the effective components is increased, the purity of the substance is improved, and the waste of the effective components is avoided; and the time required by each step of the whole extraction process is shorter, the extraction period of the cistanche tubulosa is obviously shortened, and the extraction efficiency is also improved.
While the present invention has been described in detail with reference to the specific embodiments thereof, it should not be construed as limited by the scope of the present patent. Various modifications and changes may be made by those skilled in the art without inventive step within the scope of the appended claims.
Claims (10)
1. A preparation method of cistanche tubulosa extract is characterized by comprising the following steps:
(1) mixing pretreated cistanche tubulosa with deionized water, performing multi-stage countercurrent ultrasonic extraction, filtering, and mixing filtrates to obtain filter residue and an extract I;
(2) mixing the filter residue obtained in the step (1) with 60-80 vt% ethanol solution, extracting for 2-3 times (30-90 s each time) by flash extraction equipment, filtering, and combining the filtrates to obtain an extract II;
(3) and (2) combining the first extract obtained in the step (1) and the second extract obtained in the step (2), concentrating under reduced pressure until the relative density is 1.1-1.3, eluting for 2-4 times by respectively passing through 2-4 times of volume of deionized water and 2-5 times of volume of ethanol solution by using a macroporous adsorption resin column, concentrating the eluent under reduced pressure until the relative density is 1.1-1.2, and finally drying, crushing and sterilizing in sequence to obtain the cistanche tubulosa extract.
2. The method for preparing cistanche tubulosa extract according to claim 1, wherein in the step (1), the pre-treatment comprises the following specific steps: washing cistanche tubulosa with deionized water for 2-4 times, drying at 40-60 deg.C, pulverizing, and sieving with 70-80 mesh sieve to obtain pretreated cistanche tubulosa.
3. The method for preparing cistanche tubulosa extract as set forth in claim 1, wherein in the step (1), the ultrasonic power is 50-90KHz and the extraction time is 0.4-2h each time during the ultrasonic countercurrent extraction.
4. The method for preparing cistanche tubulosa extract as set forth in claim 3, wherein in step (1), at least two stages of countercurrent ultrasonic extraction are performed, and the power of countercurrent ultrasonic extraction in the next stage is 5-10KHz more than that in the previous stage.
5. The method for preparing cistanche tubulosa extract according to claim 1, wherein in the step (1), when cistanche tubulosa is mixed with deionized water, the ratio of material to liquid is 1: 5-10.
6. The method for preparing cistanche tubulosa extract as claimed in claim 1, wherein in the step (2), when the residue is mixed with the ethanol solution, the ratio of the material to the liquid is 1: 10-20.
7. The method for preparing cistanche tubulosa extract as claimed in claim 1, wherein in step (2), the rotation speed of the flash extraction equipment is 3000-6000 r/min.
8. The method of preparing cistanche tubulosa extract according to claim 1, wherein in the step (3), the concentration is performed under reduced pressure at 40-60 ℃ under a vacuum degree of 0.7-1 MPa.
9. The method for preparing cistanche tubulosa extract as set forth in claim 1, wherein in the step (3), the instant sterilization is performed at a temperature of 130-140 ℃.
10. The cistanche tubulosa extract obtained by the method for preparing a cistanche tubulosa extract according to any one of claims 1 to 9.
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| CN114515008A (en) * | 2022-03-04 | 2022-05-20 | 广东青云山药业有限公司 | Cistanche tubulosa extract and preparation method thereof |
| CN115227741A (en) * | 2022-06-09 | 2022-10-25 | 新疆汇峰农业科技有限公司 | Cistanche deserticola extract purification method and equipment |
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| CN114515008A (en) * | 2022-03-04 | 2022-05-20 | 广东青云山药业有限公司 | Cistanche tubulosa extract and preparation method thereof |
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