CN113018333A - Extraction method of cistanche tubulosa - Google Patents
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Abstract
The invention discloses a method for extracting cistanche tubulosa, which comprises the following steps: taking fresh cistanche, sequentially carrying out enzyme deactivation, cutting into blocks, drying and coarse crushing treatment to obtain powder; sequentially carrying out ultrasonic extraction on cistanche deserticola powder in a petroleum ether/30-60% ethanol mixed solution, a 60-95% ethanol solution and water, filtering after each extraction, standing and cooling, separating and removing petroleum ether, ether and precipitates, collecting and combining a 30-60% ethanol extracting solution, a 60-95% ethanol extracting solution and a water extracting solution, and then concentrating to remove ethanol to obtain a cistanche deserticola extracting solution; concentrating and drying the cistanche extracting solution, and crushing to obtain the cistanche extract. The extraction method can effectively solve the problems of large solvent consumption, low extraction rate and low purity of effective components in the existing extraction method.
Description
Technical Field
The invention relates to the technical field of active ingredient extraction, in particular to a method for extracting active ingredients from cistanche tubulosa.
Background
Cistanche tubulosa is a parasitic plant of the family Orobanchaceae, commonly called tamarix rupestris, parasitic on the roots of tamarix plants, and mainly distributed in the northern regions of Xinjiang and around Takrama desert in the southern regions of Xinjiang in China. Meanwhile, cistanche tubulosa is a precious nourishing Chinese herbal medicine, is known as 'desert ginseng', and has the functions of nourishing kidney, resisting aging, enhancing blood essence, moistening large intestine and smoothing stool. Studies show that phenylethanoid glycosides, iridoids and polysaccharides are the main chemical components of cistanche tubulosa. Phenylethanoid glycosides are the main active ingredients of cistanche tubulosa, and have neuroprotective, immunoregulatory, antiinflammatory, hepatoprotective, and antioxidant effects. Phenylethanoid glycosides are a group of water-soluble natural products, are a common structure consisting of cinnamic acid and hydroxyphenyl ethyl, are connected with beta-glucopyranose through ester and glycosidic bonds, and mainly comprise echinacoside and verbascoside.
The existing cistanche extraction method mainly comprises the following steps: solvent extraction, microwave-assisted extraction, ultrasonic extraction, high shear-assisted extraction, and the like. Among them, the solvent extraction method has the disadvantages of large solvent dosage, long time consumption and the like. The microwave extraction method has the advantages of simple equipment, short operation time, less solvent consumption, lower extraction rate, difficult automation and lack of possibility of online connection with other instruments. The ultrasonic extraction method has simple operation, simple equipment and high extraction rate, but has long working time, large solvent consumption and difficult automation.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides the extraction method of cistanche tubulosa, which can effectively solve the problems of large solvent consumption, low extraction rate and low purity of phenylethanoid glycosides in the existing extraction method.
In order to achieve the purpose, the technical scheme adopted by the invention for solving the technical problems is as follows:
a method for extracting cistanche tubulosa comprises the following steps:
(1) taking fresh cistanche, sequentially carrying out enzyme deactivation, cutting into blocks, drying and coarse crushing treatment to obtain powder;
(2) sequentially carrying out ultrasonic extraction on cistanche deserticola powder in a petroleum ether/30-60% ethanol mixed solution, a 60-95% ethanol solution and water, filtering after each extraction, standing and cooling, separating and removing petroleum ether, ether and precipitates, collecting and combining a 30-60% ethanol extracting solution, a 60-95% ethanol extracting solution and a water extracting solution, and then concentrating to remove ethanol to obtain a cistanche deserticola extracting solution;
(3) concentrating and drying the cistanche extracting solution, and crushing to obtain the cistanche extract.
According to the scheme, fresh cistanche is subjected to enzyme deactivation treatment, so that enzymatic reaction in the subsequent treatment process is reduced, and the content of effective components in the cistanche is improved; then cutting the cistanche deserticola into pieces and drying the cistanche deserticola, coarsely drying and crushing the cistanche deserticola, sieving the cistanche deserticola by a 40-mesh sieve, extracting the obtained cistanche deserticola powder in a petroleum ether/diethyl ether/30-60% ethanol mixed solution, and stirring the cistanche deserticola powder while extracting, wherein the petroleum ether and the diethyl ether have smaller polarities and different polarities and have a certain span, and both the petroleum ether and the diethyl ether are organic solvents;
the method comprises the steps of firstly extracting by using a low-concentration ethanol solution and then extracting by using a high-concentration ethanol solution, extracting by using ethanol with different volume concentrations due to different polarities and different penetrating power in cells, fully extracting effective components in the cistanche deserticola, and finally extracting by using water, wherein the phenylethanoid glycoside is easy to dissolve in a solvent with large polarity due to the maximum polarity of the water, so that the effective components can be further extracted.
In the invention, different solvents are used for extraction by utilizing the different solubilities of the effective components and the impurity components in different solvents in the extraction process, the impurity components are separated in the extraction process, and the separation of the effective components of the phenylethanoid glycoside is improved.
Further, the enzyme deactivation operation in the step (1) is as follows: decocting fresh Cistanchis herba at 70-80 deg.C for 20-40 min.
Further, the drying temperature in the step (1) is 50-80 ℃.
Further, the drying temperature in step (1) was 80 ℃.
In the above scheme, too high drying temperature can lead to degradation and damage of effective components, reduce extraction rate, and too low drying temperature can lead to prolonged drying time, and is not favorable for energy conservation.
Further, in the step (2), the ultrasonic treatment times of the cistanche powder in each solvent are 2-3 times, each ultrasonic treatment time is 5-10min, and each ultrasonic treatment interval is 15-30 min.
Further, in the step (2), the ultrasonic treatment times of the cistanche powder in each solvent are 2 times, each ultrasonic treatment time is 10min, and each ultrasonic treatment interval is 20 min.
Further, the ultrasonic power in the step (2) is 150- & lt 250 & gt W.
Further, the ultrasonic power in the step (2) is 200W.
In the scheme, the cavitation of ultrasonic waves is utilized to destroy cells, the dissolution of effective components is accelerated, the solubility of the dissolved components in different solvents can be increased in the ultrasonic treatment process, and the separation effect of impurities and the effective components is improved.
Further, the extraction temperature in the step (2) is 60-80 ℃.
Further, the extraction temperature in step (2) was 80 ℃.
In the scheme, the extraction temperature is not too high, otherwise, the active ingredients are easy to damage, the extraction rate is reduced, the solubility of different ingredients in different solvents can be increased by extracting at a certain temperature, the separation effect of the active ingredients and impurities is further improved, and the extraction rate of the active ingredients is improved.
Further, the mass ratio of the cistanche powder to the petroleum ether/diethyl ether/30-60% ethanol mixed solution, the mass ratio of the 60-95% ethanol solution to the water in the step (2) are respectively 1:15-25, 1:10-20 and 1: 10-20.
Further, the mass ratio of the cistanche powder to the petroleum ether/diethyl ether/30-60% ethanol mixed solution, the mass ratio of the 60-95% ethanol solution to the water in the step (2) are respectively 1:15, 1:10 and 1: 10.
In the scheme, the cistanche powder is respectively mixed with different solvents according to a certain proportion, so that the dissolution of effective components is promoted, and the extraction rate is improved.
Further, the volume ratio of the petroleum ether, the ethyl ether and the 30-60% ethanol in the petroleum ether/ethyl ether/30-60% ethanol mixed solution in the step (2) is 1-2:1-2: 3-5.
Further, the volume ratio of the petroleum ether, the ethyl ether and the 30-60% ethanol in the petroleum ether/ethyl ether/30-60% ethanol mixed solution in the step (2) is 1:1: 4.
In the scheme, the cistanche also contains a large amount of iridoid substances and other impurities, and the impurities can be dissolved and adsorbed by using petroleum ether and diethyl ether as solvents, so that the dissolving amount of the impurities in an ethanol solution is reduced, and the extraction purity is further improved.
Further, the pH values of the petroleum ether/diethyl ether/30-60% ethanol mixed solution, the 60-95% ethanol solution and the water in the step (2) are 4-6.
Further, the pH values of the petroleum ether/diethyl ether/30-60% ethanol mixed solution, the 60-95% ethanol solution and the water in the step (2) are all 5.
In the scheme, extraction is carried out under a weak acidic condition, the structures of impurity components such as iridoid in the cistanche can be destroyed under the weak acidic condition, and the content of effective components is further improved.
Further, in the step (2), the cistanche powder is sequentially subjected to ultrasonic extraction in a petroleum ether/50% ethanol mixed solution, a 75% ethanol solution and water, filtering is performed after each extraction, standing and cooling are performed, petroleum ether, ether and precipitates are separated and removed, 50% ethanol extract, 75% ethanol extract and water extract are collected and combined, and then the ethanol is removed through concentration, so that the cistanche extract is obtained.
In the scheme, 50% and 75% volume concentration ethanol is adopted for extraction respectively, and the active ingredients of the cistanche are fully extracted by utilizing the characteristic that the ethanol with different concentrations has different polarities, so that the extraction rate of the active ingredients is improved.
The beneficial effects produced by the invention are as follows:
1. according to the invention, the cistanche is firstly extracted under a weak acidic condition, a precipitate is generated after the structure of part of impurity components is changed under the weak acidic condition, the impurity content in an extraction solvent can be preliminarily reduced, then a petroleum ether/diethyl ether/30-60% ethanol mixed solution, a 60-95% ethanol solution and water are respectively adopted for extraction, the petroleum ether and the diethyl ether can be further used for dissolving and absorbing the impurity components in the cistanche, the impurity content in an ethanol extracting solution and a water extracting solution is reduced, the solubility of effective components in the ethanol extracting solution and the water extracting solution is improved, and the usage amount of the ethanol extracting solution and the water extracting solution is further reduced.
2. In the invention, impurity components are decomposed or adsorbed in different modes in the extraction process, so that the content of impurities in the extract can be fully reduced, and the purity and the extraction rate of the active components of the phenylethanoid glycosides are improved.
Detailed Description
Example 1
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 70 deg.C for 20min to inactivate enzyme, cutting into small pieces of 1 × 1cm, drying at 60 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) sequentially carrying out ultrasonic extraction on cistanche powder in a petroleum ether/30% ethanol mixed solution, a 60% ethanol solution and water at 60 ℃ and pH value of 4, wherein the ultrasonic power is 150W, the ultrasonic treatment frequency in each solvent is 2 times, the ultrasonic time is 5min each time, the ultrasonic interval is 15min each time, filtering after extraction in each solvent, standing and cooling, separating and removing petroleum ether, ether and precipitates, collecting and combining a 30% ethanol extract, a 60% ethanol extract and a water extract, and then concentrating and removing ethanol to obtain a cistanche extract; wherein, in the extraction process, the mass ratio of the cistanche powder to the petroleum ether/30% ethanol mixed solution, the mass ratio of the 60% ethanol solution to the mass ratio of the water are respectively 1:15, 1:10 and 1: 10; the volume ratio of the petroleum ether to the diethyl ether to the 30% ethanol in the petroleum ether/diethyl ether/30% ethanol mixed solution is 1:1: 3;
(3) concentrating and drying the cistanche extracting solution at 60 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Example 2
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 75 deg.C for 40min, inactivating enzyme, cutting into 2 × 2cm pieces, drying at 70 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) sequentially carrying out ultrasonic extraction on cistanche powder in a petroleum ether/60% ethanol mixed solution, a 95% ethanol solution and water at the temperature of 80 ℃ and the pH value of 6, wherein the ultrasonic power is 250W, the ultrasonic treatment frequency in each solvent is 3 times, the ultrasonic time is 10min each time, the ultrasonic interval is 30min each time, filtering after extraction in each solvent, standing and cooling, separating and removing petroleum ether, ether and precipitates, collecting and combining a 60% ethanol extract, a 95% ethanol extract and a water extract, and then concentrating and removing ethanol to obtain a cistanche extract; wherein, in the extraction process, the mass ratio of the cistanche powder to the petroleum ether/diethyl ether/60% ethanol mixed solution, the mass ratio of the 95% ethanol solution to the mass ratio of the water are respectively 1:25, 1:20 and 1: 20; the volume ratio of the petroleum ether to the diethyl ether to the 60% ethanol in the petroleum ether/diethyl ether/60% ethanol mixed solution is 2:1: 4;
(3) concentrating and drying the cistanche extracting solution at 80 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Example 3
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 75 deg.C for 30min to inactivate enzyme, cutting into small pieces of 2 × 2cm, drying at 80 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) sequentially carrying out ultrasonic extraction on cistanche deserticola powder in a petroleum ether/diethyl ether/50% ethanol mixed solution, a 75% ethanol solution and water at the temperature of 80 ℃ and the pH value of 5, wherein the ultrasonic power is 200W, the ultrasonic treatment frequency in each solvent is 2 times, the ultrasonic time is 10min each time, the ultrasonic interval is 20min each time, filtering after extraction in each solvent, standing and cooling, separating and removing petroleum ether, diethyl ether and precipitates, collecting and combining a 50% ethanol extract, a 75% ethanol extract and a water extract, and then concentrating and removing ethanol to obtain a cistanche deserticola extract; wherein, in the extraction process, the mass ratio of the cistanche powder to the petroleum ether/diethyl ether/50% ethanol mixed solution, the mass ratio of the 75% ethanol solution to the mass ratio of the water are respectively 1:15, 1:10 and 1: 10; the volume ratio of the petroleum ether to the diethyl ether to the 50% ethanol in the petroleum ether/diethyl ether/50% ethanol mixed solution is 1:1: 4;
(3) concentrating and drying the cistanche extracting solution at 80 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Comparative example 1
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 75 deg.C for 30min to inactivate enzyme, cutting into small pieces of 2 × 2cm, drying at 80 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) ultrasonically extracting Cistanchis herba powder in 75% ethanol solution at 80 deg.C with ultrasonic power of 200W and ultrasonic treatment frequency of 2 times, each time ultrasonic treatment time of 10min, each time ultrasonic treatment interval of 20min, filtering, standing, cooling, separating to remove precipitate, collecting 75% ethanol extractive solution, and concentrating to remove ethanol to obtain Cistanchis herba extractive solution;
(3) concentrating and drying the cistanche extracting solution at 80 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Comparative example 2
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 75 deg.C for 30min to inactivate enzyme, cutting into small pieces of 2 × 2cm, drying at 80 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) sequentially carrying out ultrasonic extraction on cistanche powder in 50% ethanol solution, 75% ethanol solution and water at 80 ℃, wherein the ultrasonic power is 200W, the ultrasonic treatment frequency in each solvent is 2 times, the ultrasonic time is 10min each time, the ultrasonic interval is 20min each time, extracting in each solvent, filtering, standing, cooling, separating and removing precipitates, collecting and combining 50% ethanol extract, 75% ethanol extract and water extract, and then concentrating and removing ethanol to obtain cistanche extract;
(3) concentrating and drying the cistanche extracting solution at 80 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Comparative example 3
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 75 deg.C for 30min to inactivate enzyme, cutting into small pieces of 2 × 2cm, drying at 80 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) carrying out ultrasonic extraction on cistanche powder in water with the temperature of 80 ℃ and the pH value of 5, wherein the ultrasonic power is 200W, the ultrasonic treatment times are 2 times, the ultrasonic time is 10min each time, the ultrasonic interval is 20min each time, filtering is carried out after extraction, and standing and cooling are carried out to obtain cistanche extract;
(3) concentrating and drying the cistanche extracting solution at 80 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Comparative example 4
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 75 deg.C for 30min to inactivate enzyme, cutting into small pieces of 2 × 2cm, drying at 80 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) sequentially carrying out reflux extraction on cistanche deserticola powder in a petroleum ether/diethyl ether/40% ethanol mixed solution, a 90% ethanol solution and water at the temperature of 80 ℃ and the pH value of 5, filtering after extracting in each solvent, standing and cooling, separating and removing petroleum ether, diethyl ether and precipitates, collecting and combining a 40% ethanol extract, a 90% ethanol extract and a water extract, and then concentrating and removing ethanol to obtain a cistanche deserticola extract; wherein, in the extraction process, the mass ratio of the cistanche powder to the petroleum ether/diethyl ether/50% ethanol mixed solution, the mass ratio of the 75% ethanol solution to the mass ratio of the water are respectively 1:15, 1:10 and 1: 10; the volume ratio of the petroleum ether to the diethyl ether to the 50% ethanol in the petroleum ether/diethyl ether/50% ethanol mixed solution is 1:1: 4;
(3) concentrating and drying the cistanche extracting solution at 80 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Comparative example 5
A method for extracting cistanche tubulosa comprises the following steps:
(1) decocting fresh Cistanchis herba at 75 deg.C for 30min to inactivate enzyme, cutting into small pieces of 2 × 2cm, drying at 80 deg.C, coarse pulverizing, and sieving with 40 mesh sieve to obtain powder;
(2) sequentially carrying out ultrasonic extraction on cistanche deserticola powder in a petroleum ether/diethyl ether/50% ethanol mixed solution, a 75% ethanol solution and water at the temperature of 80 ℃ and the pH value of 5, wherein the ultrasonic power is 200W, the ultrasonic treatment frequency in each solvent is 2 times, the ultrasonic time is 10min each time, the ultrasonic interval is 20min each time, filtering after extraction in each solvent, standing and cooling, separating and removing petroleum ether, diethyl ether and precipitates, collecting and combining a 50% ethanol extract, a 75% ethanol extract and a water extract, and then concentrating and removing ethanol to obtain a cistanche deserticola extract; wherein, in the extraction process, the mass ratio of the cistanche powder to the petroleum ether/diethyl ether/50% ethanol mixed solution, the mass ratio of the 75% ethanol solution to the mass ratio of the water are respectively 1:10, 1:5 and 1: 5; the volume ratio of the petroleum ether to the diethyl ether to the 50% ethanol in the petroleum ether/diethyl ether/50% ethanol mixed solution is 3:3: 5;
(3) concentrating and drying the cistanche extracting solution at 80 ℃ until the water content is less than 15%, and crushing to obtain the cistanche extract.
Test examples
The collected powders of examples 1-3 and comparative examples 1-5 were weighed, respectively, to calculate the yield of the extract, and the contents of echinacoside, verbascoside and phenylethanol total glycosides in the extract were determined, respectively, as shown in tables 1-2.
Yield calculation formula: the yield is equal to the mass of the extract of the cistanche deserticola/the mass of the cistanche deserticola is multiplied by 100 percent
Table 1: statistics of yield
The obtained extracts are respectively detected by the following specific detection method:
1. HPLC determination of echinacoside and verbascoside
1.1 instruments and appliances: high performance liquid chromatograph, volumetric flask 100ml, analytical balance, pipette and ultrasonic instrument.
1.2 reagent and test solution: 50% methanol, pure methanol and pure methanol as mobile phase A, 0.1% formic acid solution as mobile phase B, echinacoside standard product, and acteoside standard product.
1.3 chromatographic conditions and System suitability test: octadecylsilane chemically bonded silica is used as a filling agent; pure methanol was used as mobile phase A, 0.1% formic acid solution was used as mobile phase B (34.5:65.5), and the detection wavelength was 330 nm. 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 deserticola extract (screened by a sieve of No. four), precisely weighing, placing in a 100ml brown volumetric flask, precisely adding a proper amount of 50 percent methanol, carrying out ultrasonic treatment for 10 minutes (power is 250W, frequency is 35kHz), dissolving, then adding 50 percent methanol to dilute to scale, and shaking up to obtain the cistanche deserticola 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, 0.6l, o.8ml and 1.0ml, respectively placing in 10ml volumetric flasks, diluting with 50% methanol to scale, and shaking uniformly to obtain the final product. 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.
Table 2: analysis of Cistanchis herba extract components
| Echinacoside | Acteoside | Phenethyl alcohol Total glycosides | Ash content | |
| Example 1 | ≥35％ | ≥14％ | ≥80％ | ≤5％ |
| Example 2 | ≥35％ | ≥14％ | ≥80％ | ≤5％ |
| Example 3 | ≥35％ | ≥14％ | ≥80％ | ≤5％ |
| Comparative example 1 | ≤35％ | ≤14％ | ≤80％ | ≤5％ |
| Comparative example 2 | ≤35％ | ≤14％ | ≤80％ | ≤5％ |
| Comparative example 3 | ≤35％ | ≤14％ | ≤80％ | ≤5％ |
| Comparative example 4 | ≤35％ | ≤14％ | ≤80％ | ≤5％ |
| Comparative example 5 | ≤35％ | ≤14％ | ≤80％ | ≤5％ |
As can be seen by combining Table 1 and Table 2, the yield of the extract in examples 1-3 is 3.5-3.8%, the content of echinacoside in the extract is more than or equal to 35%, the content of verbascoside is more than or equal to 14%, the content of phenylethanol total glycosides is more than or equal to 80%, and the ash content is less than or equal to 5%. The extraction yield of the comparative examples 1-3 is higher than that of the examples 1-3, but the contents of the active ingredients including echinacoside, verbascoside and phenylethanol total glycoside are all lower than those of the examples, and the extraction process in the examples is the extraction process in the comparative examples.
Comparing the comparative example 1 with the example 3, the extraction is carried out under the undefined weak acidic condition, the addition of the petroleum ether and the ether is cancelled, and the extraction is carried out only in 75 percent ethanol, and the impurity components in the cistanche deserticola are dissolved in the ethanol solvent due to the cancellation of the petroleum ether and the ether, so that the yield is improved; the yield is further increased by increasing impurity components without limiting the weakly acidic condition; but as the impurity components in the extract are not separated and removed, the content of the effective components in the extract is reduced, so that the product quality does not meet the standard requirement.
Comparing the comparative example 2 with the example 3, the extraction is not limited under the weak acidic condition, and petroleum ether and ether are eliminated, so that the impurity components in the cistanche deserticola are dissolved in the ethanol solvent, the extraction rate is improved, the weak acidic condition is not limited, the impurity components are increased, and the yield is further increased; but the impurity components in the extract are not separated and removed, so that the content of effective components in the extract is reduced, and the product quality does not meet the standard requirement; comparing comparative example 1 and comparative example 2, it can be seen that the ethanol and water with different concentrations adopted in comparative example 2 are respectively extracted, so that the components in cistanche can be fully extracted, and the yield of the extract is improved.
When comparative example 3 is compared with example 3, the extraction is performed only in water, and the water-soluble components in cistanche deserticola are dissolved in water, the yield is general, but the content of the effective components in the extract is reduced because of more impurities in water.
Comparing the comparative example 4 with the example 3, the reflux extraction is carried out in ethanol solutions with different concentrations, and because the ultrasonic extraction is cancelled, the cavitation disappears, the component dissolution is reduced, and the yield is reduced; the concentration of the ethanol is too high, so that the osmosis effect in the cistanche is influenced, and the dissolution amount of the effective components along with the solvent is further reduced, so that the ratio of the effective components in the extract is reduced.
Comparing the comparative example 5 with the example 3, the proportion relation of the cistanche powder and different extraction solvents is changed, so that the dissolution of the effective components in the cistanche is limited, and the yield is reduced.
Claims (10)
1. The extraction method of cistanche tubulosa is characterized by comprising the following steps:
(1) taking fresh cistanche, sequentially carrying out enzyme deactivation, cutting into blocks, drying and coarse crushing treatment to obtain powder;
(2) sequentially carrying out ultrasonic extraction on cistanche deserticola powder in a petroleum ether/30-60% ethanol mixed solution, a 60-95% ethanol solution and water, filtering after each extraction, standing and cooling, separating and removing petroleum ether, ether and precipitates, collecting and combining a 30-60% ethanol extracting solution, a 60-95% ethanol extracting solution and a water extracting solution, and then concentrating to remove ethanol to obtain a cistanche deserticola extracting solution;
(3) concentrating and drying the cistanche extracting solution, and crushing to obtain the cistanche extract.
2. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the enzyme deactivation operation in step (1) is: decocting fresh Cistanchis herba at 70-80 deg.C for 20-40 min.
3. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the drying temperature in step (1) is 50-80 ℃.
4. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the number of times of sonication of the cistanche tubulosa powder in each solvent in step (2) is 2-3, each sonication time is 5-10min, and each sonication interval is 15-30 min.
5. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the ultrasonic power in step (2) is 150- > 250W.
6. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the extraction temperature in step (2) is 60-80 ℃.
7. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the mass ratio of the cistanche tubulosa powder to the mixed solution of petroleum ether/diethyl ether/30-60% ethanol, the mixed solution of 60-95% ethanol and water in step (2) is 1:15-25, 1:10-20 and 1:10-20, respectively.
8. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the volume ratio of petroleum ether, diethyl ether and 30-60% ethanol in the mixed solution of petroleum ether/diethyl ether/30-60% ethanol of step (2) is 1-2:1-2: 3-5.
9. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the pH values of the petroleum ether/diethyl ether/30-60% ethanol mixed solution, the 60-95% ethanol solution and water in step (2) are all 4-6.
10. The method for extracting cistanche tubulosa as claimed in claim 1, wherein the cistanche tubulosa powder in step (2) is sequentially subjected to ultrasonic extraction in a mixed solution of petroleum ether/diethyl ether/50% ethanol, a 75% ethanol solution and water, filtering after each extraction, standing and cooling, separating to remove petroleum ether, diethyl ether and precipitates, collecting and combining a 50% ethanol extract, a 75% ethanol extract and a water extract, and then concentrating to remove ethanol to obtain a cistanche tubulosa extract.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114588201A (en) * | 2022-03-30 | 2022-06-07 | 北京中科健宇生物科技有限公司 | Preparation method of cistanche deserticola extract and alcohol effect relieving and liver protecting product containing cistanche deserticola extract |
| CN115120639A (en) * | 2022-06-02 | 2022-09-30 | 内蒙古三口生物科技有限公司 | Cistanche superfine powder and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441040A (en) * | 2011-12-07 | 2012-05-09 | 中国科学院新疆理化技术研究所 | Preparation method of cistanche deserticola phenylethanoid glycosides |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102441040A (en) * | 2011-12-07 | 2012-05-09 | 中国科学院新疆理化技术研究所 | Preparation method of cistanche deserticola phenylethanoid glycosides |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114588201A (en) * | 2022-03-30 | 2022-06-07 | 北京中科健宇生物科技有限公司 | Preparation method of cistanche deserticola extract and alcohol effect relieving and liver protecting product containing cistanche deserticola extract |
| CN114588201B (en) * | 2022-03-30 | 2024-01-02 | 北京中科健宇生物科技有限公司 | Preparation method of cistanche extract and anti-alcohol liver-protecting product containing cistanche extract |
| CN115120639A (en) * | 2022-06-02 | 2022-09-30 | 内蒙古三口生物科技有限公司 | Cistanche superfine powder and preparation method and application thereof |
| CN115120639B (en) * | 2022-06-02 | 2024-02-09 | 内蒙古三口生物科技有限公司 | Cistanche superfine powder and preparation method and application thereof |
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