CN113350827A - Fissistigma Oldhamii extractive solution and its preparation method - Google Patents
Fissistigma Oldhamii extractive solution and its preparation method Download PDFInfo
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- CN113350827A CN113350827A CN202110758997.7A CN202110758997A CN113350827A CN 113350827 A CN113350827 A CN 113350827A CN 202110758997 A CN202110758997 A CN 202110758997A CN 113350827 A CN113350827 A CN 113350827A
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Abstract
The invention belongs to the technical field of food, and particularly relates to a spilanthus fragrans extracting solution and a preparation method thereof. The preparation method comprises the following steps: (1) taking fresh spotted-blue leaves, drying at the temperature of 30-50 ℃, and crushing to obtain spotted-blue leaf powder; (2) adding an entrainer into the variegated orchid leaf powder, and stirring to obtain a premix, wherein the premix is a paste; (3) covering an adsorption material on the premix to form an adsorption layer and the premix to form a chromatographic structure, extracting by using a supercritical carbon dioxide extraction method, wherein during extraction, supercritical carbon dioxide fluid flows to the adsorption layer from the premix, and collecting an extract to prepare the radix Fissistigmatis Oldhamii extracting solution. The preparation method is simple in process, strong in operability, green, environment-friendly and energy-saving, and the obtained spiderflower herb extract is small in flavor and color loss in the preparation process and good in storage stability.
Description
Technical Field
The invention belongs to the technical field of food, and particularly relates to a spilanthus fragrans extracting solution and a preparation method thereof.
Background
The leaf of herba Epilobii is a plant spice, which is known as herba Pandani Paniculati or herba Vanillae Planifoliae, and has resistance to yin and dampness, little pest and disease damage, and strong vitality. The leaf of the spotted orchid is originally produced by Srilanka, Malaysia and Philippines, the leaf is mainly characterized in that an aromatic substance is 2-acetyl-1-pyrroline, can emit special rice dumpling aroma, is one of common spices in southeast Asia countries, is successfully bred with the high-flux spotted orchid seedling breeding success of the spice beverage research institute of the Chinese tropical agrology academy of sciences in recent years, is mainly planted in Hainan, Yunnan and the like, has been gradually developed into tropical characteristic agricultural industries, and has wide development and utilization prospects.
The leaf of variegated orchid is rich in active ingredients such as squalene and phytol, has the functions of enhancing cell activity, accelerating metabolism and improving human immunity, is widely applied to the industries of food, medicine and daily necessities, such as being generally used for making cakes, biscuits, cool drinks, candies and the like, and has wide market prospect.
The leaf of the variegated orchid is a herbaceous spice plant, is mainly sold in a fresh leaf form at present, and is mainly sold in places such as cake shops, hotels, restaurants and the like in the market to provide color, aroma and taste for food. However, since the fresh leaves are not easy to preserve and juice is required to be extracted from the fresh leaves, the use of the leaf of the variegated orchid is greatly limited when the leaf is used at present. Therefore, some technical schemes are also provided in the market for processing fresh leaf of variegated orchid into instant powder, so as to improve the transportation, storage and quality guarantee conditions of the product and increase the convenience of the application and processing of the product. However, because the characteristic aroma substance 2-acetyl-1-pyrroline of the leaf of the variegated orchid is very volatile, the aroma loss of the instant powder is serious in the processing process by adopting the processes of hot concentration, spray drying and the like, and the aroma of a finished product is seriously influenced. Therefore, the retention of the aroma of the leaf of the variegated orchid becomes one of the difficulties of the production and the market popularization of the product.
In order to solve the existing problems, patent CN202010092512.0 discloses a preparation method of a leaf product of variegated orchid, which adopts complex technical methods of ultralow temperature freezing, uniform temperature rise drying and the like to realize color retention and aroma enhancement of the variegated orchid, and the prepared leaf product of variegated orchid has the characteristics of high content of substances such as 2-acetyl-1-pyrroline, phytol, squalene and the like. Patent CN201410659988.2 discloses a method for preparing instant powder of high-aroma herba Epilobii leaf, which comprises the steps of adding water into herba Epilobii leaf, juicing, performing enzymolysis to obtain juice, performing centrifugal separation, performing membrane concentration on the centrifugate, adding maltodextrin, and freeze-drying to obtain instant powder of herba Epilobii leaf. The process for preparing the instant powder of the leaf of the variegated orchid avoids the modes of heating concentration, spray drying and the like, reduces the loss of color and aroma, but adopts membrane concentration and an enzymolysis method, and has more complex process. Generally, the existing process for preparing the instant powder of the variegated orchid is complex in preparation process and high in cost, and the variegated orchid pure powder has coarse fibers and can generate precipitates when being applied to beverage products, so that the patent technology is difficult to popularize on a large scale. Patent CN202011423384 discloses a method for preparing a gorgeous leaf juice or powder with complete gorgeous leaf nutrients, which provides an effective method for the nutrients in gorgeous leaves by preparing juice of gorgeous leaves: drying fresh herba Sonchi Oleracei leaves, cutting into pieces, squeezing into juice, adding cellulase, pectinase, etc., mixing for enzymolysis, centrifuging to obtain juice, and concentrating to obtain herba Sonchi Oleracei juice with sugar degree of 8-15. The herba Epilobii juice prepared by the method has short shelf life, needs thermal processes such as concentration, enzymolysis and the like, has complex process and has large flavor loss in the process.
Disclosure of Invention
Therefore, the preparation method of the high-quality fragrant cattleya extract is needed to be provided, and the preparation method is simple in preparation process, small in loss of flavor and color in the preparation process and good in storage stability.
A fragrant cattail extract and a preparation method thereof comprise the following steps:
taking fresh spotted-blue leaves, drying at the temperature of 30-50 ℃, and crushing to obtain spotted-blue leaf powder;
adding an entrainer into the variegated orchid leaf powder, and stirring to obtain a premix, wherein the premix is a paste;
covering an adsorption material on the premix to form an adsorption layer and the premix to form a chromatographic structure, extracting by using a supercritical carbon dioxide extraction method, wherein during extraction, supercritical carbon dioxide fluid flows to the adsorption layer from the premix, and collecting an extract to prepare the radix Fissistigmatis Oldhamii extracting solution.
In one embodiment, the drying temperature is 30-50 ℃, and a low-temperature dryer is adopted to dry the leaf of the cymbidium sinense.
In one embodiment, the adsorbent material is selected from one or both of diatomaceous earth and activated carbon.
In one embodiment, the weight ratio of the adsorbing material to the variegated blue powder is (1-5): 10.
in one embodiment, the entrainer is a mixed solution of alcohol and water;
the alcohol is selected from one or two of ethanol and propylene glycol.
In one embodiment, the alcohol is 20-90% by mass of the entrainer.
In one embodiment, the weight ratio of the entrainer to the leaf powder of the variegated orchid is (1-3): 1.
in one embodiment, the particle size of the leaf powder of the melaleuca indica is 20-60 meshes.
In one embodiment, the process parameters of the supercritical carbon dioxide extraction method comprise: the extraction pressure is 10-20 MPa, the extraction temperature is 30-45 ℃, the separation pressure is 4-8 MPa, the separation temperature is 30-60 ℃, and the extraction time is 30-90 min.
The invention also provides the vanillic aquaria extract prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
firstly, carrying out low-temperature drying and crushing pretreatment on the fresh leaves of the variegated orchid to obtain variegated orchid leaf powder, and keeping the color and the flavor of the fresh variegated orchid leaves to the maximum extent. And then mixing an entrainer and the variegated orchid leaf powder to prepare a premix, changing the weak polarity and the solubility of the supercritical carbon dioxide fluid by adding the entrainer, improving the solubility of the aroma substances and the active ingredients in the variegated orchid leaf in the supercritical carbon dioxide fluid, and effectively retaining the color and the flavor of the final variegated orchid extracting solution. Meanwhile, an adsorption material is covered on the premix, a formed adsorption layer and the premix form a chromatographic structure, during extraction, supercritical carbon dioxide fluid starts to dissolve and extract the premix of the leaf powder of the melaleuca sinica and the entrainer from the bottom of the chromatographic structure, then the supercritical carbon dioxide fluid flows to the adsorption layer, and polar impurities such as glue, wax, fine suspended matters and the like in the melaleuca sinica leaves are easily adsorbed by the adsorption layer, so that the impurities are adsorbed by the adsorption layer and are retained in the extraction kettle, and effective components flow out along with the supercritical carbon dioxide fluid. That is to say, the method realizes the synchronization of extraction and separation and purification, and effectively avoids the phenomena that the extract of the variegated orchid is easy to be turbid and layered in the process of placing at low temperature. Therefore, the invention discloses a preparation method which is simple in process, strong in operability, green, environment-friendly and energy-saving to obtain the extract of the fragrant variegated orchid, and the obtained extract has small loss of flavor and color and good storage stability in the preparation process.
In addition, the extraction method is stable, the process is easy to control, the processing capacity is large, the industrialized continuous large production is convenient to realize, and certain technical support and theoretical guidance are provided for the large-scale extraction of the leaf of the herba Epilobii.
Drawings
FIG. 1 is a schematic diagram of a supercritical carbon dioxide extraction apparatus;
reference numerals: 1-CO2 steel bottle, 2-filter, 3-refrigerator, 4-diaphragm pump, 5-hot water machine, 6-extraction kettle, 7-separation kettle, and 8-collection valve.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description taken in conjunction with the accompanying drawings. The detailed description sets forth the preferred embodiments of the invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The solid content of the paste is 25-50%.
The invention provides a radix Fissistigmatis Oldhamii extract and its preparation method, which comprises the following steps:
s101: taking fresh spotted-blue leaves, drying at the temperature of 30-50 ℃, and crushing to obtain spotted-blue leaf powder;
further, in step S101, the leaf of the cymbidium sinensis is subjected to a low-temperature drying process using a low-temperature dryer.
Further, in step S101, the fresh leaves of the melaleuca variegata need to be washed and drained before being dried at low temperature.
Further, in the step S101, the particle size of the leaf powder of the arundina graminifolia is 20-60 meshes.
According to the method, the Spot blue leaf powder is prepared by drying and crushing the fresh Spot blue leaves at a low temperature of 30-50 ℃, so that the color and the flavor of the fresh Spot blue leaves are retained to the greatest extent, and the color and the flavor quality of the final Spot blue leaf extracting solution are improved.
S102: adding an entrainer into the variegated orchid leaf powder, and stirring to obtain a premix, wherein the premix is a paste.
Further, in the step S102, the solid content of the paste is 25-50%.
Further, in the step S102, the entrainer is a mixed solution of alcohol and water.
Further, in the step S102, the alcohol is selected from one or both of ethanol and propylene glycol. Furthermore, the alcohol accounts for 20-90% of the entrainer by mass.
Further, in the step S102, the weight ratio of the entrainer to the variegated blue powder is (1-3): 1.
s103: covering an adsorption material on the premix to form an adsorption layer and the premix to form a chromatographic structure, extracting by using a supercritical carbon dioxide extraction method, wherein during extraction, supercritical carbon dioxide fluid flows to the adsorption layer from the premix, and collecting an extract to prepare the radix Fissistigmatis Oldhamii extracting solution.
Further, in the step S103, the adsorbing material is one or two selected from diatomite and activated carbon.
Further, in the step S103, the particle size of the adsorbing material is 60-80 meshes.
Further, in the step S103, the weight ratio of the adsorbing material to the leaf powder of the cymbidium maculatum is (1-5): 10.
further, in step S103, the process parameters of the supercritical carbon dioxide extraction method include: the extraction pressure is 10-20 MPa, the extraction temperature is 30-45 ℃, the separation pressure is 4-8 MPa, the separation temperature is 30-60 ℃, and the extraction time is 30-90 min.
Further, in step S103, the extract of tulipa edulis is a uniform mixture containing an entrainer. Furthermore, the yield of the extracting solution is 65-75% (the yield of the extracting solution is the solid content in the extracting solution/the weight of the fed herba lycopi powder is 100%).
According to the preparation method, the entrainer and the leaf powder of the variegated orchid are mixed to prepare a premix, the premix is placed in an extraction kettle, the supercritical carbon dioxide fluid is used as an extraction solvent, and then the entrainer is added to change the weak polarity and the solubility of the supercritical carbon dioxide fluid, so that the solubility of active ingredients such as aromatic substances and active ingredients in the variegated orchid leaves in the supercritical carbon dioxide fluid is improved, and the color and the flavor of the variegated orchid leaves in the final variegated orchid leaf extracting solution are effectively reserved. Further, the weight ratio of the entrainer to the leaf powder of the variegated orchid in the application is (1-3): compared with the weight ratio of the solvent used in the ordinary soxhlet extraction method to the leaf powder of the variegated orchid, the entrainer used in the method has less weight, and the obtained extracting solution is stronger and does not need to be concentrated. The adsorbing material is covered on the premix, so that a formed adsorbing layer and the premix form a chromatographic structure, further, polar impurities such as glue, wax, fine suspended matters and the like in the herba Zealand extracting solution can be removed by a method of combining supercritical carbon dioxide extraction and chromatographic adsorption, the herba Zealand extracting solution is purified, the phenomena of easy turbidity and layering of the herba Zealand extracting solution in the low-temperature placing process are effectively avoided, and the extraction and the separation and purification can be synchronously carried out.
According to the method, the loss of effective components in the melaleuca leaves is reduced by adjusting the weight ratio of the entrainer, the adsorption material and the melaleuca leaf powder and the extraction and separation conditions of supercritical carbon dioxide, so that the purity of the obtained fragrant melaleuca extracting solution is improved, and the flavor and the color of the melaleuca leaf powder are more effectively maintained.
The following are specific examples:
example 1
The preparation method of the radix Fissistigmatis Oldhamii extract in the embodiment comprises the following steps:
(1) taking fresh spotted-blue leaves as a raw material, cleaning and draining, drying the spotted-blue leaves at a low temperature of 35 ℃, and then crushing to obtain spotted-blue leaf powder with the granularity of 20-60 meshes.
(2) Weighing 1000g of the variegated leaf powder and 1000g of 60% alcohol water solution by mass, slowly adding the alcohol water solution into the variegated leaf powder, and stirring and mixing to obtain a premix, wherein the premix is paste.
(3) Referring to fig. 1, carbon dioxide comes out of a carbon dioxide steel cylinder 1, impurities in the carbon dioxide are removed through filtering by a filter 2, the carbon dioxide is cooled to be in a liquid state through a refrigerator 3, the liquid carbon dioxide is continuously pumped into a 5L extraction kettle 6 through a carbon dioxide diaphragm pump 4, the pressure of the liquid carbon dioxide reaches 15MPa of extraction pressure, the liquid carbon dioxide fluid is heated through a hot water machine 5, the temperature of the liquid carbon dioxide fluid reaches 40 ℃, and at the moment, the carbon dioxide reaches a supercritical state in the extraction kettle 6.
And (3) putting the premix into a supercritical carbon dioxide extraction kettle 6, continuously covering 200g of diatomite with the granularity of 60-80 meshes on the premix for 60min, after extraction is finished, putting the effective components of the premix into a separation kettle 7 along with the supercritical carbon dioxide, setting the separation pressure of the separation kettle 7MPa and the separation temperature of the separation kettle 7 to 45 ℃, collecting the extract in the separation kettle 7 in real time through a valve 8, and finally obtaining the fragrant variegated blue extracting solution.
Example 2
The preparation method of the radix Fissistigmatis Oldhamii extract in the embodiment comprises the following steps:
(1) taking fresh spotted-blue leaves as a raw material, cleaning and draining, drying the spotted-blue leaves at a low temperature of 35 ℃, and then crushing to obtain spotted-blue leaf powder with the granularity of 20-60 meshes.
(2) Weighing 1000g of the variegated leaf powder and 2000g of 60% alcohol water solution by mass, slowly adding the alcohol water solution into the variegated leaf powder, and stirring and mixing to obtain a premix, wherein the premix is paste.
(3) Referring to fig. 1, carbon dioxide comes out of a carbon dioxide steel cylinder 1, impurities in the carbon dioxide are removed through filtering by a filter 2, the carbon dioxide is cooled to be in a liquid state through a refrigerator 3, the liquid carbon dioxide is continuously pumped into a 5L extraction kettle 6 through a carbon dioxide diaphragm pump 4, the pressure of the liquid carbon dioxide reaches 15MPa of extraction pressure, the liquid carbon dioxide fluid is heated through a hot water machine 5, the temperature of the liquid carbon dioxide fluid reaches 40 ℃, and at the moment, the carbon dioxide reaches a supercritical state in the extraction kettle 6.
And (3) putting the premix into a supercritical carbon dioxide extraction kettle 6, continuously covering 200g of diatomite with the granularity of 60-80 meshes on the premix for 60min, after extraction is finished, putting the effective components of the premix into a separation kettle 7 along with the supercritical carbon dioxide, setting the separation pressure of the separation kettle 7MPa and the separation temperature of the separation kettle 7 to 45 ℃, collecting the extract in the separation kettle 7 in real time through a valve 8, and finally obtaining the fragrant variegated blue extracting solution.
Example 3
The preparation method of the radix Fissistigmatis Oldhamii extract in the embodiment comprises the following steps:
(1) taking fresh spotted-blue leaves as a raw material, cleaning and draining, drying the spotted-blue leaves at a low temperature of 35 ℃, and then crushing to obtain spotted-blue leaf powder with the granularity of 20-60 meshes.
(2) Weighing 1000g of the variegated leaf powder and 3000g of 60% alcohol water solution by mass, slowly adding the alcohol water solution into the variegated leaf powder, and stirring and mixing to obtain a premix, wherein the premix is paste.
(3) Referring to fig. 1, carbon dioxide comes out of a carbon dioxide steel cylinder 1, impurities in the carbon dioxide are removed through filtering by a filter 2, the carbon dioxide is cooled to be in a liquid state through a refrigerator 3, the liquid carbon dioxide is continuously pumped into a 5L extraction kettle 6 through a carbon dioxide diaphragm pump 4, the pressure of the liquid carbon dioxide reaches 15MPa of extraction pressure, the liquid carbon dioxide fluid is heated through a hot water machine 5, the temperature of the liquid carbon dioxide fluid reaches 40 ℃, and at the moment, the carbon dioxide reaches a supercritical state in the extraction kettle 6.
And (3) putting the premix into a supercritical carbon dioxide extraction kettle 6, continuously covering 200g of diatomite with the granularity of 60-80 meshes on the premix for 60min, after extraction is finished, putting the effective components of the premix into a separation kettle 7 along with the supercritical carbon dioxide, setting the separation pressure of the separation kettle 7MPa and the separation temperature of the separation kettle 7 to 45 ℃, collecting the extract in the separation kettle 7 in real time through a valve 8, and finally obtaining the fragrant variegated blue extracting solution.
Example 4
The preparation method of the radix Fissistigmatis Oldhamii extract in the embodiment comprises the following steps:
(1) taking fresh spotted-blue leaves as a raw material, cleaning and draining, drying the spotted-blue leaves at a low temperature of 35 ℃, and then crushing to obtain spotted-blue leaf powder with the granularity of 20-60 meshes.
(2) Weighing 1000g of the variegated leaf powder and 1000g of 60% alcohol water solution by mass, slowly adding the alcohol water solution into the variegated leaf powder, and stirring and mixing to obtain a premix, wherein the premix is paste.
(3) Referring to fig. 1, carbon dioxide comes out of a carbon dioxide steel cylinder 1, impurities in the carbon dioxide are removed through filtering by a filter 2, the carbon dioxide is cooled to be in a liquid state through a refrigerator 3, the liquid carbon dioxide is continuously pumped into a 5L extraction kettle 6 through a carbon dioxide diaphragm pump 4, the pressure of the liquid carbon dioxide reaches 15MPa of extraction pressure, the liquid carbon dioxide fluid is heated through a hot water machine 5, the temperature of the liquid carbon dioxide fluid reaches 40 ℃, and at the moment, the carbon dioxide reaches a supercritical state in the extraction kettle 6.
And (2) putting the premix into a supercritical carbon dioxide extraction kettle 6, continuously covering 300g of diatomite with the granularity of 60-80 meshes on the premix for 60min, after extraction is finished, putting the effective components of the premix into a separation kettle 7 along with the supercritical carbon dioxide, setting the separation pressure of the separation kettle 7MPa and the separation temperature of the separation kettle 7 to 45 ℃, collecting the extract in the separation kettle 7 in real time through a valve 8, and finally obtaining the fragrant variegated blue extracting solution.
Example 5
The preparation method of the radix Fissistigmatis Oldhamii extract in the embodiment comprises the following steps:
(1) taking fresh spotted-blue leaves as a raw material, cleaning and draining, drying the spotted-blue leaves at a low temperature of 35 ℃, and then crushing to obtain spotted-blue leaf powder with the granularity of 20-60 meshes.
(2) Weighing 1000g of the variegated leaf powder and 1000g of 60% alcohol water solution by mass, slowly adding the alcohol water solution into the variegated leaf powder, and stirring and mixing to obtain a premix, wherein the premix is paste.
(3) Referring to fig. 1, carbon dioxide comes out from a carbon dioxide steel cylinder 1, impurities in the carbon dioxide are removed by filtering through a filter 2, the carbon dioxide is cooled to be in a liquid state through a refrigerator 3, the liquid carbon dioxide is continuously pumped into a 5L extraction kettle 6 through a carbon dioxide diaphragm pump 4, the pressure of the liquid carbon dioxide reaches 10MPa of extraction pressure, the liquid carbon dioxide fluid is heated through a hot water machine 5, the temperature of the liquid carbon dioxide fluid reaches 45 ℃ of extraction temperature, and at the moment, the carbon dioxide reaches a supercritical state in the extraction kettle 6.
And (3) putting the premix into a supercritical carbon dioxide extraction kettle 6, continuously covering 200g of diatomite with the granularity of 60-80 meshes on the premix for 60min, after extraction is finished, putting the effective components of the premix into a separation kettle 7 along with the supercritical carbon dioxide, setting the separation pressure of the separation kettle 7 to be 4MPa and the separation temperature to be 50 ℃, collecting the extract in the separation kettle 7 in real time through a valve 8, and finally obtaining the fragrant variegated blue extracting solution.
Comparative example 1
The extract of the vanillic aquatica in the comparative example and the preparation method thereof are basically the same as those in the example 2, and the main difference is that no adsorbing material is added, and the steps are as follows:
(1) taking fresh spotted-blue leaves as a raw material, cleaning and draining, drying the spotted-blue leaves at a low temperature of 35 ℃, and then crushing to obtain spotted-blue leaf powder with the granularity of 20-60 meshes.
(2) Weighing 1000g of the variegated leaf powder and 2000g of 60% alcohol water solution by mass, slowly adding the alcohol water solution into the variegated leaf powder, and stirring and mixing to obtain a premix, wherein the premix is paste.
(3) Referring to fig. 1, carbon dioxide comes out of a carbon dioxide steel cylinder 1, impurities in the carbon dioxide are removed through filtering by a filter 2, the carbon dioxide is cooled to be in a liquid state through a refrigerator 3, the liquid carbon dioxide is continuously pumped into a 5L extraction kettle 6 through a carbon dioxide diaphragm pump 4, the pressure of the liquid carbon dioxide reaches 15MPa of extraction pressure, the liquid carbon dioxide fluid is heated through a hot water machine 5, the temperature of the liquid carbon dioxide fluid reaches 40 ℃, and at the moment, the carbon dioxide reaches a supercritical state in the extraction kettle 6.
And (2) putting the premix into a supercritical carbon dioxide extraction kettle 6, wherein the extraction time is 60min, after the extraction is finished, enabling the effective components and the impurity components of the premix to enter a separation kettle 7 along with the supercritical carbon dioxide, setting the separation pressure of 7MPa and the separation temperature of 45 ℃ of the separation kettle 7, and collecting the extract in the separation kettle 7 in real time through a valve 8 to finally obtain the fragrant variegated blue extract.
Comparative example 2
The preparation method of the radix Fissistigmatis Oldhamii extract in the comparative example comprises the following steps:
(1) taking fresh spotted-blue leaves as a raw material, cleaning and draining, drying the spotted-blue leaves at a low temperature of 35 ℃, and then crushing to obtain spotted-blue leaf powder with the granularity of 20-60 meshes.
(2) Weighing 100g of the variegated leaf powder and 600g of 60% alcohol water solution by mass, slowly adding the alcohol water solution into the variegated leaf powder, and stirring and mixing to obtain a premix, wherein the premix is paste.
(3) Placing the premix in a filter paper sleeve, placing the filter paper sleeve in an extraction chamber, performing ordinary hot extraction by adopting a Soxhlet extraction method, heating and boiling alcohol at a circulating dynamic temperature of 85 ℃, rising alcohol vapor through an air duct, condensing the alcohol vapor into liquid, feeding the liquid into an extractor, collecting the liquid to obtain an extract, filtering the extract by adopting a 0.45-micrometer filter membrane, and finally concentrating the filtered extract to prepare the leaf extract of the variegated orchid.
Finally, color and flavor evaluations were performed on the extracts of examples 1 to 5 and comparative examples 1 to 2, respectively, specifically:
color evaluation
And measuring absorbance values with the wavelengths of 645nm and 663nm by adopting a spectrophotometry method so as to evaluate the color of the variegated blue extracting solution.
2g of the extract of Epilobium angustifolium of examples 1-5 and comparative examples 1-2 was weighed, the extract was diluted with 95% ethanol to 100g, and the absorbance of the 2% extract of Epilobium angustifolium was measured.
Flavor evaluation
The flavor of the extract of the spotted blue was evaluated by adding 0.5% of an aqueous sugar solution.
Specific test results are shown in table 1;
table 1 presents the color and flavor evaluation results of the spotted blue extract solutions in examples and comparative examples. The appearance of examples 1-5 was a dark green, homogeneous solution, while the flavor profile was: the flavor is rich, natural and light green, and the aftertaste has the special bitter taste of the spotted orchid. In contrast, in comparative example 1, although the appearance of the extract liquid was blackish green, dotted black-green particles were observed, and the extract liquid was turbid after filtration and standing. The adsorption material is added to remove impurities such as glue, wax, fine suspended matters and the like in the herba Epilobii extract, so that the herba Epilobii extract is purified, and the phenomenon that the herba Epilobii extract is easily turbid and layered in the low-temperature placing process is effectively avoided. In contrast, in comparative example 2, the leaves of the maculate were subjected to a concentration treatment by ordinary heat extraction at a cycle temperature of 85 ℃, and the color and flavor of the leaves were greatly lost. By combining the examples 1-5 and the comparative examples 1-2, the method for combining the supercritical carbon dioxide extraction and the chromatographic adsorption in the application is further demonstrated to obtain the high-quality radix Fissistigmatis Oldhamii extract with small flavor and color loss and good storage stability in the preparation process.
TABLE 1
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be defined by the appended claims.
Claims (10)
1. A preparation method of a radix Fissistigmatis Oldhamii extract is characterized by comprising the following steps:
taking fresh spotted-blue leaves, drying at the temperature of 30-50 ℃, and crushing to obtain spotted-blue leaf powder;
adding an entrainer into the variegated orchid leaf powder, and stirring to obtain a premix, wherein the premix is a paste;
covering an adsorption material on the premix to form an adsorption layer and the premix to form a chromatographic structure, extracting by using a supercritical carbon dioxide extraction method, wherein during extraction, supercritical carbon dioxide fluid flows to the adsorption layer from the premix, and collecting an extract to prepare the radix Fissistigmatis Oldhamii extracting solution.
2. The method for preparing the fragrant cattleya extract as claimed in claim 1, wherein the adsorbing material is selected from one or two of diatomite and activated carbon.
3. The preparation method of the radix Fissistigmatis Oldhamii extract according to claim 1, wherein the particle size of the adsorbing material is 60-80 meshes.
4. The preparation method of the fragrant cattleya extract as claimed in claim 1, wherein the weight ratio of the adsorbing material to the cattleya leaf powder is (1-5): 10.
5. the method for preparing the fragrant cattleya extract as claimed in claim 1, wherein the entrainer is a mixed solution of alcohol and water; and
the alcohol is selected from one or two of ethanol and propylene glycol.
6. The preparation method of the radix Fissistigmatis Oldhamii extract according to claim 5, wherein the alcohol accounts for 20-90% of the entrainer by mass.
7. The preparation method of the radix Fissistigmatis Oldhamii extract according to claim 1, wherein the weight ratio of the entrainer to the leaf powder of the herba Fissistigmatis Oldhamii is (1-3): 1.
8. the preparation method of the fragrant cattleya extract as claimed in claim 1, wherein the particle size of the cattleya leaf powder is 20-60 meshes.
9. The preparation method of the radix Fissistigmatis Oldhamii extract according to claim 1, wherein the supercritical carbon dioxide extraction method comprises the following process parameters: the extraction pressure is 10-20 MPa, the extraction temperature is 30-45 ℃, the separation pressure is 4-8 MPa, the separation temperature is 30-60 ℃, and the extraction time is 30-90 min.
10. A Fissistigma Oldhamii extractive solution prepared by the method of any one of claims 1-9.
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