CN113274324B - Preparation method of saponin extract - Google Patents

Preparation method of saponin extract Download PDF

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CN113274324B
CN113274324B CN202110561147.8A CN202110561147A CN113274324B CN 113274324 B CN113274324 B CN 113274324B CN 202110561147 A CN202110561147 A CN 202110561147A CN 113274324 B CN113274324 B CN 113274324B
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saponin
extract
solution
decoloration
oxidation
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CN113274324A (en
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陈殿松
马铃
王靖
杨井囯
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Guangzhou Gude Personal Nursing Products Co ltd
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783Angiosperms [Magnoliophyta]
    • A61K8/9789Magnoliopsida [dicotyledons]
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00Preparations for care of the skin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/10General cosmetic use
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/80Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
    • A61K2800/805Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95

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Abstract

The invention discloses a preparation method of saponin extract, which comprises the steps of filtering a crushed saponin fruit body solution to obtain a crude saponin horn extract, adding gelatin for decoloring to obtain adsorbed and decolored saponin extract; and adding hydrogen peroxide into the adsorption-decolored saponin extract liquid for oxidation-decoloration treatment, wherein the addition amount of the hydrogen peroxide is 30-120% of the mass of solids in the adsorption-decolored saponin extract liquid, and the decoloration temperature is 40-90 ℃, so that the decolored saponin extract liquid is obtained. The method provided by the invention obviously improves the decolorization effect, can also enhance the stability of the extracting solution, thereby avoiding the introduction of ethanol in the traditional process, and solving the technical problems that the decolorization efficiency is poor, the solution stability is not enough, and the solution is easy to become turbid and the foam performance is influenced after being added into daily chemical products by the conventional water extraction method.

Description

Preparation method of saponin extract
Technical Field
The invention belongs to the technical field of chemical extraction processes, and particularly relates to a preparation method of a saponin extraction solution.
Background
The surfactant derived from natural plants has a series of outstanding advantages of good biodegradability, high mildness, low skin irritation and the like, and is increasingly one of important research directions of daily chemical research. Chinese plant resources are rich, and among the Chinese honey locust tree (Gleditsia sinensis) pods are rich in a large amount of saponin, have excellent foam property, and are discovered by ancient people for a long time and applied to daily life. In recent years, how to realize the industrial extraction of the saponin of the gleditsia sinensis is one of the research hotspots in the fields of biology and daily chemicals.
The existing extraction technology of the saponin can be mainly divided into alcohol extraction and water extraction. The alcohol extraction method uses organic solvents such as ethanol and butanediol as extraction media, and has the advantages that a large amount of water-soluble impurities can be removed, the obtained saponin has high purity, but the alcohol extraction method relates to the organic solvents, so the economic cost is high, explosion-proof equipment is required in the production environment, and great inconvenience is brought to industrial production. In addition, the product obtained by the alcohol extraction method often retains considerable water-insoluble impurities, and the water solubility is poor, so that the inconvenience is brought to the application of the saponin extract in an aqueous phase daily chemical product system. In comparison, the water extraction method has lower cost and correspondingly lower equipment requirement, and is more suitable for industrial production. The main problem of the water extraction method is that besides the saponin of the gleditsia sinensis, the extract also has a large amount of colloid, polysaccharide, flavone and other impurities, so that the gleditsia sinensis extract has darker color and poorer stability, and is easy to deteriorate and settle after being placed for a long time. Currently, the method of water extraction and alcohol precipitation is commonly used, i.e. ethanol is added into water extraction saponin extract to change the solubility of impurities and separate the impurities out. However, the method is complex in process, ethanol needs to be removed and recovered in the subsequent process, the equipment investment is large, and the use of the organic solvent is not in accordance with the concept of green process. Therefore, the development of an efficient water extraction method of the saponin extraction solution ensures that the saponin extraction solution has less impurities, low color and high stability, is convenient for subsequent application, and has important practical significance.
Disclosure of Invention
This section is for the purpose of summarizing some aspects of embodiments of the invention and to briefly introduce some preferred embodiments. In this section, as well as in the abstract and the title of the invention of this application, simplifications or omissions may be made to avoid obscuring the purpose of the section, the abstract and the title, and such simplifications or omissions are not intended to limit the scope of the invention.
The invention provides a preparation method of a saponin extract, which is characterized by comprising the following steps: comprises filtering crushed fructus Gleditsiae Abnormalis fruit body solution to obtain crude fructus Gleditsiae Abnormalis extractive solution, adding gelatin for decolorizing treatment to obtain adsorption decolorized fructus Gleditsiae Abnormalis extractive solution; and adding hydrogen peroxide into the adsorption-decolored saponin extract liquid for oxidation-decoloration treatment, wherein the addition amount of the hydrogen peroxide is 30-120% of the mass of solids in the adsorption-decolored saponin extract liquid, and the decoloration temperature is 40-90 ℃, so that the decolored saponin extract liquid is obtained.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: and filtering the crushed saponin fruit body solution, dissolving the crushed seed-removed saponin fruit body in water, stirring and extracting for 0.5-3 h at 40-80 ℃, and filtering to obtain a crude saponin extraction liquid.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: the filtration is carried out by adopting a Buchner funnel and rapid qualitative filter paper for suction filtration; the crushed seed-removed saponin pod entity is dissolved in water, and the ratio of the seed-removed saponin pod entity to the water is 1: 5-20.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: the gelatin is added for decoloring, and the gelatin is soaked in deionized water for 0.5 to 2 hours, then added into the crude saponin extracting solution for adsorption decoloring, and stirred at normal temperature for 0.5 to 2 hours; and filtering to remove gelatin after the decolorization treatment is finished.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: and the gelatin is added for decoloring treatment, wherein the gelatin is added according to the proportion of 50-90% of the solid content in the crude soap horn extracting solution.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: adding hydrogen peroxide into the adsorption-decolored saponin extract to perform oxidation-decoloration treatment, wherein the addition amount of the hydrogen peroxide is 35-50% of the mass of solids in the adsorption-decolored saponin extract; and adding the raw materials twice or more in the decoloring process; and maintaining the solution pH above 10.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: adding hydrogen peroxide for three times in the decoloring process to perform oxidation decoloring treatment; the total oxidation and decoloration time is 1-3 h.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: the oxidation and decoloration treatment is carried out at the temperature of 50-70 ℃,
as a preferable embodiment of the method for producing the saponin extract liquid of the present invention: the total oxidation and decoloration time of the oxidation and decoloration treatment is 2 h.
As a preferable embodiment of the method for producing the saponin extract liquid of the present invention: and further comprises adding sodium chloride solid as an auxiliary agent while performing oxidation decoloring treatment, wherein the addition amount of the sodium chloride is more than 1%.
The invention has the beneficial effects that: the method provided by the invention obviously improves the decolorization effect, can also enhance the stability of the extracting solution, thereby avoiding the introduction of ethanol in the traditional process, and solving the technical problems that the decolorization efficiency is poor, the solution stability is not enough, and the solution is easy to become turbid and the foam performance is influenced after being added into daily chemical products by the conventional water extraction method. The extraction and decoloration process provided by the invention has the characteristics of simple operation, outstanding effect and stable product, and is suitable for industrial production practice.
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In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise. Wherein:
FIG. 1 is an appearance diagram of decolorized extract of Gleditsia sinensis prepared by different methods.
FIG. 2 is an external view of a decolorized extract of Gleditsia sinensis prepared in example 1.
FIG. 3 is a graph showing the stability test of the decolorized extract of Gleditsia sinensis Lam prepared in example 4.
FIG. 4 is a graph showing the stability of an extract solution of Gleditsia sinensis Lam prepared in example 5.
FIG. 5 is a graph showing the stability of an extract solution of Gleditsia sinensis Lam prepared in example 1.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, but the present invention may be practiced in other ways than those specifically described and will be readily apparent to those of ordinary skill in the art without departing from the spirit of the present invention, and therefore the present invention is not limited to the specific embodiments disclosed below.
Furthermore, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one implementation of the invention. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1:
after the clean washing of fresh whole pod entity of saponin, 50 ℃ is dried to the constant weight, subtracts the segmentation clamp after saponin pod both ends and smashes to get rid of the seed, obtain the broken seed removal saponin pod entity, weigh 100g fruit entity according to 1: 10(g/mL) of deionized water is added, extraction is carried out for 2h under the conditions of 70 ℃ and stirring speed of 20rpm, filter residue and filtrate are filtered and separated, a Buchner funnel and rapid qualitative filter paper are adopted for filtration under 1 atmospheric pressure to obtain 1000mL of crude soap horn extract, the concentration of solids (note: the solid content is hereinafter calculated by CL, the solid refers to substances except water in the filtrate) is tested, and the concentration CL of the solids is 3.8 percent, namely the mass of the solids is 38 g.
Weighing gelatin (product number 10010328) at a ratio of 70% of the solid in the crude fructus Gleditsiae Abnormalis extractive solution, soaking the gelatin in deionized water for 1 hr, adding into the crude fructus Gleditsiae Abnormalis extractive solution, adsorbing and decolorizing, and stirring at room temperature for 60 min; the gelatin was removed by filtration in the same manner to obtain an adsorption-decolorized extract of Gleditsia sinensis (Saponaria japonica) having a solid concentration (i.e., the solid concentration in the adsorption-decolorized extract of Gleditsia sinensis) of 3.7% while the volume loss of the extract was kept at 1000mL regardless of a small volume loss in the experiment.
Adding hydrogen peroxide with the mass of 35% of the solid in the adsorption-decolored saponin extracting solution into the adsorption-decolored saponin extracting solution for three times on average, carrying out oxidation decoloration treatment, simultaneously adding NaCl solid serving as an auxiliary agent, wherein the addition amount of NaCl is 2 wt% of the total weight (g) of the liquid, the decoloration temperature is 70 ℃, the total oxidation decoloration time is 2 hours, the pH value is adjusted to 10.5 by adding a NaOH solution with the mass fraction of 5%, the pH of the solution is reduced along with the decoloration, and the alkali liquor is added in time to keep the pH to be more than or equal to 10; after the decolorization is finished, insoluble substances generated in the decolorization process are removed by filtering by the same method, and the pH is adjusted to 7 to obtain decolorized saponin extract.
The experimental results are as follows:
1. and (3) testing the extraction rate:
the yield EY (%) of the decolorized saponin extract of the present invention is represented by EY ═ (CL × VL)/M × 100, where M is the total mass of the de-seeded saponin pod entities, and CL and VL are the concentration of solids in the aqueous phase and the volume of the aqueous phase, respectively. Wherein CL is determined by the following method: weighing 10mL of saponin extract, drying at 70 ℃ to constant weight to obtain a solid with mass m, wherein the concentration CL of the solid is m/10 mL. The extraction rate of the saponin extract of the present invention was 36%. The saponin content in the saponin extracting solution of the invention is 3.98 mg/mL.
2. Decoloring efficiency:
the decolorization efficiency is measured by absorbance, and the absorbance of the extracted saponin extract of the present invention is measured by spectrophotometry. The concrete method is that the decolorized saponin extract is taken and is compared with deionized water, and the absorbance of the saponin extract at 465nm is tested. The decolorization rate can be calculated to be 85.6% by comparing the absorbance of the saponin with that of the crude saponin extraction solution, which shows that the method has very excellent decolorization efficiency on the saponin extraction solution.
3. Stability of the solution:
the obtained saponin extract is sampled in a conical flask with a plug and placed in a thermostat, and the obtained solution is placed at 50 ℃ for 48 hours, so that the clarity of the obtained solution is unchanged, and the prepared saponin extract is proved to have good stability. See fig. 5.
4. Foam performance:
the foaming power of the saponin extract was tested according to GB/T13173-2008 Roche foam apparatus method, with a foam height of 105mm and a foam height of 65mm after 5 min.
According to the invention, the gelatin and the hydrogen peroxide are combined, and the NaCl solid is added during the hydrogen peroxide decolorization treatment, so that the prepared saponin extracting solution is clear and transparent, the decolorization efficiency is high, and the solution stability and the foam performance are good. The extraction and decoloration process provided by the invention has the characteristics of simple operation, outstanding effect and stable product, and is suitable for industrial production practice.
Example 2:
after the clean washing of fresh whole pod entity of saponin, 50 ℃ is dried to the constant weight, subtracts the segmentation clamp after saponin pod both ends and smashes to get rid of the seed, obtain the broken seed removal saponin pod entity, weigh 100g fruit entity according to 1: 10(g/mL) of deionized water was added, extraction was carried out at 40 ℃ and a stirring speed of 200rpm for 3 hours, filtration was carried out to separate the residue from the filtrate, and filtration was carried out by suction filtration using a Buchner funnel and a rapid qualitative filter paper under 1 atm to obtain 1000mL of a crude soapberry extract, and the concentration of a solid was measured (note: solid content hereinafter, it is determined by CL, and solid means a substance other than water in the filtrate).
Weighing gelatin according to the proportion of 50% of the solid substance in the crude soap horn extracting solution, soaking the gelatin in deionized water for 2h, adding the gelatin into the crude saponin extracting solution, performing adsorption and decoloration treatment, and stirring at normal temperature for 120 min; filtering to remove gelatin to obtain adsorbed and decolorized fructus Gleditsiae Abnormalis extractive solution, and measuring the solid concentration (i.e. the solid concentration in the adsorbed and decolorized fructus Gleditsiae Abnormalis extractive solution) at the time when the volume of fructus Gleditsiae Abnormalis extractive solution is still 1000mL regardless of small volume loss in the experiment.
Adding hydrogen peroxide with the solid mass of 50% in the adsorption-decolored saponin extracting solution into the adsorption-decolored saponin extracting solution for three times to perform oxidation-decoloration treatment, simultaneously adding NaCl solid serving as an auxiliary agent, wherein the addition amount of NaCl is 1 wt% of the total weight (g) of the liquid, the decoloring temperature is 50 ℃, the total decoloring time is 120min, the pH value is adjusted to 10.5 by adding a NaOH solution with the mass fraction of 5%, the pH value of the solution is reduced along with the progress of decoloration, and the pH value is maintained to be more than or equal to 10 by timely supplementing alkali liquor; filtering to remove insoluble substances generated in the decolorization process after decolorization is finished, and adjusting pH to 7 to obtain decolorized fructus Gleditsiae Abnormalis extractive solution.
The yield EY (%) of the decolorized saponin extract of the present invention is represented by EY ═ (CL × VL)/M × 100, where M is the total mass of the de-seeded saponin pod entities, and CL and VL are the concentration of solids in the aqueous phase and the volume of the aqueous phase, respectively. Wherein CL is determined by the following method: weighing 10mL of saponin extract, drying at 70 ℃ to constant weight to obtain a solid with mass m, wherein the concentration CL of the solid is m/10 mL. The extraction rate of the saponin extract of the present invention was 28%.
The decolorization efficiency is measured by absorbance, and the absorbance of the extracted saponin extract of the present invention is measured by spectrophotometry. The concrete method is that the decolorized saponin extract is taken and is compared with deionized water, and the absorbance of the saponin extract at 465nm is tested. The absorbance of the extracted saponin extract liquid is 0.046, and the corresponding decolorization rate is 78.6%.
Example 3:
after the clean washing of fresh whole pod entity of saponin, 50 ℃ is dried to the constant weight, subtracts the segmentation clamp after saponin pod both ends and smashes to get rid of the seed, obtain the broken seed removal saponin pod entity, weigh 100g fruit entity according to 1: 10(g/mL) of deionized water, extracting at 80 ℃ and 10rpm of stirring speed for 1h, filtering and separating filter residue and filtrate, filtering by using a Buchner funnel and a quick qualitative filter paper under 1 atmosphere to obtain 1000mL of crude saponin extract, and measuring the concentration of a solid (note: the solid content is hereinafter calculated by CL, and the solid refers to substances except water in the filtrate).
Weighing gelatin according to the proportion of 90% of the solid matter in the crude soap horn extract, soaking the gelatin in deionized water for 0.5h, adding the gelatin into the crude soap horn extract, performing adsorption decoloration treatment, and stirring at normal temperature for 30 min; filtering to remove gelatin to obtain adsorbed and decolorized fructus Gleditsiae Abnormalis extractive solution, and measuring the solid concentration (i.e. the solid concentration in the adsorbed and decolorized fructus Gleditsiae Abnormalis extractive solution) at the time when the volume of fructus Gleditsiae Abnormalis extractive solution is still 1000mL regardless of small volume loss in the experiment.
Adding hydrogen peroxide with the solid mass of 120% in the adsorption-decolored saponin extracting solution into the adsorption-decolored saponin extracting solution for three times to perform oxidation-decoloration treatment, simultaneously adding NaCl solid serving as an auxiliary agent, wherein the addition amount of NaCl is 3 wt% of the total weight (g) of the liquid, the decoloring temperature is 90 ℃, the total decoloring time is 30min, the pH value is adjusted to 10.5 by adding a NaOH solution with the mass fraction of 5%, the pH value of the solution is reduced along with the progress of decoloration, and the pH value is maintained to be more than or equal to 10 by timely supplementing alkali liquor; filtering to remove insoluble substances generated in the decolorization process after decolorization is finished, and adjusting pH to 7 to obtain decolorized fructus Gleditsiae Abnormalis extractive solution.
The yield EY (%) of the decolorized saponin extract of the present invention is represented by EY ═ (CL × VL)/M × 100, where M is the total mass of the de-seeded saponin pod entities, and CL and VL are the concentration of solids in the aqueous phase and the volume of the aqueous phase, respectively. Wherein CL is determined by the following method: weighing 10mL of saponin extract, drying at 70 ℃ to constant weight to obtain a solid with mass m, wherein the concentration CL of the solid is m/10 mL. The extraction rate of the saponin extract of the present invention was 33%.
The decolorization efficiency is measured by absorbance, and the absorbance of the extracted saponin extract of the present invention is measured by spectrophotometry. The concrete method is that the decolorized saponin extract is taken and is compared with deionized water, and the absorbance of the saponin extract at 465nm is tested. The absorbance of the extracted saponin extract liquid is 0.038, and the corresponding decolorization rate is 82.3%.
Example 4:
in comparison with example 1, the other preparation methods were the same as example 1 without adding NaCl.
The decolorization efficiency is measured by absorbance, and the absorbance of the extracted saponin extract of the present invention is measured by spectrophotometry. The concrete method is that the decolorized saponin extract is taken and is compared with deionized water, and the test shows that the absorbance of the saponin extract at 465nm is 0.062, the corresponding decolorization rate is 71.2%, and the decolorization rate is better.
Stability of the solution: sampling the obtained fructus Gleditsiae Abnormalis extractive solution, placing in conical flask with plug, standing in constant temperature incubator at 50 deg.C for 48 hr, wherein flocculent precipitate is visible on the bottom of conical flask, and the upper part of the solution is cloudy. The sodium chloride with proper concentration is added while decoloring, so that the stability of the prepared saponin extraction solution can be obviously improved. FIG. 3 is a graph showing the results of the stability test of the extract liquid of Gleditsia sinensis prepared in this example.
Example 5:
the amount of NaCl added was 0.5 wt% as compared with example 1, and the other experimental procedures were the same as in example 1.
Solution stability the stability of the solution was tested in the same way and after 48h a flocculent precipitate was visible (figure 4), indicating that a lower amount of sodium chloride added did not significantly improve the solution stability.
Comparative example 1:
compared with example 4, the gelatin is replaced by diatomite, and other preparation methods are the same as example 4.
The decolorization efficiency is measured by absorbance, and the absorbance of the extracted saponin extract of the present invention is measured by spectrophotometry. The concrete method is that the decolorized saponin extract is taken and is compared with deionized water, and the absorbance of the saponin extract at 465nm is tested to be 0.185, and the corresponding decolorization rate is 14.0%. Which indicates that the decoloring effect is not good.
Poor solution stability and foam properties: the solution was tested for stability in the same way and after 48h a flocculent precipitate was visible.
The foam properties were tested in the same way, with a foam height of 41mm, which disappeared completely after 5 min. The solution stability and the foaming power are not good after the diatomite is decolored.
Comparative example 2:
compared with example 4, gelatin was replaced with activated carbon, and other preparation methods were the same as example 4.
The decolorization efficiency is measured by absorbance, and the absorbance of the extracted saponin extract of the present invention is measured by spectrophotometry. The concrete method is that the decolorized saponin extract is taken and is compared with deionized water, the absorbance of the saponin extract at 465nm is tested to be 0.076, the corresponding decolorization rate is 64.7%, and the sensory color of the solution is black. The active carbon has poor decolorizing effect, and active carbon scraps are remained in the solution and are difficult to filter and remove.
Solution stability and foam properties: the solution was tested for stability in the same way, and after 48h a flocculent precipitate was visible with a black powdery material.
The foaming force was measured in the same manner, and the foam height was 64mm and after 5min was 11 mm. The solution stability and the foaming force are not good after the activated carbon is decolorized.
Comparative example 3:
the decolorization temperature was 30 ℃ in the case of oxidative decolorization treatment using hydrogen peroxide as compared with example 1, and other preparation methods were the same as in example 1.
The decolorization efficiency is measured by absorbance, and the absorbance of the extracted saponin extract of the present invention is measured by spectrophotometry. The concrete method is that the decolorized saponin extract is taken and is compared with deionized water, and the absorbance of the saponin extract at 465nm is tested to be 0.105, and the corresponding decolorization rate is 51.2%. It is shown that the decoloring effect is not good due to the excessively low decoloring temperature.
Comparative example 4:
the decolorization temperature was 95 ℃ in the case of oxidative decolorization treatment using hydrogen peroxide as compared with example 1, and the other preparation methods were the same as in example 1. The saponin extract evaporated too quickly in the experiment, making the experiment difficult to perform.
Comparative example 5:
in comparison with example 1, hydrogen peroxide was added to the extract of saponin at a time, and NaOH was not supplemented during the decoloring, and the other preparation methods were the same as example 1.
The absorbance of the test saponin extract at 465nm was 0.065, corresponding to a decolorization rate of 69.8%. The method for decoloring by adding hydrogen peroxide at one time is obviously lower than the method for adding hydrogen peroxide at different times.
From left to right in fig. 1 are: a left one: the extract of Chinese honeylocust fruit obtained by only using the oxidation decoloring method (compared with example 4, no gelatin is added, and other preparation methods are the same as those of example 4) has a decoloring effect obviously inferior to that of example 4, Zuo-Di: the extract of gleditsia sinensis lam prepared in example 4, right one: the extract of gleditsia sinensis lam prepared in comparative example 2; FIG. 2 shows the decolorized extract of Gleditsia sinensis Lam obtained in example 1. Comparing fig. 1 and fig. 2, it is clearly evident that the decolorization effect of example 1 is significantly better, and the solution is clear and has the highest transparency.
In conclusion, the method provided by the invention obviously improves the decoloring effect, and can also enhance the stability of the extracting solution, thereby avoiding the introduction of ethanol in the traditional process, and solving the technical problems that the conventional water extraction method is poor in decoloring efficiency and solution stability, and is easy to become turbid and the foam performance is influenced after being added into daily chemical products. The extraction and decoloration process provided by the invention has the characteristics of simple operation, outstanding effect and stable product, and is suitable for industrial production practice.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (9)

1. A method for preparing saponin extract is characterized by comprising the following steps: comprises filtering crushed fructus Gleditsiae Abnormalis fruit body solution to obtain crude fructus Gleditsiae Abnormalis extractive solution, adding gelatin for decolorizing treatment to obtain adsorption decolorized fructus Gleditsiae Abnormalis extractive solution; adding hydrogen peroxide into the adsorbed and decolored saponin extract to perform oxidation decoloration treatment, and adding sodium chloride solid as an auxiliary agent while performing the oxidation decoloration treatment, wherein the addition amount of the sodium chloride is more than 1% of the total weight of the liquid; the addition amount of the hydrogen peroxide is 30-120% of the solid substance in the saponin extracting solution after adsorption and decoloration, and the decoloration temperature is 40-90%oAnd C, obtaining decolorized saponin extract.
2. The method for producing an extract liquid of gleditsia sinensis as claimed in claim 1, characterized in that: filtering the crushed saponin fruit body solution, dissolving the crushed seed-removed saponin fruit body in water at 40-80 DEG CoAnd C, stirring and extracting for 0.5-3 h, and filtering to obtain a crude soap horn extracting solution.
3. The method for producing an extract liquid of gleditsia sinensis as claimed in claim 2, characterized in that: the filtration is carried out by adopting a Buchner funnel and rapid qualitative filter paper for suction filtration; the crushed seed-removed saponin pod entity is dissolved in water, and the mass ratio of the seed-removed saponin pod entity to the water is 1: 5-20.
4. The method for producing an extract liquid of gleditsia sinensis as claimed in any one of claims 1 to 3, characterized in that: the gelatin is added for decoloring, and the gelatin is soaked in deionized water for 0.5 to 2 hours, then added into the crude saponin extracting solution for adsorption decoloring, and stirred at normal temperature for 0.5 to 2 hours; and filtering to remove gelatin after the decolorization treatment is finished.
5. The method for producing an extract liquid of gleditsia sinensis as claimed in any one of claims 1 to 3, characterized in that: and the gelatin is added for decoloring treatment, wherein the gelatin is added according to the proportion of 50-90% of the solid content in the crude soap horn extracting solution.
6. The method for producing an extract liquid of gleditsia sinensis as claimed in any one of claims 1 to 3, characterized in that: adding hydrogen peroxide into the adsorption-decolored saponin extract to perform oxidation-decoloration treatment, wherein the addition amount of the hydrogen peroxide is 35-50% of the mass of solids in the adsorption-decolored saponin extract; and adding the raw materials twice or more in the decoloring process; and maintaining the solution pH above 10.
7. The method for producing the saponin extract as claimed in claim 4, wherein: adding hydrogen peroxide for three times in the decoloring process to perform oxidation decoloring treatment; the total oxidation and decoloration time is 1-3 h.
8. The method for producing an extract liquid of gleditsia sinensis as claimed in any one of claims 1 to 3, characterized in that: the oxidation and decoloration treatment is carried out, wherein the temperature of the oxidation and decoloration is 50-70 DEGoC,
9. The method for producing an extract liquid of gleditsia sinensis as claimed in any one of claims 1 to 3, characterized in that: the total oxidation and decoloration time of the oxidation and decoloration treatment is 2 h.
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