CN112494402A - Iris root extract and preparation method and application thereof - Google Patents
Iris root extract and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of plant extract preparation, and discloses a preparation method of an iris root extract, which comprises the step of extracting iris roots by using a solution impregnated with an auxiliary agent, wherein the leaching auxiliary agent can promote the leaching of flavonoid compounds in the iris roots, and comprises at least one of potassium sodium tartrate, ammonium citrate, phenanthroline and 8-hydroxyquinoline. According to the method, potassium sodium tartrate, ammonium citrate, phenanthroline or 8-hydroxyquinoline are added into the extraction solvent, so that the leaching rate of flavonoid components in the iris root is effectively improved. The preparation method of the invention effectively improves the yield of the effective components in the iris root extract, improves the content of the total flavonoids, shortens the extraction time, reduces the extraction cost, and the prepared iris root extract has better antioxidation, whitening and collagenase inhibition effects and good application prospect in cosmetics.
Description
Technical Field
The invention belongs to the technical field of plant extract preparation, and particularly relates to an iris root extract and a preparation method and application thereof.
Background
Iris root is root of Iris floribunda (Iris tectorum Maxim.) of Iris of Iridaceae. Rhizoma Iridis Tectori contains abundant flavonoids, mainly contains isoflavone, and can be used for clearing away heat and toxic materials, eliminating phlegm, relieving sore throat, and relieving cough and asthma. In addition, flavonoids in iris root can generate aroma components in the cracking process, so that the flavonoid is applied to the sweet and fragrant products. For extracting effective components from rhizoma Iridis Tectori, the prior art generally adopts a single extraction method, and mostly adopts a solvent extraction method or supercritical CO2And (4) extracting. Wherein, the yield of the effective components in the extract obtained by singly adopting a solvent extraction method is lower, and the economy is not high; and supercritical CO is adopted2Although the extraction can improve the yield of the effective components in the extract to a certain extent, the cost of the method is higher.
Disclosure of Invention
In order to solve the defects in the prior art, the invention aims to provide an iris root extract and a preparation method and application thereof. The preparation method can effectively improve the yield of the effective components in the extract and reduce the extraction cost.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of an iris root extract comprises the step of extracting iris roots by using a solution containing an extraction aid, wherein the extraction aid can promote the extraction of flavonoid compounds in the iris roots, and the extraction aid comprises at least one of potassium sodium tartrate, ammonium citrate, phenanthroline and 8-hydroxyquinoline.
The inventor finds that the leaching of flavonoid components in iris root can be effectively promoted and the total flavone content in the extracted product can be remarkably improved by adding potassium sodium tartrate, ammonium citrate, phenanthroline or 8-hydroxyquinoline into the extraction solvent.
Preferably, the leaching aid comprises sodium potassium tartrate. The potassium sodium tartrate has better effect of promoting the leaching of flavonoid components in the iris root.
Preferably, the preparation method of the iris root extract comprises the following steps:
(1) pulverizing rhizoma Iridis Tectori to obtain rhizoma Iridis Tectori powder;
(2) mixing the iris root powder obtained in the step (1) with an extraction solvent containing the leaching aid, and heating and extracting;
(3) pressurizing the extraction system in the step (2), centrifuging, and taking supernatant;
(4) performing acid precipitation treatment on the supernatant obtained in the step (3), centrifuging, and taking a precipitate;
(5) drying the precipitate obtained in step (4) to obtain the iris root extract.
Preferably, the iris root is a dry root.
Preferably, the extraction solvent is an aqueous solution containing 50% to 80% ethanol. The extraction solvent has good extraction effect on Iris root.
Preferably, the amount of the extraction solvent used is 20 to 60 times of the weight of the iris root powder. With the dosage, effective components in rhizoma Iridis Tectori can be effectively extracted.
Preferably, the addition amount of the leaching aid is 0.01-0.1% of the weight of the extraction solvent. Under the addition amount, the leaching auxiliary agent can effectively promote the leaching of the flavonoid components in the iris root.
Preferably, the amount of the leaching aid added is 0.05% by weight of the extraction solvent. Under the addition amount, the auxiliary agent can effectively promote the leaching of the flavonoid components in the iris root.
Preferably, the temperature for heating and extracting is 50-70 ℃. At this temperature, effective components in Iris root can be effectively extracted.
Preferably, the pressure treatment is carried out under the condition of 50-300 MPa for 1-5 min. Under the pressure environment, the leaching of effective components in iris root plant cells can be effectively promoted.
Preferably, the acid precipitation treatment is to add a pH regulator into the supernatant to adjust the pH value to 3-6. Under the condition, effective components in the supernatant can be sufficiently precipitated.
Preferably, the acid precipitation treatment is to add a pH regulator into the supernatant to adjust the pH value to 5. Under the condition, the effective components in the supernatant can be more fully separated out, and the cost is lower.
Preferably, the pH regulator includes at least one of acetic acid, citric acid, malic acid, hydrochloric acid. The above acids can effectively precipitate the effective components in the supernatant.
More preferably, the pH adjusting agent is citric acid. The citric acid can more fully separate out effective components in the supernatant.
Preferably, the drying mode is reduced pressure drying. The reduced pressure drying is a method for drying after vacuumizing in a closed container, the temperature of the method is low, the loss of effective components in the extract in the drying process can be reduced, the adverse effect of air on the product can be reduced, and the dried product is loose and easy to crush.
The process conditions can effectively extract the effective components in the iris root, and the obtained extract has high flavone content, short time consumption, simple equipment and low cost.
In another aspect, the present invention provides an iris root extract, which is prepared by the above-described preparation method of the iris root extract of the present invention. The total flavone content of the iris root extract prepared by the preparation method is higher, more than 50 percent, and the iris root extract has better antioxidation, whitening and collagenase inhibition effects.
In another aspect, the present invention provides the use of said iris root extract in cosmetics. The iris root extract prepared by the invention has better antioxidation, whitening and collagenase inhibition effects and better skin care effects, so the iris root extract has better application prospects in cosmetics, and is particularly applied to cosmetics with the types of aging resistance, whitening and the like.
Compared with the prior art, the invention has the beneficial effects that: according to the method, potassium sodium tartrate, ammonium citrate, phenanthroline or 8-hydroxyquinoline are added into the extraction solvent, so that the leaching rate of flavonoid components in the iris root is effectively improved. The preparation method adopts a multistage extraction method, firstly adopts a solvent extraction method to extract the effective components in the iris root, then is supplemented with pressure treatment to further promote the leaching of the effective components in plant cells, and finally separates out the effective components in the extracting solution in an acid precipitation mode. The preparation method of the invention effectively improves the yield of the effective components in the iris root extract, improves the content of the total flavone, shortens the extraction time, reduces the extraction cost, simplifies the production equipment and has high economy. The iris root extract prepared by the preparation method has good antioxidation, whitening and collagenase inhibition effects, and has good application prospects in cosmetics.
Drawings
FIG. 1 is a standard curve of total flavonoids measured by colorimetric method.
Detailed Description
The technical solutions of the present invention will be further described with reference to the following embodiments, and it should be apparent that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The raw materials, reagents and the like used in the examples were all commercially available.
Example 1
A method for preparing rhizoma Iridis Tectori extract comprises the following steps:
(1) pulverizing dried root of Iris tectorum L, and sieving with 40 mesh sieve to obtain Iris tectorum L powder;
(2) adding 40 times of the rhizoma Iridis Tectori powder weight of 60% ethanol water solution, adding 0.05% potassium sodium tartrate, and extracting at 60 deg.C for 0.5 hr;
(3) pressurizing the extraction system in the step (2) to 100MPa, maintaining the pressure for 2min, instantly recovering the environmental pressure, centrifuging, and taking supernatant;
(4) adding citric acid into the supernatant obtained in the step (3) to adjust the pH value to 5, centrifuging, and taking a precipitate;
(5) and (4) drying the precipitate obtained in the step (4) under reduced pressure to obtain the iris root extract.
Example 2
A process for the preparation of an extract from iris root which differs from example 1 only in that the sodium potassium tartrate in example 1 is replaced by ammonium citrate and the other conditions are not changed.
Example 3
A process for preparing an extract of iris root, which is different from example 1 only in that sodium potassium tartrate in example 1 is replaced with phenanthroline, and other conditions are not changed.
Example 4
A process for the preparation of an extract from iris root which differs from example 1 only in that the sodium potassium tartrate in example 1 is replaced by 8-hydroxyquinoline and the other conditions are not changed.
Example 5
A method for preparing rhizoma Iridis Tectori extract comprises the following steps:
(1) pulverizing dried root of Iris tectorum L, and sieving with 40 mesh sieve to obtain Iris tectorum L powder;
(2) adding the aqueous solution containing 80% ethanol 60 times the weight of the rhizoma Iridis Tectori powder into the rhizoma Iridis Tectori powder obtained in step (1), adding 0.01% potassium sodium tartrate of the weight of the aqueous solution, and stirring at 70 deg.C for 0.5 hr;
(3) pressurizing the extraction system in the step (2) to 300MPa, maintaining the pressure for 1min, instantly recovering the environmental pressure, centrifuging, and taking supernatant;
(4) adding hydrochloric acid into the supernatant obtained in the step (3) to adjust the pH value to 3, centrifuging, and taking the precipitate;
(5) and (4) drying the precipitate obtained in the step (4) under reduced pressure to obtain the iris root extract.
Example 6
A method for preparing rhizoma Iridis Tectori extract comprises the following steps:
(1) pulverizing dried root of Iris tectorum L, and sieving with 40 mesh sieve to obtain Iris tectorum L powder;
(2) adding the aqueous solution containing 50% ethanol 20 times the weight of the rhizoma Iridis Tectori powder into the rhizoma Iridis Tectori powder obtained in step (1), adding 0.1% potassium sodium tartrate in the weight of the aqueous solution, and extracting at 50 deg.C under stirring for 0.5 hr;
(3) pressurizing the extraction system in the step (2) at 50MPa, maintaining the pressure for 5min, instantly recovering the environmental pressure, centrifuging, and taking supernatant;
(4) adding malic acid into the supernatant obtained in the step (3) to adjust the pH value to be 6, centrifuging, and taking the precipitate;
(5) and (4) drying the precipitate obtained in the step (4) under reduced pressure to obtain the iris root extract.
Comparative example 1
A method for preparing rhizoma Iridis Tectori extract comprises the following steps:
(1) pulverizing dried root of Iris tectorum L, and sieving with 40 mesh sieve to obtain Iris tectorum L powder;
(2) adding 40 times of the rhizoma Iridis Tectori powder weight of 60% ethanol water solution into rhizoma Iridis Tectori powder obtained in step (1), and extracting at 60 deg.C under stirring for 0.5 h;
(3) pressurizing the extraction system in the step (2) to 200MPa, maintaining the pressure for 5min, instantly recovering the environmental pressure, centrifuging, and taking supernatant;
(4) adding citric acid into the supernatant obtained in the step (3) to adjust the pH value to 5, centrifuging, and taking a precipitate;
(5) and (4) drying the precipitate obtained in the step (4) under reduced pressure to obtain the iris root extract.
Comparative example 2
A method for preparing rhizoma Iridis Tectori extract comprises the following steps:
(1) pulverizing dried root of Iris tectorum L, and sieving with 40 mesh sieve to obtain Iris tectorum L powder;
(2) taking the iris root powder obtained in the step (1), adding an aqueous solution containing 60% ethanol, the weight of which is 40 times that of the iris root powder, stirring and extracting at 60 ℃ for 1h, centrifuging, and taking supernate;
(3) adding citric acid into the supernatant obtained in the step (2) to adjust the pH value to be 5, centrifuging, and taking a precipitate;
(4) and (4) drying the precipitate obtained in the step (3) under reduced pressure to obtain the iris root extract.
Test examples
Firstly, determining the content of total flavonoids
The total flavone content of the iris root extracts prepared in examples 1 to 6 and comparative examples 1 to 2 was measured by a sodium nitrite-aluminum nitrate-sodium hydroxide colorimetric method. The flavone mother nucleus contains basic oxygen atom, generally has phenolic hydroxyl group, and can produce yellow complex with aluminium ion, then sodium nitrite and sodium hydroxide are added to make the solution be red in alkaline solution, and the solution has maximum absorption at 510 nm. And (4) testing the content of the total flavonoids of the iris root by using rutin as a standard substance.
The specific operation steps are as follows;
(1) placing the mixture into a 10mL test tube with a plug, and adding 2.4mL of a solution to be detected which is diluted by a certain multiple;
(2) adding 5% NaNO2Shaking and mixing 0.4mL of the solution, standing for 6min, and adding 10% Al (NO)3)30.4mL of solution is shaken and mixed evenly and is kept stand for 6 min; adding 4.0mL of 4% NaOH solution, adding water to a constant volume of 10mL, oscillating, mixing uniformly, and standing for 15 min;
(3) the absorbance was measured at 510nm with the corresponding solvent blank zeroed.
Total flavone content (mg/mL) ═ CX × 10/V) × K
Total flavone content of Iris root extract%
In the formula:
the value 10 is the test volume mL, and 0.001 is converted by unit;
CX: substituting the concentration calculated by the standard curve for the test light absorption value, mg/mL;
v: volume to aspirate sample for testing, mL;
k: is the sample dilution factor;
a is the content of total flavone, mg/mL;
b: is the total volume of the extracting solution, mL;
c: the mass of iris root extract powder, g, is used for extraction.
FIG. 1 is a standard curve of total flavonoids measured by colorimetric method.
The results of measuring the total flavone content of the iris root extracts obtained in examples 1 to 6 and comparative examples 1 to 2 are shown in table 1.
TABLE 1 Total Flavonoids content of Iris root extract
| Sample (I) | Colour of powder | Total flavone content% |
| Example 1 | Light yellow | 76.1 |
| Example 2 | Orange yellow | 65.2 |
| Example 3 | Orange yellow | 62.8 |
| Example 4 | Orange yellow | 63.1 |
| Example 5 | Yellow-brown color | 55.4 |
| Example 6 | Yellow-brown color | 63.6 |
| Comparative example 1 | Brown colour | 26.9 |
| Comparative example 2 | Brown colour | 15.3 |
As can be seen from the measurement results in table 1: in examples 1-4, the total flavone content in example 1 is the highest, which indicates that potassium sodium tartrate can better promote the leaching of total flavone in iris root. In example 1 and examples 5 to 6, the total flavone content in example 1 was the highest, which indicates that the extraction by the process of example 1 was more effective. In addition, the content of total flavonoids in comparative example 1 is remarkably reduced, which indicates that the addition of potassium sodium tartrate, ammonium citrate, phenanthroline or 8-hydroxyquinoline can effectively improve the leaching rate of flavonoid components in iris root. The total flavone content of comparative example 2 is significantly lower than that of comparative example 1, indicating that the pressure treatment is further effective in promoting the leaching of the active ingredients from iris root.
Second, testing the oxidation resistance
Examining the capability of the iris root extracts prepared in examples 1-6 and comparative examples 1-2 to remove ABTS +, ABTS is oxidized into green ABTS + under the appropriate oxidation, the generation of ABTS + is inhibited in the presence of antioxidant, and the total antioxidant capability of the sample can be measured and calculated by measuring the absorbance of ABTS at 734 nm. The iris root extracts of examples 1 to 6 and comparative examples 1 to 2 were prepared into solutions with consistent flavone content, each of which was 0.2mg/mL (flavone content/solvent), according to the following specific experimental procedures:
(1) taking a 7mmol/L ABTS solution, and diluting the ABTS solution by 50 times with 10mmol/L PBS (pH 7.4) to obtain an ABTS working solution;
(2) draw 200. mu.L ABTS working solution (or PBS), add 10uL sample solution (or PBS), shake for 10s, stand at 30 ℃ for 6min, and measure the absorbance A at 734 nm.
In the formula:
a0: no sample was added, ABTS was added;
a1: adding the sample, and adding ABTS;
a2: samples were added, no ABTS was added.
The test results are shown in table 2.
TABLE 2 Ellis extract ability to scavenge ABTS +
As can be seen from table 2, the orris root extracts of examples 1 to 6 have higher clearance rate for ABTS +, which indicates that the preparation method of the present invention can better extract flavonoid components with antioxidant ability from orris root.
Tyrosinase inhibition performance test
Tyrosinase is the rate-limiting enzyme in the melanin synthesis pathway, which affects melanin production mainly by affecting tyrosine conversion to dopa, and oxidation of dopa to dopaquinone. Therefore, the whitening efficacy of the extract can be evaluated by measuring the inhibition result of the extract on tyrosinase. The iris root extracts of examples 1 to 6 and comparative examples 1 to 2 were prepared into solutions having a uniform flavone content, each of which was 1.0mg/mL (flavone content/solvent).
The specific experimental steps are as follows:
phosphate buffer solution, test solutions with different concentration gradients (including positive control) and 500U/mL enzyme solution are sequentially added into a 96-well plate, finally 1.5mmol/L L-tyrosine is added into a substrate, timing is started immediately, and the light absorption value at the wavelength of 475nm is measured when the reaction is carried out for 20 min.
In the formula:
a: without sample addition, L-tyrosine was added
B: adding sample, adding L-tyrosine
The test results are shown in table 3.
TABLE 3 inhibitory potency of Iris root extract on tyrosinase
As can be seen from table 3, the iris root extract has inhibitory activity against tyrosinase, and can be applied to daily chemical whitening products. The iris root extracts of examples 1 to 6 have a stronger inhibitory activity on tyrosinase, which indicates that the preparation method of the present invention can obtain flavonoid components with a significant whitening effect.
Fourth, collagenase inhibition performance test
With the aging, the synthesis capacity of fibroblasts is reduced, and if the skin lacks collagen, collagen fibers are solidified, so that intercellular mucopolysaccharides are reduced, the skin loses softness, elasticity and luster, and the skin is aged. The experiment tests the inhibitory ability of iris root extract on collagenase to evaluate its anti-aging efficacy. The iris root extracts of examples 1 to 6 and comparative examples 1 to 2 were prepared into solutions having a uniform flavone content, each of which was 1.0mg/mL (flavone content/solvent).
The specific experimental steps are as follows:
incubating 50 μ L of the sample with 20 μ L of 1.1U/mLChc solution and 60 μ L of glycine buffer for 20 minutes at 37 ℃; the reaction was initiated by adding 50 μ L of FALGPA solution and for the sample blank, glycine buffer was added instead of FALGPA solution. After incubation at 37 ℃ for 30 minutes, the absorbance was measured at 335 nm.
In the formula:
a: adding the sample, adding FALGPA;
A0: sample addition, no FALGPA was added;
b, adding FALGPA without adding a sample;
B0: no sample was added, no FALGPA was added.
The test results are shown in table 4.
TABLE 4 inhibitory Activity of Iris root extract on collagenase
| Sample (I) | Inhibition rate% |
| Example 1 | 73.6 |
| Example 2 | 65.0 |
| Example 3 | 61.1 |
| Example 4 | 59.7 |
| Example 5 | 61.5 |
| Example 6 | 67.2 |
| Comparative example 1 | 46.1 |
| Comparative example 2 | 38.2 |
As can be seen from table 4, the iris root extract has collagenase inhibitory activity and can be used in anti-aging products for daily use; meanwhile, the iris root extracts prepared by different processes have different inhibition effects on collagenase, and the iris root extracts of examples 1 to 6 have stronger inhibition capability on collagenase.
The test results are combined to show that the potassium sodium tartrate is taken as the leaching aid, so that the total flavone content in the iris root extract is more favorably improved, the aggregation of brass active ingredients with antioxidant effect, whitening effect and anti-aging effect is more favorably realized, the prepared iris root extract has better antioxidant effect, whitening effect and collagenase inhibition effect,
finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the protection scope of the present invention, and although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can 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.
Claims (10)
1. The preparation method of the iris root extract is characterized by comprising the step of extracting the iris root by using a solution containing an extraction aid, wherein the extraction aid can promote the extraction of flavonoid compounds in the iris root, and the extraction aid comprises at least one of potassium sodium tartrate, ammonium citrate, phenanthroline and 8-hydroxyquinoline.
2. The method of claim 1, wherein the leaching aid comprises sodium potassium tartrate.
3. The process for the preparation of an iris root extract according to claim 1 or 2, wherein the process for the preparation of an iris root extract comprises the steps of:
(1) pulverizing rhizoma Iridis Tectori to obtain rhizoma Iridis Tectori powder;
(2) mixing the iris root powder obtained in the step (1) with an extraction solvent containing the leaching aid, and heating and extracting;
(3) pressurizing the extraction system in the step (2), centrifuging, and taking supernatant;
(4) performing acid precipitation treatment on the supernatant obtained in the step (3), centrifuging, and taking a precipitate;
(5) drying the precipitate obtained in step (4) to obtain the iris root extract.
4. The process for preparing an iris root extract of claim 3, wherein the extraction solvent is an aqueous solution containing 50% to 80% ethanol.
5. The process for preparing an iris root extract according to claim 3, wherein the extraction solvent is used in an amount of 20 to 60 times the weight of iris root powder, and the temperature for the extraction by heating is 50 to 70 ℃.
6. The process for preparing an iris root extract of claim 3, wherein the leaching aid is added in an amount of 0.01 to 0.1% by weight of the extraction solvent.
7. The process for producing an iris root extract according to claim 3, wherein the pressure treatment is carried out under a pressure of 50 to 300MPa for 1 to 5 minutes.
8. The process for preparing an iris root extract of claim 3, wherein the acid precipitation treatment is to add a pH adjusting agent to the supernatant to adjust the pH to 3 to 6; more preferably, the acid precipitation treatment is to add a pH regulator into the supernatant to adjust the pH value to 5; preferably, the pH regulator comprises at least one of acetic acid, citric acid, malic acid, hydrochloric acid; more preferably, the pH adjusting agent is citric acid.
9. An iris root extract produced by the process for producing an iris root extract as claimed in any one of claims 1 to 8.
10. The use of an iris root extract according to claim 9 in cosmetics.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114878729A (en) * | 2022-05-11 | 2022-08-09 | 云南省农业科学院花卉研究所 | Method for extracting irone and method for measuring irone content in iris root |
| WO2022256476A1 (en) * | 2021-06-04 | 2022-12-08 | Access Business Group International Llc | Orris root extracts, compositions, and methods for skin applications |
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