Extraction process and application of xanthoceraside leaf extract

Abstract

The present application relates to the field of extraction, in particular to a kind of extraction process and application of phellodendri chinensis leaf extract, the extraction process of the phellodendri chinensis leaf extract, comprising the following steps: S1, after drying phellodendri chinensis leaf, it is crushed, and phellodendri chinensis leaf powder is obtained;S2, phellodendri chinensis leaf powder obtained in step S1 is added to solvent and leached, and a mixture is obtained;S3, microwave treatment is carried out to the mixture obtained in step S2 by adding microwave-assisted absorber, filtration, washing, collecting filtrate, and drying to obtain phellodendri chinensis leaf extract.The extraction process of the present application can shorten the extraction time and has higher extraction rate.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of extraction, in particular to an extraction process of Clausia montana leaf extract and application. BACKGROUND

[0002] Clausia montana leaf is the leaf of Clausia montana, a common Chinese herbal medicine, mainly distributed in Fujian, Guangxi, Guangdong and Hainan, etc. Clausia montana leaf contains flavonoids, phenols and amino acids and other chemical components, and can be used for the prevention and treatment of influenza, epidemic cerebrospinal meningitis, malaria, and the treatment of symptoms such as cold and fever, and has good medicinal value. Therefore, the extraction of effective components in Clausia montana leaf has gradually become the research focus of the people in the field.

[0003] Patent CN104027436A discloses a preparation method of Clausia montana leaf extract. The raw material is washed, dried, and then extracted with low-carbon alcohol as the extracting agent, ultrasonic, concentrated and dried to prepare the Clausia montana leaf extract. The present application uses Clausia montana leaf as raw material, and uses ultrasonic-assisted organic solvent method to extract active ingredients of Clausia montana leaf. The preparation method of the present application is simple and short in period, and makes great contribution to the development of food preservation, natural preservative and comprehensive utilization of Clausia montana leaf, but does not study the improvement of extraction rate. Patent CN106491503A discloses an extraction method of effective components of Clausia montana leaf and its use for preparing skin cream. Cellulase and compound protease are used to make plant cell wall loose, broken and reduce mass transfer resistance, accelerate the release of flavonoids and polyphenols, and the weak alkaline small molecule group water is used to extract the effective components remaining in the residue of Clausia montana leaf, and the Clausia montana leaf extract prepared by modern biological engineering technology such as microfiltration membrane purification of the extract is rich in antioxidant components such as polyphenols and flavonoids, and antibacterial and anti-inflammatory components, and has high extraction and separation yield, and can be used for preparing skin cream, but the enzyme cannot be recycled after breaking the cell wall, and the cost is high.

[0004] Therefore, it is urgent to develop an extraction method with high extraction rate and recyclable material. SUMMARY

[0005] In view of the problems in the prior art, the present application develops an extraction process of Clausia montana leaf extract, which has a high extraction rate of more than 33%.

[0006] In order to achieve the above-mentioned purpose, the technical scheme adopted by the present application is as follows:

[0007] The present application provides an extraction process of Clausia montana leaf extract, comprising the following steps:

[0008] S1, drying and crushing Clausia montana leaf to obtain Clausia montana leaf powder;

[0009] S2, the yellow skin leaf powder obtained in step S1 is added into a solvent for leaching to obtain a mixture;

[0010] S3, a microwave-assisted absorbent is added into the mixture obtained in step S2 for microwave treatment, filtration, washing, collection of the filtrate, and drying to obtain a yellow skin leaf extract.

[0011] The present application uses microwave-assisted extraction method to extract the yellow skin leaf by adding a microwave-assisted absorbent, effectively reduces the leaching times, shortens the extraction time, and improves the extraction rate.

[0012] In some embodiments, the solvent is a mixture of 1,4-dioxane and anhydrous ethanol, and the volume ratio of the two is (0.3-0.6):1.

[0013] The present application preferably uses a mixture of 1,4-dioxane and anhydrous ethanol as the extraction solvent, and further limits the ratio of the two to improve the extraction rate of the yellow skin leaf extract, and effectively reduce the use amount of volatile toxic reagents. The possible reason is that the specific solvent ratio is more close to the polarity of the effective components in the yellow skin leaf, which is beneficial to the precipitation of the effective components in the yellow skin leaf.

[0014] In some embodiments, the mass ratio of the yellow skin leaf powder to the solvent in step S2 is 1:(15-25).

[0015] In some embodiments, the leaching temperature in step S2 is 40-50℃, and the leaching time is 1-2h.

[0016] In some embodiments, the preparation method of the microwave-assisted absorbent comprises the following steps:

[0017] (1) carbon nanotubes are soaked in a nitric acid solution for 1-2h, washed, and dried to obtain pretreated carbon nanotubes;

[0018] (2) the pretreated carbon nanotubes obtained in step (1) and silane coupling agent KH570 are added into ethanol and reacted at 50-60℃ for 5-6h, filtered, washed, and dried to obtain silane-modified carbon nanotubes;

[0019] (3) the silane-modified carbon nanotubes obtained in step (2), 2-hydroxy-4-acryloyloxy benzophenone, 1-allyl-3-vinylimidazole hexafluorophosphate, and an initiator are added into ethanol and reacted at 70-80℃ for 1-2h, filtered, washed, and dried to obtain a microwave-assisted absorbent.

[0020] The microwave-assisted extraction of effective components in plants is a simple, green and efficient method, the application improves the extraction efficiency and the precipitation of effective components by adding a microwave-assisted absorber during the microwave extraction process, the possible reasons are that the silane modified carbon nanotubes are polymerized with 2-hydroxy-4-acryloyloxy benzophenone and 1-allyl-3-vinylimidazole hexafluorophosphate, the dispersibility of the carbon nanotubes is increased, the carbon nanotubes can fully contact with the phellodendri chinensis leaf powder, the ketone groups added enhance the force with flavonoids in the phellodendri chinensis leaf extract, the precipitation of flavonoids is increased, in addition, the surface of the silane modified carbon nanotubes after the polymerization reaction has a large number of phenolic hydroxyl groups, which plays a certain antioxidant role, can reduce the oxidation of effective components in the extract during the microwave treatment process, and the imidazole groups and a large number of fluorine atoms increase the hydrogen bond interaction with phenolic and amino acid substances in the extract, further improving the extraction rate and shortening the extraction time; in addition, the crosslinking degree of the microwave-assisted absorber is increased by selecting 1-allyl-3-vinylimidazole hexafluorophosphate with multiple double bonds for polymerization reaction, the stability of the microwave-assisted absorber is increased, and the microwave-assisted absorber can be reused.

[0021] In some embodiments, the carbon nanotubes are single-walled carbon nanotubes.

[0022] In some embodiments, the mass ratio of the pretreated carbon nanotubes to the silane coupling agent KH570 in step (2) is 1:(0.8-1).

[0023] In some embodiments, the mass ratio of the silane modified carbon nanotubes, 2-hydroxy-4-acryloyloxy benzophenone and 1-allyl-3-vinylimidazole hexafluorophosphate in step (2) is 1:(0.2-0.4):(0.3-0.5).

[0024] The application specifically selects single-walled carbon nanotubes for pretreatment and limits the mass ratio of the pretreated carbon nanotubes to the silane coupling agent KH570, grafts double bonds on the surface of the pretreated carbon nanotubes, and then polymerizes with 2-hydroxy-4-acryloyloxy benzophenone and 1-allyl-3-vinylimidazole hexafluorophosphate, which can effectively improve the dispersibility of single-walled carbon nanotubes and increase the extraction rate, the possible reasons are that single-walled carbon nanotubes have a single-layer structure, the surface groups after pretreatment are more active, and the reactivity with the silane coupling agent is stronger, in addition, by limiting the mass ratio of the silane modified carbon nanotubes, 2-hydroxy-4-acryloyloxy benzophenone and 1-allyl-3-vinylimidazole hexafluorophosphate, the dispersibility of single-walled carbon nanotubes is improved, and the wave absorption property of the carbon nanotubes is not reduced.

[0025] In some embodiments, the addition amount of the microwave-assisted absorber is 0.7%-1% of the mass of the phellodendri chinensis leaf powder in step S2.

[0026] In some embodiments, the time of the microwave treatment in step S3 is 40-50 s, and the microwave power is 180-200 W.

[0027] The second aspect of the present application provides an application of the extract of the leaf of Phellodendri chinensis in a disinfectant.

[0028] Compared with the prior art, the present application has the following beneficial effects:

[0029] (1) The present application effectively reduces the extraction times, shortens the extraction time, reduces the loss of effective components in the extract, and improves the extraction rate by adding a microwave-assisted absorbent in the extraction process of the leaf of Phellodendri chinensis. The extraction rate is more than 33%.

[0030] (2) The present application increases the dispersibility of the carbon nanotubes by polymerizing the silane-modified carbon nanotubes with 2-hydroxy-4-acryloyloxybenzophenone and 1-allyl-3-vinylimidazole hexafluorophosphate, so that the carbon nanotubes can fully contact with the leaf powder of Phellodendri chinensis. In addition, the ketone group added enhances the force of the flavonoids in the extract of the leaf of Phellodendri chinensis, increases the precipitation of the flavonoids, and the silane-modified carbon nanotubes after the polymerization reaction have a large number of phenolic hydroxyl groups, which play a certain antioxidant role, can reduce the oxidation of the effective components in the extract during the microwave treatment, and the imidazole group and a large number of fluorine atoms increase the hydrogen bond interaction with the phenolic and amino acid substances in the extract, further improving the extraction rate and shortening the extraction time.

[0031] (3) The present application selects 1-allyl-3-vinylimidazole hexafluorophosphate with multiple double bonds to carry out a polymerization reaction to increase the cross-linking degree of the microwave-assisted absorbent, increase the stability of the microwave-assisted absorbent, and enable it to be reused while reducing the amount of reduction of the extraction rate. DETAILED DESCRIPTION

[0032] The present application will be described below in conjunction with specific embodiments. It should be noted that the following examples are examples of the present application and are only used to illustrate the present application, but not to limit the present application. Other combinations and various modifications within the concept of the present application can be made without departing from the spirit or scope of the present application.

[0033] In the following examples and comparative examples, the compounds and related reagents used are commercially available, and the single-walled carbon nanotubes are CNT100 purchased from Zhongke Leiming (Beijing) Technology Co., Ltd.

[0034] Preparation Example 1

[0035] The preparation method of the microwave-assisted absorbent-1 includes the following steps:

[0036] (1) 20 g of single-walled carbon nanotubes were immersed in 200 ml of a 75 wt% nitric acid solution for 1.5 h, washed, and dried to obtain pretreated carbon nanotubes;

[0037] (2) 10 g of the pretreated carbon nanotubes obtained in step (1) and 9 g of a silane coupling agent KH570 were added to 200 ml of anhydrous ethanol, and reacted at 55°C for 5.5 h. The product was filtered, washed, and dried to obtain silane-modified carbon nanotubes;

[0038] (3) 10 g of the silane-modified carbon nanotubes obtained in step (2), 3 g of 2-hydroxy-4-acryloyloxybenzophenone, 4 g of 1-allyl-3-vinylimidazolium hexafluorophosphate, and 0.02 g of azobisisobutyronitrile were added to 100 ml of anhydrous ethanol, and reacted at 75°C for 1.5 h. The product was filtered, washed, and dried to obtain microwave-assisted absorber-1.

[0039] Preparation Example 2

[0040] The preparation method of microwave-assisted absorber-2 was the same as that of Preparation Example 1, except that the amount of the silane coupling agent KH570 added was 12 g.

[0041] Preparation Example 3

[0042] The preparation method of microwave-assisted absorber-3 was the same as that of Preparation Example 1, except that the amount of 2-hydroxy-4-acryloyloxybenzophenone added was 6 g.

[0043] Preparation Example 4

[0044] The preparation method of microwave-assisted absorber-4 was the same as that of Preparation Example 1, except that the amount of 1-allyl-3-vinylimidazolium hexafluorophosphate added was 7 g.

[0045] Example 1

[0046] An extraction process of a Clausena lansium leaf extract includes the following steps:

[0047] S1, 1000 g of dried Clausena lansium leaves were crushed to obtain Clausena lansium leaf powder;

[0048] S2, 200 g of the Clausena lansium leaf powder obtained in step S1 was added to 4000 g of a solvent to extract, the solvent was a mixture of 1,4-dioxane and anhydrous ethanol, the volume ratio of the two was 0.5:1, the extraction temperature was 45°C, and the extraction time was 1.5 h to obtain a mixture;

[0049] S3, 1.6 g of microwave-assisted absorber-1 was added to 4200 g of the mixture obtained in step S2 for microwave treatment for 45 s at a microwave power of 190 W, and the filtrate was collected by filtering, washing, and drying to obtain a Clausena lansium leaf extract.

[0050] Example 2

[0051] An extraction process of a Clausena lophantthi leaf extract, comprising the following steps:

[0052] S1, 1000g of dried Clausena lophantthi leaves are crushed to obtain Clausena lophantthi leaf powder;

[0053] S2, 200g of the Clausena lophantthi leaf powder obtained in step S1 is added to 3000g of a solvent for extraction, the solvent is a mixture of 1.4-dioxane and anhydrous ethanol, the volume ratio of the two is 0.3:1, the extraction temperature is 40℃, the extraction time is 2h, and a mixture is obtained;

[0054] S3, 1.4g of microwave-assisted absorber-1 is added to 3200g of the mixture obtained in step S2 for microwave treatment for 40s, the microwave power is 180W, filtration, washing, collection of the filtrate, and drying to obtain a Clausena lophantthi leaf extract.

[0055] Example 3

[0056] S1, 1000g of dried Clausena lophantthi leaves are crushed to obtain Clausena lophantthi leaf powder;

[0057] S2, 200g of the Clausena lophantthi leaf powder obtained in step S1 is added to 5000g of a solvent for extraction, the solvent is a mixture of 1.4-dioxane and anhydrous ethanol, the volume ratio of the two is 0.6:1, the extraction temperature is 45℃, the extraction time is 55min, and a mixture is obtained;

[0058] S3, 2g of microwave-assisted absorber-1 is added to 5200g of the mixture obtained in step S2 for microwave treatment for 50s, the microwave power is 200W, filtration, washing, collection of the filtrate, and drying to obtain a Clausena lophantthi leaf extract.

[0059] Example 4

[0060] An extraction process of a Clausena lophantthi leaf extract, the specific implementation manner is the same as that of Example 1, and the difference lies in that the microwave-assisted absorber-1 is replaced by microwave-assisted absorber-2 in equal amount.

[0061] Example 5

[0062] An extraction process of a Clausena lophantthi leaf extract, the specific implementation manner is the same as that of Example 1, and the difference lies in that the microwave-assisted absorber-1 is replaced by microwave-assisted absorber-3 in equal amount.

[0063] Example 6

[0064] An extraction process of a Clausena lophantthi leaf extract, the specific implementation manner is the same as that of Example 1, and the difference lies in that the microwave-assisted absorber-1 is replaced by microwave-assisted absorber-4 in equal amount.

[0065] Example 7

[0066] An extraction process of the extract of the leaf of Phellodendri amurense Rupprecht, the same as that in Example 1, except that the microwave-assisted absorber-1 is replaced by single-walled carbon nanotubes.

[0067] Comparative Example 1

[0068] An extraction process of the extract of the leaf of Phellodendri amurense Rupprecht, comprising the following steps:

[0069] S1, 1000g of the leaf of Phellodendri amurense Rupprecht is dried and crushed to obtain leaf powder of Phellodendri amurense Rupprecht;

[0070] S2, 200g of the leaf powder of Phellodendri amurense Rupprecht obtained in step S1 is added into 4000g of a solvent for extraction, the solvent is a mixture of 1.4-dioxane and anhydrous ethanol, the volume ratio of the two is 0.5:1, the extraction temperature is 45℃, the extraction time is 1.5h, filtration, washing, collection of the filtrate, and drying to obtain the extract of the leaf of Phellodendri amurense Rupprecht.

[0071] Performance test

[0072] The extract of the leaf of Phellodendri amurense Rupprecht obtained by the extraction process of each of the above examples and the comparative example is tested as follows:

[0073] Extraction rate: the extraction rate is calculated according to the formula extraction rate = mass of the extract of the leaf of Phellodendri amurense Rupprecht / mass of the leaf powder of Phellodendri amurense Rupprecht x 100%.

[0074] The test results are shown in Table 1:

[0075] Table 1

[0076]

[0077]

[0078] It can be known from the comparison of the experimental data of Table 1 Examples 1-3 that the extract obtained by the extraction process has a high extraction rate; it can be known from the comparison of Example 4 and Example 1 that the change of the ratio of the pretreated carbon nanotubes and the silane coupling agent KH570 causes the uniformity of the microwave-assisted absorber to decrease, which affects the dispersion ability and causes the extraction rate to decrease; it can be known from the comparison of Example 5, 6 and Example 1 that the change of the ratio of the silane-modified carbon nanotubes, 2-hydroxy-4-acryloyloxybenzophenone and 1-allyl-3-vinylimidazolium hexafluorophosphate may cause the crosslinking degree to be too large, which affects the wave absorption rate and causes the extraction rate to decrease; it can be known from the comparison of Example 7 and Example 1 that the direct use of carbon nanotubes as the microwave-assisted absorber has a weak force with the effective components, which causes the extraction rate to decrease; it can be known from the comparison of Comparative Example 1 and Example 1 that the use of the ordinary method for extraction causes the effective components to be less precipitated, which results in a lower extraction rate.

[0079] 2. Circulation of the microwave-assisted extraction agent

[0080] After the microwave-assisted extraction agent-1 is recycled for 15 times, it is used in Example 1, and the extraction rate is calculated to be 34.9%, indicating that the microwave-assisted extraction agent has good recycling performance and long service life.

[0081] The above embodiments are only for illustrating the technical concept and characteristics of the present application, and the purpose is to enable those skilled in the art to understand the content of the present application and implement it, and cannot limit the protection scope of the present application. Any equivalent changes or modifications made in accordance with the spirit and essence of the present application shall be covered within the protection scope of the present application.

Claims

1. A process for the extraction of an extract from the leaves of Phellodendron amurense Rupprecht, characterized in that, The method comprises the following steps: S1, drying and crushing the leaves of Phellodendri Amurensis Rupr to obtain leaf powder of Phellodendri Amurensis Rupr; S2, adding the leaf powder of Phellodendri Amurensis Rupr obtained in step S1 into a solvent to extract, to obtain a mixture; S3, adding a microwave-assisted absorbent into the mixture obtained in step S2 to perform microwave treatment, filtering, washing, collecting the filtrate, and drying to obtain an extract of Phellodendri Amurensis Rupr; The preparation method of the microwave-assisted absorbent comprises the following steps: (1) soaking carbon nanotubes in a nitric acid solution for 1-2 h, washing, and drying to obtain pretreated carbon nanotubes; (2) adding the pretreated carbon nanotubes obtained in step (1) and silane coupling agent KH570 into ethanol, and reacting at 50-60℃ for 5-6 h, filtering, washing, and drying to obtain silane-modified carbon nanotubes; (3) adding the silane-modified carbon nanotubes obtained in step (2), 2-hydroxy-4-acryloyloxybenzophenone, 1-allyl-3-vinylimidazolium hexafluorophosphate, and an initiator into ethanol, and reacting at 70-80℃ for 1-2 h, filtering, washing, and drying to obtain the microwave-assisted absorbent; In step (2), the mass ratio of the pretreated carbon nanotubes to the silane coupling agent KH570 is 1:(0.8-1); In step (3), the mass ratio of the silane-modified carbon nanotubes, 2-hydroxy-4-acryloyloxybenzophenone, and 1-allyl-3-vinylimidazolium hexafluorophosphate is 1:(0.2-0.4):(0.3-0.5); The solvent is a mixture of 1,4-dioxane and anhydrous ethanol, and the mass ratio of the two is (0.3-0.6):

1.

2. The extraction process of the extract of the leaves of Phellodendri Chinensis according to claim 1, characterized in that, In step S2, the mass ratio of the leaf powder of Phellodendri Amurensis Rupr to the solvent is 1:(15-25).

3. The extraction process of the extract of the leaves of Phellodendri Chinensis according to claim 1, characterized in that, In step S2, the extraction temperature is 40-50℃, and the extraction time is 1-2 h.

4. The extraction process of the extract of the leaves of Phellodendri Chinensis according to claim 1, characterized in that, The addition amount of the microwave-assisted absorbent in step S3 is 0.7%-1% of the mass of the leaf powder of Phellodendri Amurensis Rupr in step S2.

5. The extraction process of the extract of the leaves of Phellodendri Chinensis according to claim 1, characterized in that, In step S3, the microwave treatment time is 40-50 s, and the microwave power is 180-200 W.

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