Efficient extraction of active components from agilawood leaves by supermolecular solvent and preparation method and application thereof

Abstract

The application discloses an active ingredient efficient extraction super-molecular solvent of Aquilaria sinensis leaves and a preparation method and application thereof, and relates to the technical field of plant extraction and chemical engineering. The preparation method comprises the following steps: mixing and dissolving amphiphilic substances containing hydrophilic groups and hydrophobic groups with water-soluble organic solvents, then adding water to form aggregates, and finally vortexing and oscillating, centrifuging to obtain supernatant, and thus obtaining the super-molecular solvent. The application has the advantages of simple operation, less pollution, high extraction efficiency, short extraction time, low cost and the like. The application overcomes the shortcomings of traditional organic solvents, such as great toxicity and environmental pollution.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of chemical engineering, and particularly relates to an active ingredient of Aquilaria sinensis leaves, a supermolecular solvent for efficiently extracting the active ingredient, and a preparation method and application thereof. BACKGROUND

[0002] Aquilaria sinensis (Lour.) Gilg belongs to the plant of Aquilaria in the family of Thymelaeaceae, and the resin-containing wood thereof is a famous traditional Chinese medicine, Aquilaria sinensis, which is an oil produced by the plant of Aquilaria in the family of Thymelaeaceae, and is famous for sinking in water and aromatic. In China, Japan, India and other Southeast Asian countries, it is not only a traditional precious medicinal material, but also a precious natural spice, and has the effects of activating qi to stop pain, warming middle to stop vomiting, and absorbing qi to relieve asthma, and is used for chest and abdominal distention and pain, stomach cold vomiting and hiccup, and kidney deficiency and asthma. It mainly distributes in southwest and south China and other places.

[0003] Aquilaria sinensis is a treasure from head to toe. With the development of the times, the utilization of Aquilaria sinensis is far from being limited to the traditional collection of Aquilaria sinensis and wood, and has developed to the comprehensive development of roots, stems, leaves, fruits and seeds. How to comprehensively utilize the resources of Aquilaria sinensis and improve the economic value is a key problem that needs to be solved for the development of Aquilaria sinensis.

[0004] It is worth noting that the resources of Aquilaria sinensis leaves are very rich, and can be collected twice a year, which is worth developing. Aquilaria sinensis leaves contain polysaccharides, amino acids, flavones and their glycosides, and phenols, and have various biological activities. The extract of Aquilaria sinensis leaves has significant anti-inflammatory, analgesic, small intestine movement promoting, purgative, hemostatic, anti-brain hypoxia-ischemia, hypoglycemic, and anti-tumor effects. Among them, these bioactive components in Aquilaria sinensis leaves are important sources of drugs and drug lead compounds, and can also be separated and purified as functional food ingredients. However, the separation process is limited by many factors, such as the type of solvent, the extraction method and condition. Usually, the active substances in most medicinal plants are extracted by organic solvents, such as ethanol, methanol, acetone and ethyl acetate. Although these organic solvents are efficient, they also have many disadvantages, such as strong volatility, high toxicity, poor biodegradability, flammability / explosiveness and high cost. SUMMARY

[0005] In view of the problems in the prior art, the present application provides a supermolecular solvent for efficiently extracting active ingredients of Aquilaria sinensis leaves, a preparation method and application thereof. By optimizing the volume ratio of different solvents of the supermolecular solvent, the best supermolecular solvent is selected, so that the extraction of the bioactive ingredients in Aquilaria sinensis leaves is optimized.

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

[0007] The present application provides a preparation method of a supermolecular solvent, comprising:

[0008] The amphiphilic substance containing hydrophilic groups and hydrophobic groups is mixed and dissolved with a water-soluble organic solvent, water is added to form an aggregate, vortex oscillation is performed, and the supernatant is obtained by centrifugation, so that the supramolecular solvent is obtained.

[0009] Preferably, the reaction raw materials and their volume percentage are as follows: 5% or 10% of the amphiphilic substance, 20% of the water-soluble organic solvent, and the balance of water.

[0010] Preferably, the amphiphilic substance is capronic acid or 1-hexanol, and the water-soluble organic solvent is tetrahydrofuran.

[0011] More preferably, the reaction raw materials and their volume percentage are as follows: 5% of capronic acid or 1-hexanol, 20% of tetrahydrofuran, and 75% of water; or 10% of 1-hexanol, 20% of tetrahydrofuran, and 70% of water.

[0012] Preferably, the rotation speed of vortex oscillation is 3000-5000 r / min, and the time is 1-3 min.

[0013] More preferably, 3 mm glass beads are further added for vortex oscillation.

[0014] Preferably, the centrifugal speed is 5000-8000 r / min, and the time is 5-10 min.

[0015] The application further provides a supramolecular solvent prepared by any of the above preparation methods.

[0016] The application further provides application of the above supramolecular solvent in efficient extraction of active ingredients of Aquilaria sinensis leaves, which comprises: vacuum freeze-drying fresh leaves of Aquilaria sinensis, crushing the leaves by a pulverizer to obtain a powder, mixing the powder with the supramolecular solvent, vortexing, then ultrasonic extraction, and obtaining a supramolecular solvent phase containing active ingredients by centrifugation and suction filtration.

[0017] Preferably, the solid-liquid ratio of the powder to the supramolecular solvent is (0.5-1):10 g / mL.

[0018] Preferably, the leaves of Aquilaria sinensis are crushed into a powder with a mesh size of 60-80.

[0019] Preferably, after mixing with the supramolecular solvent, the rotation speed of vortexing is 3000-5000 r / min, and the time is 1-3 min; and / or the ultrasonic power is 300-500 W, the ultrasonic temperature is 30-50℃, the ultrasonic time is 20-30 min; the centrifugal speed is 8000-10000 r / min, and the centrifugal time is 5-10 min.

[0020] In combination with all the above technical solutions, the application has the advantages and positive effects that several stable supermolecular solvents are screened out, the extraction time is shorter, the extraction rate is higher, the screened supermolecular solvents are safe and pollution-free, and are suitable for large-scale industrial production. The application provides a reliable method for efficient extraction of natural antioxidants in eaglewood leaves. BRIEF DESCRIPTION OF DRAWINGS

[0021] In order to more clearly illustrate the technical solutions of the embodiments of the present application, the drawings needed to be used in the embodiments of the present application will be briefly introduced as follows. Obviously, the drawings described below are only some embodiments of the present application, and other drawings can be obtained by those skilled in the art without creative labor on the basis of these drawings.

[0022] Figure 1 is a comparison diagram of total phenol content of eaglewood leaves extracted by various different supermolecular solvents provided by the embodiments of the present application.

[0023] Figure 2 is a comparison diagram of total flavonoid content of eaglewood leaves extracted by various different supermolecular solvents provided by the embodiments of the present application. DETAILED DESCRIPTION

[0024] In order to make the purpose, technical solutions and advantages of the present application more clear, the present application will be further described in detail below in combination with embodiments and drawings. It should be understood that the specific embodiments described herein are only used to explain the present application, and are not used to limit the present application.

[0025] EMBODIMENT

[0026] In this embodiment, n-hexanoic acid and n-hexanol are used as amphiphilic substances, and the extraction effect of supermolecular solvents formed by aprotic solvent tetrahydrofuran on eaglewood leaves is compared.

[0027] Table 1: Types and compositions of 18 kinds of supermolecular solvents

[0028]

[0029] Preparation method: according to the ratio in Table 1, n-hexanol or n-hexanoic acid is mixed and dissolved with tetrahydrofuran, and then water is added to form aggregates, which are vortexed at 3000 r / min (3 mm glass beads are added for vortexing) for 1 min, and then centrifuged at 6000 r / min for 5 min to obtain the supernatant, i.e. the supermolecular solvent.

[0030] TEST EXAMPLE

[0031] A batch of fresh leaves of Agarwood was vacuum freeze-dried (temperature -60℃, vacuum degree 20 Pa and time 48 h), and the powder was obtained by crushing with a pulverizer to 80 mesh. 1.0 g of the powder was mixed with 10 mL of the supramolecular solvent, and then vortexed at 5000 r / min for 3 min. Then, the supramolecular solvent phase containing active ingredients was obtained by ultrasonic extraction (ultrasonic power 360 W, ultrasonic temperature 30℃, ultrasonic time 30 min), centrifugation at 10000 r / min for 10 min and filtration.

[0032] H2O (Water), anhydrous methanol (MeOH), anhydrous ethanol (EtOH), 70% methanol (MeOH), 70% ethanol (EtOH), and ethyl acetate were used as extraction solvents, respectively. 1.0 g of the Agarwood leaf powder was added to 10 mL of the extraction solvent, vortexed at 5000 r / min for 3 min, and then extracted by ultrasonic extraction (ultrasonic power 360 W, ultrasonic temperature 30℃, ultrasonic time 30 min). The supernatant was obtained by centrifugation at 10000 r / min for 10 min.

[0033] The results are shown in Figure 1 and Figure 2 It can be clearly found that the solvents HT-1, HT-4 and CT-1 prepared according to the screened formula of the present application have significantly higher extraction efficiency than the existing solvents, and the natural antioxidants in the extracted Agarwood leaves have high antioxidant activity. See Tables 2 and 3 for details.

[0034] Table 2 Comparison of extraction efficiency of different solvents for plant active components in Agarwood leaves

[0035]

[0036] Table 3 Comparison of antioxidant activity of natural active ingredients extracted from Agarwood leaves by different extraction solvents

[0037]

[0038] The above is only a specific embodiment of the present application, but the protection scope of the present application is not limited thereto. Any modification, equivalent replacement and improvement made by those skilled in the art within the technical range disclosed in the present application, as long as it is within the spirit and principles of the present application, should be covered within the protection scope of the present application.

Claims

1. Application of a supramolecular solvent in efficient extraction of active ingredients in Aquilaria sinensis leaves, comprising: The fresh leaves of Aquilaria sinensis are vacuum freeze-dried at a temperature of-60 ℃, a vacuum degree of 20 Pa and a time of 48 h, and are crushed by a pulverizer to obtain a powder with a mesh size of 80. The powder is mixed with the supramolecular solvent, stirred at 5000 r / min for 3 min, and then extracted by ultrasonic waves at an ultrasonic power of 360 W, an ultrasonic temperature of 30 ℃ and an ultrasonic time of 30 min. The supramolecular solvent phase containing active ingredients is obtained by centrifugation at 10000 r / min for 10 min and suction filtration. The solid-liquid ratio of the powder to the supramolecular solvent is 1:10 g / mL. The supramolecular solvent is prepared by mixing n-hexanol and tetrahydrofuran, dissolving, adding water to form aggregates, stirring at 3000 r / min for 1 min, and then centrifuging at 6000 r / min for 5 min to obtain supernatant. The volume percentage of each raw material is as follows: n-hexanol 5%, tetrahydrofuran 20% and water 75%.

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