Method for extracting dogwood neoglycoside through megasonic-microwave synergy

Abstract

The invention discloses a method for extracting dogwood neoglycoside through megasonic-microwave synergy, which comprises a sound wave device, and further comprises the following steps: (1) weighing a certain amount of dogwood coarse powder, putting the dogwood coarse powder into a reaction container, adding a methanol solution with the volume fraction of 80% according to a ratio, sealing, weighing, connecting a condensing device, putting the reaction container into the sound wave device, and carrying out ultrasonic treatment for 2-3 hours; extracting for Tmin under the conditions that the ultrasonic wave F is greater than or equal to 15KHz and the megasonic wave F is greater than or equal to 1MHz to obtain an extracting solution; after the reactor is pretreated by utilizing ultrasonic waves, the reactor is positioned at a sound wave interference position under the simultaneous action of the ultrasonic waves and megasonic waves, then the sound wave frequencies are sequentially increased when the ultrasonic waves and the megasonic waves act at the same time, the sound wave interference position changes around the reactor, and the yield is controlled between 0.121% and 0.154%. And the purity is controlled between 99.3% and 99.7%.

Description

Technical Field

[0001] The invention relates to the technical field of teaching tools, in particular to a method for extracting new cornus officinalis glycosides in a megasonic-microwave collaborative manner. Background Art

[0002] The main extraction methods of cornus officinalis iridoid glycosides are Soxhlet extraction, heating reflux extraction, ultrasound-assisted extraction, microwave-assisted extraction, and the two traditional methods of Soxhlet extraction and heating reflux extraction have the disadvantages of long extraction time, low extraction rate, and easy destruction of the extract structure. Most of the iridoid glycosides are unstable in nature and are easily decomposed when exposed to acid and high temperature. Soxhlet extraction and heating reflux extraction use high-temperature condensation reflux to precipitate the raw material components, while simple ultrasound-assisted extraction can use ultrasound to generate strong vibration, cavitation and stirring to accelerate the solubility and movement speed of the substance, but the extraction time is relatively long; microwave-assisted extraction has the advantages of high selectivity and short extraction time, but its heating is uneven. Summary of the invention

[0003] The technical problem to be solved by the present invention is to solve the defects of the existing single extraction method and improve the yield.

[0004] To achieve the above object, the technical solution adopted by the present invention is:

[0005] The method for extracting new cornus officinalis glycosides by megasonic-microwave synergistic extraction comprises a sonic wave device and the following steps:

[0006] (1) Weigh a certain amount of cornus officinalis powder, place it in a reaction container, add 80% methanol solution by volume in proportion, seal it, weigh it, connect a condenser, place the reaction container in a sonic device, extract it under ultrasonic wave F ≥ 15KHz and megasonic F ≥ 1MHz for Tmin to obtain an extract;

[0007] (2) filtering the extract to obtain a filtrate, adding 80% methanol solution to the filtrate to a predetermined weight, shaking it evenly, passing it through a microporous filter membrane, concentrating and drying it, and then purifying it to obtain Cornus officinalis iridoid glycosides;

[0008] The ultrasonic wave in the middle part of step (1) is one of 20KHz≤F≤35KHz, 41KHz≤F≤55KHz, 70KHz≤F≤85KHz;

[0009] One of the megasonics 1.12MHz≤F≤1.31MHz, 2.12MHz≤F≤4.31MHz, 5.1MHz≤F≤5.5MHz;

[0010] The extraction time T ranges from 6min≤T≤15min to 2min≤T≤5min.

[0011] Furthermore, the acoustic wave device includes an acoustic wave device body, a reactor, a condenser, and a three-pronged shunt pipe. An acoustic wave generator a and an acoustic wave generator b are symmetrically arranged in the acoustic wave device body. The acoustic wave generator a emits ultrasonic waves, and the acoustic wave generator b emits megasonic waves.

[0012] The ultrasonic wave generator 5 in step (1) emits an ultrasonic wave of one of 20KHz≤F≤35KHz, 41KHz≤F≤55KHz, and 70KHz≤F≤85KHz;

[0013] The megasonic wave generator b6 has a frequency of one of 1.12 MHz ≤ F ≤ 1.31 MHz, 2.12 MHz ≤ F ≤ 4.31 MHz, and 5.1 MHz ≤ F ≤ 5.5 MHz;

[0014] The extraction time T ranges from 6min≤T≤15min to 2min≤T≤5min.

[0015] Furthermore, in step (1), the reaction container is placed in a sonic device, and the sonic generator a first operates at an ultrasonic wave F of one of 23 KHz, 27 KHz, and 30 KHz, and the time ta is maintained at 136 s, 94 s, and 66 s in sequence; then the sonic generator a and the sonic generator b work together for a time tb, wherein the ultrasonic wave emitted by the sonic generator a is gradually increased from 20 KHz to 35 KHz, and the megasonic wave emitted by the sonic generator b is gradually increased from 1.12 MHz to 1.31 MHz, and the time tb is 340 s;

[0016] Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides are 0.121%, 0.143%, and 0.143%, and the purities are 99.4%, 99.3%, and 99.3%, respectively.

[0017] Further, in step (1), the reaction container is placed in a sound wave device, and the sound wave generator a first works under an ultrasonic wave F of one of 46KHz, 49KHz, and 55KHz, and the time ta is maintained successively for 120s, 82s, and 63s; then the sound wave generator a and the sound wave generator b work together for a time tb, wherein the ultrasonic wave emitted by the sound wave generator a5 is gradually increased from 41KHz to 55KHz, and the megasonic wave emitted by the sound wave generator b6 is gradually increased from 2.12MHz to 4.31MHz, and the time tb is 230s;

[0018] Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides are 0.143%, 0.143%, and 0.165%, and the purities are 99.4%, 99.8%, and 99.3%, respectively.

[0019] Furthermore, in step (1), the reaction container is placed in a sonic device, and the sonic generator a first operates at an ultrasonic wave F of one of 72KHz, 78KHz, and 84KHz, and the time ta is maintained at 54s, 44s, and 33s in sequence; then the sonic generator a and the sonic generator b work together for a time tb, wherein the ultrasonic wave emitted by the sonic generator a is gradually increased from 70KHz to 85KHz, and the megasonic wave emitted by the sonic generator b is gradually increased from 5.1MHz to 5.5MHz, and the time tb is 77s;

[0020] Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides were 0.154%, 0.143%, and 0.121%, and the purities were 99.4%, 99.7%, and 99.3%, respectively.

[0021] Furthermore, the extract collected by the sonic generator a working alone is put into the collecting bottle a through a three-pronged shunt tube, and then the extract is introduced into the collecting bottle b when the sonic generator a and the sonic generator b work simultaneously. When extracting again, the extract in the collecting bottle a is added to the reactor to improve the yield.

[0022] Working principle and beneficial effects: The extraction method of the present invention first pre-treats the reactor with ultrasound, and then uses ultrasound and megasonic waves to act simultaneously, so that the reactor is in a sound wave interference position. When ultrasound and megasonic waves act simultaneously, the sound wave frequencies increase successively, and the sound wave interference position changes around the reactor. The yield is controlled between 0.121% and 0.154%, and the purity is controlled between 99.3% and 99.7%. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of the structure of the acoustic wave device of the present invention.

[0024] In the figure: 1. Sound wave device body; 2. Reactor; 3. Condenser; 4. Three-pronged shunt pipe; 5. Sound wave generator a; 6. Sound wave generator b. DETAILED DESCRIPTION

[0025] The present invention can be better understood with reference to the following examples.

[0026] The structures, proportions, sizes, etc. illustrated in the drawings of the specification are only used to match the contents disclosed in the specification for people familiar with this technology to understand and read, and are not used to limit the limiting conditions for the implementation of the present invention, so they have no substantial technical significance. Any modification of the structure, change of the proportional relationship, and adjustment of the size should still fall within the scope of the technical content disclosed by the present invention without affecting the effects and purposes that can be achieved by the present invention. At the same time, the terms such as "upper", "lower", "front", "back", "middle" and so on quoted in this specification are only for the convenience of description, and are not used to limit the scope of the implementation of the present invention. The changes and adjustments of their relative relationships should also be regarded as the scope of the implementation of the present invention without substantially changing the technical content.

[0027] like Figure 1 As shown,

[0028] The method for extracting new cornus officinalis glycosides by megasonic-microwave synergistic extraction comprises a sonic wave device and the following steps:

[0029] (1) Weigh a certain amount of cornus officinalis powder, place it in a reaction container, add 80% methanol solution by volume in proportion, seal it, weigh it, connect a condenser, place the reaction container in a sonic device, extract it under ultrasonic wave F ≥ 15KHz and megasonic F ≥ 1MHz for Tmin to obtain an extract;

[0030] (2) filtering the extract to obtain a filtrate, adding 80% methanol solution to the filtrate to a predetermined weight, shaking it evenly, passing it through a microporous filter membrane, concentrating and drying it, and then purifying it to obtain Cornus officinalis iridoid glycosides;

[0031] The middle ultrasonic wave of step (1) is one of 20KHz≤F≤35KHz, 41KHz≤F≤55KHz, 70KHz≤F≤85KHz;

[0032] Megasound: one of 1.12MHz≤F≤1.31MHz, 2.12MHz≤F≤4.31MHz, 5.1MHz≤F≤5.5MHz;

[0033] The extraction time T is in the range of 6min≤T≤15min and 2min≤T≤5min. The acoustic wave device comprises an acoustic wave device body 1, a reactor 2, a condenser 3, and a three-fork shunt pipe 4. An acoustic wave generator a5 and an acoustic wave generator b6 are symmetrically arranged in the acoustic wave device body 1. The acoustic wave generator a5 emits ultrasonic waves, and the acoustic wave generator b6 emits megasonic waves.

[0034] The ultrasonic wave emitted by the sound wave generator a5 in step (1) is one of 20KHz≤F≤35KHz, 41KHz≤F≤55KHz, and 70KHz≤F≤85KHz;

[0035] One of the megasonic 1.12MHz≤F≤1.31MHz, 2.12MHz≤F≤4.31MHz, 5.1MHz≤F≤5.5MHz of the sound wave generator b6;

[0036] The range of extraction time T is 6min≤T≤15min, 2min≤T≤5min.

[0037] Embodiment 1, step (1) the reaction container is placed in a sonic device, the sonic generator a5 first works under an ultrasonic wave F of one of 23KHz, 27KHz, and 30KHz, and the time ta is successively maintained at 136s, 94s, and 66s; then the sonic generator a5 and the sonic generator b6 work together for a time tb, wherein the ultrasonic wave emitted by the sonic generator a5 is gradually increased from 20KHz to 35KHz, and the megasonic wave emitted by the sonic generator b6 is gradually increased from 1.12MHz to 1.31MHz, and the time tb is 340s;

[0038] Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides are 0.121%, 0.143%, and 0.143%, and the purities are 99.4%, 99.3%, and 99.3%, respectively.

[0039] Embodiment 2, step (1) the reaction container is placed in a sonic device, the sonic generator a5 first works under an ultrasonic wave F of one of 46KHz, 49KHz, and 55KHz, and the time ta is maintained successively for 120s, 82s, and 63s; then the sonic generator a5 and the sonic generator b6 work together for a time tb, wherein the ultrasonic wave emitted by the sonic generator a5 is gradually increased from 41KHz to 55KHz, and the megasonic wave emitted by the sonic generator b6 is gradually increased from 2.12MHz to 4.31MHz, and the time tb is 230s;

[0040] Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides are 0.143%, 0.143%, and 0.165%, and the purities are 99.4%, 99.8%, and 99.3%, respectively.

[0041] Embodiment 3, step (1) the reaction container is placed in a sonic device, the sonic generator a5 first works under an ultrasonic wave F of one of 72KHz, 78KHz, and 84KHz, and the time ta is successively maintained at 54s, 44s, and 33s; then the sonic generator a5 and the sonic generator b6 work together for a time tb, wherein the ultrasonic wave emitted by the sonic generator a5 is gradually increased from 70KHz to 85KHz, and the megasonic wave emitted by the sonic generator b6 is gradually increased from 5.1MHz to 5.5MHz, and the time tb is 77s;

[0042] Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides were 0.154%, 0.143%, and 0.121%, and the purities were 99.4%, 99.7%, and 99.3%, respectively.

[0043] In Example 4, the extract collected by the sonic wave generator a5 working alone is placed into the collecting bottle a through the three-pronged shunt tube 4, and then the extract is introduced into the collecting bottle b when the sonic wave generators a5 and b6 work simultaneously. When extracting again, the extract in the collecting bottle a is added to the reactor to increase the yield.

[0044] Combining Example 1, Example 2, Example 3 and Example 4, the extraction method of the present invention first pre-treats the reactor with ultrasound, and then uses ultrasound and megasonic waves to act simultaneously, so that the reactor is in a sound wave interference position, and then when ultrasound and megasonic waves act simultaneously, the sound wave frequency increases successively, and the sound wave interference position changes around the reactor. The yield is controlled between 0.121% and 0.154%, and the purity is controlled between 99.3% and 99.7%. The yield of the prior art is controlled at 0.1%, which is much higher than the prior art. In order to further improve the yield, reference can be made to the method of Example 4.

Claims

1. A method for extracting new glycosides of Cornus officinalis by megasonic-microwave synergistic extraction, comprising a sonic device, characterized in that The following steps are involved: (1) Weigh a certain amount of cornus officinalis powder, place it in a reaction container, add 80% methanol solution by volume in proportion, seal it, weigh it, connect a condenser, place the reaction container in a sonic device, extract it under ultrasonic wave F ≥ 15KHz and megasonic F ≥ 1MHz for Tmin to obtain an extract; (2) filtering the extract to obtain a filtrate, adding 80% methanol solution to the filtrate to a predetermined weight, shaking it evenly, passing it through a microporous filter membrane, concentrating and drying it, and then purifying it to obtain Cornus officinalis iridoid glycosides; The ultrasonic wave in the middle part of step (1) is one of 20KHz≤F≤35KHz, 41KHz≤F≤55KHz, 70KHz≤F≤85KHz; One of the megasonics 1.12MHz≤F≤1.31MHz, 2.12MHz≤F≤4.31MHz, 5.1MHz≤F≤5.5MHz; The extraction time T ranges from 6min≤T≤15min to 2min≤T≤5min.

2. The method for extracting new Cornus officinalis glycosides by megasonic-microwave synergistic extraction according to claim 1, characterized in that: The acoustic wave device comprises an acoustic wave device body (1), a reactor (2), a condenser (3), and a three-pronged shunt pipe (4). An acoustic wave generator a (5) and an acoustic wave generator b (6) are symmetrically arranged in the acoustic wave device body (1). The acoustic wave generator a (5) emits ultrasonic waves, and the acoustic wave generator b (6) emits megasonic waves. The ultrasonic wave generator a (5) in step (1) emits an ultrasonic wave of one of 20KHz≤F≤35KHz, 41KHz≤F≤55KHz, and 70KHz≤F≤85KHz; The megasonic wave generator b (6) has a frequency of one of 1.12 MHz ≤ F ≤ 1.31 MHz, 2.12 MHz ≤ F ≤ 4.31 MHz, and 5.1 MHz ≤ F ≤ 5.5 MHz; The extraction time T ranges from 6min≤T≤15min to 2min≤T≤5min.

3. The method for extracting new Cornus officinalis glycosides by megasonic-microwave synergistic extraction according to claim 2, characterized in that: Step (1) The reaction container is placed in a sound wave device, and the sound wave generator a (5) first works under an ultrasonic wave F of one of 23KHz, 27KHz and 30KHz, and the time ta is maintained at 136s, 94s and 66s in sequence; then the sound wave generator a (5) and the sound wave generator b (6) work together for a time tb, wherein the ultrasonic wave emitted by the sound wave generator a (5) is gradually increased from 20KHz to 35KHz, and the megasonic wave of the sound wave generator b (6) is gradually increased from 1.12MHz to 1.31MHz, and the time tb is 340s; Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides are 0.121%, 0.143%, and 0.143%, and the purities are 99.4%, 99.3%, and 99.3%, respectively.

4. The method for extracting new Cornus officinalis glycosides by megasonic-microwave synergistic extraction according to claim 2, characterized in that: Step (1) The reaction container is placed in a sound wave device, and the sound wave generator a (5) first works under an ultrasonic wave F of one of 46KHz, 49KHz and 55KHz, and the time ta is maintained at 120s, 82s and 63s in sequence; then the sound wave generator a (5) and the sound wave generator b (6) work together for a time tb, wherein the ultrasonic wave emitted by the sound wave generator a (5) is gradually increased from 41KHz to 55KHz, and the megasonic wave of the sound wave generator b (6) is gradually increased from 2.12MHz to 4.31MHz, and the time tb is 230s; Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides are 0.143%, 0.143%, and 0.165%, and the purities are 99.4%, 99.8%, and 99.3%, respectively.

5. The method for extracting new Cornus officinalis glycosides by megasonic-microwave synergistic extraction according to claim 2, characterized in that: Step (1) The reaction container is placed in a sound wave device, and the sound wave generator a (5) first works under an ultrasonic wave F of one of 72KHz, 78KHz, and 84KHz, and the time ta is maintained at 54s, 44s, and 33s in sequence; then the sound wave generator a (5) and the sound wave generator b (6) work together for a time tb, wherein the ultrasonic wave emitted by the sound wave generator a (5) is gradually increased from 70KHz to 85KHz, and the megasonic wave of the sound wave generator b (6) is gradually increased from 5.1MHz to 5.5MHz, and the time tb is 77s; Among them, T=ta+tb, and the yields of the obtained new Cornus officinalis glycosides were 0.154%, 0.143%, and 0.121%, and the purities were 99.4%, 99.7%, and 99.3%, respectively.

6. The method for extracting new glycosides of Cornus officinalis by megasonic-microwave synergistic extraction according to any one of claims 3, 4 and 5, characterized in that: The extract collected by the sonic wave generator a (5) working alone is placed into the collection bottle a through the three-pronged shunt tube (4), and then the extract is introduced into the collection bottle b when the sonic wave generator a (5) and the sonic wave generator b (6) work simultaneously. When extracting again, the extract in the collection bottle a is added to the reactor to improve the yield.

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