Extraction method and application of peony root bark extract with soothing effect
By regulating the moisture content of peony root crust and using soaking, ultrasonic soaking and multiple increase of ethanol at multiple temperatures, the problem of poor extraction effect when ethanol is used in combination with other solvents is solved, and efficient extraction of calcium is achieved, improving the quality and efficacy of the extract.
Patent Information
- Application Number
- CN202510138788.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-02-08
- Publication Date
- 2025-03-07
AI Technical Summary
In the prior art, when ethanol is used in combination with other solvents, the extraction effect of ethanol on the calcium phenol in the root crust of peony is affected, resulting in poor extraction effect.
By regulating the moisture content of the peony root crust, combining soaking at multiple temperatures, ultrasonic soaking and multiple increase in ethanol, the contact surface and contact time between ethanol and peony root crust can be expanded to fully utilize ethanol to extract pyraphenol.
The extraction rate and extraction quality of saccharin in peony root extract is improved, highlighting the soothing effect of peony root extract and avoiding the loss of saccharin.
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Figure CN119564565A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of peony root bark extraction, and more specifically, to an extraction method and application of a peony root bark extract with soothing effect. Background Art
[0002] In the process of extracting peony root bark, ethanol is used to extract valuable ingredients in peony root bark (such as paeonol, which has analgesic, anti-inflammatory, antipyretic and anti-allergic effects; it has obvious analgesic effects on pain caused by physical or chemical factors such as tail compression and acetic acid); however, in the process of using ethanol, it may be combined with other solvents, which will affect the extraction of paeonol from peony root bark by ethanol, resulting in the inability to fully utilize ethanol to extract paeonol, and the paeonol locking extraction effect is poor. For example, in the prior art, "A peony root bark extract antibacterial bursting beads and its preparation method and application, application number 202210655931.X", the extraction method of "peony root bark extract" recorded therein mentions the situation of combining with ethyl acetate during the use of ethanol; that is, there is a situation that affects the extraction of paeonol from peony root bark by ethanol.
[0003] Therefore, an extraction method and application of a peony root bark extract with soothing effect are proposed to solve the above problems. Summary of the invention
[0004] The purpose of the present invention is to solve the shortcomings existing in the prior art: in the process of extracting peony root bark, ethanol is used to extract valuable components in the peony root bark, but in the process of using ethanol, it may be combined with other solvents, which will affect the extraction of ethanol from the paeonol component in the peony root bark, resulting in the inability to fully utilize ethanol to extract paeonol, and the paeonol locking extraction effect is poor, and the proposed peony root bark extract with soothing effect The extraction method and application are provided.
[0005] The specific technical scheme is: a method for extracting peony root bark extract with soothing effect, comprising the following steps: Step 1: Pretreatment of Peony Root Bark Clean the peony root bark, lay it flat in a 10-20 ℃ environment, and then let dry air with a temperature of 10-20 ℃ pass through it at a wind speed of 5.5-10.7 m / s to dry the peony root bark in the shade; then control the water content of the peony root bark to 5-10%; Step 2: Prepare peony root bark solution S1, crushing the root bark of Paeonia suffruticosa and grinding it into a powder of 80-120 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking at a temperature of 30-50°C for 20-30 min to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 1-3 g: 15-20 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 100-120 KHz and 50-80 W, raising the temperature of the mixed solution 1 by 60-70 °C, and placing it for 10-25 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 1-3:7-9 under stirring to obtain a mixed solution 2; S4, placing the mixed solution 2 in an ultrasonic environment of 90-100 KHz and 50-80 W, and adjusting the temperature to 30-50 °C; Therefore, the water content of the peony root bark itself is first regulated to cooperate with the subsequent simple use of ethanol to reduce the impact on the ethanol concentration; by soaking at various temperatures, ultrasonic soaking and multiple additions of ethanol, the contact is expanded, and the ethanol is fully utilized through appropriate temperature, contact surface and contact time, so as to lock the paeonol in the peony root bark extract to the greatest extent, improve the extraction rate and extraction quality of the peony root bark extract, highlight the soothing effect of the peony root bark extract, and avoid the loss of paeonol in the peony root bark extract; Step 3: Water bath reflux extraction S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 1-3:2-4; S2, stirring the deionized water and the mixed solution 2 at a stirring speed of 60-90 r / min, adding the mixture to a water bath reflux extraction system after stirring for 10-20 min, and performing water bath reflux extraction to obtain an oil-water mixture; Step 4: Let the oil-water mixture stand to obtain crystals, and leave the crystals to obtain the peony root bark extract.
[0006] The detailed technical scheme of the present invention is that in step 1, the peony root bark is pretreated, the peony root bark is cleaned, spread flat and placed in a temperature environment of 18°C, and then dry air with a temperature of 18°C is introduced at a wind speed of 8.7 m / s to dry the peony root bark in the shade; the water content of the peony root bark is controlled at 8%.
[0007] The detailed technical scheme of the present invention comprises the following steps in step 2 of preparing the peony root bark solution: S1, crushing the root bark of Paeonia suffruticosa and grinding it into a powder of 110 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking at a temperature of 45°C for 28 minutes to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 2 g:17 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 110 KHz and 68 W, raising the temperature of the mixed solution 1 by 62°C, and placing it for 22 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 2:5 under stirring to obtain a mixed solution 2; S4. Place the mixed solution 2 in an ultrasonic environment of 198 kHz and 60 W, and adjust the temperature to 40 °C.
[0008] The detailed technical solution of the present invention is that in step 2 of preparing the peony root bark solution, the purity of ethanol is 95%.
[0009] The detailed technical solution of the present invention is that in step S3 of preparing the peony root bark solution in step 2, ethanol is continuously added to the mixed solution 1 under a stirring environment with a rotation speed of 200 r / min and a temperature of 50°C.
[0010] The detailed technical scheme of the present invention comprises the following steps in step three, water bath reflux extraction: S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 2:3; S2. Stir the deionized water and the mixed solution 2 at a stirring speed of 80 r / min. After stirring for 18 min, add the mixture into a water bath reflux extraction system to perform water bath reflux extraction to obtain the oil-water mixture.
[0011] The detailed technical solution of the present invention, the water bath reflux extraction system comprises: A sealing top cover, wherein the sealing top cover is provided with a material injection pipe at the top thereof, and a sealing cover is provided on the material injection pipe; the material injection pipe is used to add materials; A heat exchange shell, wherein the heat exchange shell is detachably mounted on the bottom of the sealing top cover; A heat-conducting base, which is mounted on the bottom of the heat exchange shell; an open groove is provided at the bottom of the heat exchange shell to cooperate with the heat-conducting base, and the heat-conducting base is detachably mounted on the open groove; Wherein, the heat-conducting base is provided with a heat-exchange surface expansion structure inside the heat-exchange shell; the heat-exchange surface expansion structure is used to increase the contact surface between the heat source in the hot water bath and the material inside the heat-conducting base.
[0012] Furthermore, the heat-conducting base is provided with sealing ridges around the heat exchange surface extension structure, and the sealing ridges are used for sealing during the detachable installation process of the heat exchange shell and the heat-conducting base; The heat exchange surface extension structure includes: A main heat conducting plate, wherein the main heat conducting plate is provided with a plurality of material penetration ports on its main body, and a material passage cavity is provided inside its main body; the material passage cavity is connected to a hot water inlet provided on the heat conducting base; A plurality of unit heat exchange elements are arranged in an array on the main heat-conducting plate, and the unit heat exchange elements are connected to the material-passing cavity.
[0013] Therefore, after the heat-conducting base is detachably installed inside the heat exchange shell, the material is added into the heat-conducting base and placed in a hot water bath for reflux extraction; the material will enter the heat exchange surface extension structure installed on the heat-conducting base inside the heat exchange shell. The heat exchange surface extension structure uses a main heat-conducting plate and multiple unit heat exchange elements to protrude into the heat exchange shell, thereby expanding the contact surface between the heat source in the hot water bath and the material inside the heat-conducting base, which is beneficial to promote the comprehensive and balanced contact of the material with the heat source, and improve the efficiency and quality of water bath reflux extraction.
[0014] Furthermore, the unit heat exchange element includes: A heat conducting plate, the heat conducting plate is mounted on the main heat conducting plate, and a secondary material passage cavity is opened inside the heat conducting plate; the secondary material passage cavity is connected to the material passage cavity; A plurality of side heat-conducting telescopic plates, wherein the plurality of side heat-conducting telescopic plates are evenly spaced and distributed on the heat-conducting plate; The side heat-conducting telescopic plate includes a heat-conducting insertion plate and a heat-conducting outer sleeve movably mounted on the heat-conducting insertion plate; a material-conducting cavity is provided inside the heat-conducting insertion plate, and a partition is fixed at the center of the material-conducting cavity, and the partition divides the material-conducting cavity into an inlet channel and a water outlet channel; The partition is inserted into the secondary material passage cavity to separate the secondary material passage cavity, and the inlet channel and the water outlet channel are respectively connected at both ends of the partition; the partition is inserted into the interior of the thermal conductive jacket at the end away from the secondary material passage cavity; the thermal conductive jacket is fixed with a flushing guide plate on its inner wall, and a wedge-shaped surface is provided on the flushing guide plate.
[0015] Therefore, in the process of the heat exchange surface expansion structure using the main heat exchange plate and multiple unit heat exchange elements protruding into the heat exchange shell, the heat source in the hot water bath first enters the secondary feed cavity inside the heat conduction plate through the internal feed cavity of the main heat exchange plate in turn, and then enters the inside of the entry channel through one side of the secondary feed cavity partition, enters the heat conduction jacket along the entry channel, enters the inside of the water outlet channel, enters the secondary feed cavity along the water outlet channel, and finally is discharged through the conduit connecting the secondary feed cavity with the outside world; the heat source is realized to be quickly and comprehensively exchanged when it flows rapidly in the feed cavity, the secondary feed cavity, the entry channel and the water outlet channel, thereby improving the efficiency and quality of water bath reflux extraction; When the heat source flows into the channel, it will use the wedge-shaped surface on the flushing guide plate to push the heat-conducting jacket to slide and expand on the heat-conducting insertion plate, so as to adjust the exchange surface of the heat source by flexibly adjusting the flow rate of the heat source.
[0016] Another object of the present invention is to provide an application of a method for extracting a peony root bark extract having a soothing effect, comprising extracting the extract from the whole herb of the Asclepiadaceae plant Cynanchum wilfordii.
[0017] Compared with the prior art, the present invention can achieve: First, by regulating the water content of the root bark of peony root, it is used to cooperate with the subsequent use of ethanol alone to reduce the impact on the concentration of ethanol; by soaking at various temperatures, ultrasonic soaking and adding ethanol multiple times, the contact is expanded, and the ethanol is fully utilized through the appropriate temperature, contact surface and contact time, so as to lock the paeonol to the greatest extent, improve the extraction rate and extraction quality, highlight the soothing effect, and avoid the loss of paeonol; 2. After the heat-conducting base is detachably installed inside the heat exchange shell, the material is added into the heat-conducting base and placed in a hot water bath for water bath reflux extraction; the material will enter the heat exchange surface extension structure installed inside the heat exchange shell of the heat-conducting base. The heat exchange surface extension structure uses a main heat plate and multiple unit heat exchange components to protrude into the heat exchange shell, expanding the contact surface between the heat source in the hot water bath and the material inside the heat-conducting base, which is conducive to promoting the comprehensive and balanced contact of the material with the heat source, and improving the efficiency and quality of water bath reflux extraction; 3. In the process of using the main heat exchange plate and multiple unit heat exchange elements to protrude into the heat exchange shell in the heat exchange surface expansion structure, the heat source in the hot water bath first enters the secondary feed cavity inside the heat conduction plate through the internal feed cavity of the main heat exchange plate in turn, and then enters the inside of the entry channel through one side of the secondary feed cavity partition, enters the heat conduction jacket along the entry channel, enters the inside of the water outlet channel, enters the secondary feed cavity along the water outlet channel, and finally is discharged through the conduit connecting the secondary feed cavity with the outside world; the heat source is realized to be quickly and comprehensively exchanged when it flows rapidly in the feed cavity, the secondary feed cavity, the entry channel and the water outlet channel, thereby improving the efficiency and quality of water bath reflux extraction; When the heat source flows into the channel, it will use the wedge-shaped surface on the flushing guide plate to push the heat-conducting jacket to slide and expand on the heat-conducting insertion plate, so as to adjust the exchange surface of the heat source by flexibly adjusting the flow rate of the heat source. BRIEF DESCRIPTION OF THE DRAWINGS
[0018] Figure 1 The HPLC spectrum of paeonol in Experimental Example 1 completely relies on the extraction method specifically provided in Example 6; Figure 2 HPLC spectrum of paeonol obtained in Comparative Example 1 by adding deionized water first and then ethanol, and then completely relying on the extraction method specifically provided in Example 6; Figure 3 This is the HPLC spectrum of paeonol obtained in Comparative Example 2 after adding ethanol only three times discontinuously and completely relying on the extraction method specifically provided in Example 6; Figure 4 This is the HPLC spectrum of paeonol in Comparative Example 3, which is obtained by completely relying on the extraction method specifically provided in Example 6 without adjusting the temperature of ethanol; Figure 5It is a schematic diagram of the structure of the water bath reflux extraction system in the present invention; Figure 6 for Figure 5 Schematic diagram of the structure of the medium heat-conducting base; Figure 7 for Figure 6 A schematic diagram of the structure of the heat exchange element in the middle unit; Figure 8 for Figure 7 Schematic diagram of the transverse cross-sectional structure of the middle unit heat exchange element.
[0019] In the reference numerals: Sealing top cover 100, injection pipe 110; heat exchange shell 200, heat conductive base 300, sealing convex edge 310, main heat transfer plate 320, material penetration port 330, unit heat exchange element 340; heat conductive plate 341, side heat conductive expansion plate 342; hot water inlet 400; heat conductive jacket 3421, heat conductive insertion plate 3422, inlet channel 3423, partition 3424, water outlet channel 3425, flushing guide plate 3426. DETAILED DESCRIPTION
[0020] In order to make the purpose, technical scheme and advantages of the present invention clearer, the present invention is further described in detail below in conjunction with specific embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the present invention.
[0021] It is necessary to explain in advance that: 1. Peony root bark comes from Bozhou, Anhui; 2. The equipment used to dry the air is: adsorption compressed air dryer (AD-850Q heatless regeneration adsorption compressed air dryer, produced by Hangzhou Xinlong Purification Equipment Co., Ltd., model AD-850Q); 3. The equipment used to grind the peony root bark into powder is: a three-head grinder (XPM120*3 laboratory three-head grinder, produced by Jiangxi Longzhong Machinery Equipment Co., Ltd., model XPM120*3); 4. The equipment used for mixing peony root bark powder and ethanol is: a three-dimensional mixer (deyue, produced by Shanghai Deyue Powder Machinery Co., Ltd., model DWH-100 three-dimensional mixer); 5. The equipment used for ultrasound is: Ultrasonic micro-high pressure reactor (produced by Beijing Century Senlang Experimental Instrument Co., Ltd.).
[0022] Example 1
[0023] A method for extracting a peony root bark extract having a soothing effect comprises the following steps: Step 1: Pretreatment of Peony Root Bark The peony root bark was cleaned, spread flat in a 10 ℃ environment, and then dry in the shade with 10 ℃ dry air at a wind speed of 5.5 m / s; the water content of the peony root bark was controlled at 5%; Step 2: Prepare peony root bark solution S1, crushing the root bark of Paeonia suffruticosa and grinding it into a powder of 80 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking at a temperature of 30°C for 20 minutes to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 1 g:15 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 100 kHz and 50 W, raising the temperature of the mixed solution 1 by 60°C, and leaving it for 10 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 1:7 under stirring to obtain a mixed solution 2; S4, placing the mixed solution 2 in an ultrasonic environment of 90 kHz and 50 W, and adjusting the temperature to 30 °C; Therefore, the water content of the peony root bark itself is first regulated to cooperate with the subsequent simple use of ethanol to reduce the impact on the ethanol concentration; by soaking at various temperatures, ultrasonic soaking and multiple additions of ethanol, the contact is expanded, and the ethanol is fully utilized through appropriate temperature, contact surface and contact time, so as to lock the paeonol in the peony root bark extract to the greatest extent, improve the extraction rate and extraction quality of the peony root bark extract, highlight the soothing effect of the peony root bark extract, and avoid the loss of paeonol in the peony root bark extract; Step 3: Water bath reflux extraction S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 1:2; S2, stirring the deionized water and the mixed solution 2 at a stirring speed of 60 r / min, adding the mixture into a water bath reflux extraction system after stirring for 10 min, and performing water bath reflux extraction to obtain an oil-water mixture; Step 4: Let the oil-water mixture stand to obtain crystals, and leave the crystals to obtain the peony root bark extract.
[0024] Furthermore, in step 2 of preparing the peony root bark solution, the purity of ethanol is 95%. In step S3 of step 2 of preparing the peony root bark solution, ethanol is continuously added to the mixed solution 1 under a stirring environment at a speed of 200 r / min and a temperature of 50°C.
[0025] Example 2
[0026] A method for extracting a peony root bark extract having a soothing effect comprises the following steps: Step 1: Pretreatment of Peony Root Bark The peony root bark was cleaned, laid flat in a 20 ℃ environment, and then dry air at 20 ℃ was introduced at a wind speed of 10.7 m / s to dry the peony root bark in the shade; the water content of the peony root bark was controlled at 10%; Step 2: Prepare peony root bark solution S1, crushing the root bark of Paeonia suffruticosa and grinding it into a powder of 120 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking for 30 min at a temperature of 30-50 °C to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 3 g: 20 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 120 KHz and 80 W, raising the temperature of the mixed solution 1 by 70°C, and leaving it for 25 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 3:9 under stirring to obtain a mixed solution 2; S4, placing the mixed solution 2 in an ultrasonic environment of 100 kHz and 80 W, and adjusting the temperature to 50 °C; Step 3: Water bath reflux extraction S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 3:4; S2, stirring the deionized water and the mixed solution 2 at a stirring speed of 90 r / min, adding the mixture into a water bath reflux extraction system after stirring for 20 min, and performing water bath reflux extraction to obtain an oil-water mixture; Step 4: Let the oil-water mixture stand to obtain crystals, and leave the crystals to obtain the peony root bark extract.
[0027] Example 3
[0028] The difference between this embodiment and embodiment 1 is only that: In step 1, pretreatment of peony root bark, the peony root bark is cleaned, spread flat in an environment with a temperature of 18°C, and then dry air with a temperature of 18°C is introduced at a wind speed of 8.7 m / s to dry the peony root bark in the shade; the water content of the peony root bark is controlled at 8%.
[0029] Example 4
[0030] The difference between this embodiment and embodiment 1 is only that: In step 2, preparing the peony root bark solution, the following steps are included: S1, crushing the root bark of Paeonia suffruticosa and grinding it into a powder of 110 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking at a temperature of 45°C for 28 minutes to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 2 g:17 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 110 KHz and 68 W, raising the temperature of the mixed solution 1 by 62°C, and placing it for 22 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 2:5 under stirring to obtain a mixed solution 2; S4. Place the mixed solution 2 in an ultrasonic environment of 198 kHz and 60 W, and adjust the temperature to 40 °C.
[0031] Example 5
[0032] The difference between this embodiment and embodiment 1 is only that: In step three, water bath reflux extraction, the following steps are included: S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 2:3; S2. Stir the deionized water and the mixed solution 2 at a stirring speed of 80 r / min. After stirring for 18 min, add the mixture into a water bath reflux extraction system to perform water bath reflux extraction to obtain the oil-water mixture.
[0033] Example 6
[0034] A method for extracting a peony root bark extract having a soothing effect comprises the following steps: Step 1: Pretreatment of Peony Root Bark The peony root bark was cleaned, spread flat in an environment with a temperature of 18 ℃, and then dry in the shade with dry air at a temperature of 18 ℃ at a wind speed of 8.7 m / s; the water content of the peony root bark was controlled at 8%; Step 2: Prepare peony root bark solution S1, crushing the root bark of Paeonia suffruticosa and grinding it into a powder of 110 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking at a temperature of 45°C for 28 minutes to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 2 g:17 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 110 KHz and 68 W, raising the temperature of the mixed solution 1 by 62°C, and placing it for 22 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 2:5 under stirring to obtain a mixed solution 2; S4, placing the mixed solution 2 in an ultrasonic environment of 198 kHz and 60 W, and adjusting the temperature to 40 °C; Therefore, the water content of the peony root bark itself is first regulated to cooperate with the subsequent simple use of ethanol to reduce the impact on the ethanol concentration; by soaking at various temperatures, ultrasonic soaking and multiple additions of ethanol, the contact is expanded, and the ethanol is fully utilized through appropriate temperature, contact surface and contact time, so as to lock the paeonol in the peony root bark extract to the greatest extent, improve the extraction rate and extraction quality of the peony root bark extract, highlight the soothing effect of the peony root bark extract, and avoid the loss of paeonol in the peony root bark extract; Step 3: Water bath reflux extraction S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 2:3; S2, stirring the deionized water and the mixed solution 2 at a stirring speed of 80 r / min, and after stirring for 18 min, adding the mixture into a water bath reflux extraction system to perform water bath reflux extraction to obtain the oil-water mixture; Step 4: Let the oil-water mixture stand to obtain crystals, and leave the crystals to obtain the peony root bark extract.
[0035] Furthermore, in step 2 of preparing the peony root bark solution, the purity of ethanol is 95%. In step S3 of step 2 of preparing the peony root bark solution, ethanol is continuously added to the mixed solution 1 under a stirring environment at a speed of 200 r / min and a temperature of 50°C.
[0036] Example 7 For details, see Figure 5 and Figure 6 : The water bath reflux extraction system comprises: A sealing top cover 100, wherein the sealing top cover 100 is provided with a material injection pipe 110 at the top thereof, and a sealing cover is provided on the material injection pipe 110; the material injection pipe 110 is used to add materials; A heat exchange shell 200, wherein the heat exchange shell 200 is detachably mounted on the bottom of the sealing top cover 100; A heat-conducting base 300, wherein the heat-conducting base 300 is mounted on the bottom of the heat exchange shell 200; an opening groove is formed at the bottom of the heat exchange shell 200 to cooperate with the heat-conducting base 300, and the heat-conducting base 300 is detachably mounted on the opening groove; The heat-conducting base 300 is provided with a heat-exchange surface extension structure inside the heat-exchange shell 200 ; the heat-exchange surface extension structure is used to increase the contact surface between the heat source in the hot water bath and the material inside the heat-conducting base 300 .
[0037] For further details, see Figure 6 and Figure 7: The heat-conducting base 300 is provided with a sealing ridge 310 around the heat exchange surface extension structure, and the sealing ridge 310 is used for sealing during the detachable installation process of the heat exchange shell 200 and the heat-conducting base 300; The heat exchange surface extension structure includes: A main heat conducting plate 320, wherein the main heat conducting plate 320 has a plurality of material penetration ports 330 formed on its main body, and a material passage cavity formed inside its main body; the material passage cavity is connected to a hot water inlet 400 formed on the heat conducting base 300; A plurality of unit heat exchange elements 340 are arranged in an array on the main heat-dissipating plate 320 , and the unit heat exchange elements 340 are connected to the material-passing cavity.
[0038] Therefore, after the heat-conducting base 300 is detachably installed inside the heat exchange shell 200, the material is added into the heat-conducting base 300 and placed in a hot water bath for water bath reflux extraction; the material will enter the heat exchange surface extension structure installed on the heat-conducting base 300 inside the heat exchange shell 200. The heat exchange surface extension structure uses a main heat-conducting plate 320 and a plurality of unit heat exchange elements 340 to protrude into the heat exchange shell 200, thereby expanding the contact surface between the heat source in the hot water bath and the material inside the heat-conducting base 300, which is beneficial to promote the comprehensive and balanced contact of the material with the heat source, and improve the efficiency and quality of water bath reflux extraction.
[0039] For further details, see Figure 7 and Figure 8 The unit heat exchange element 340 includes: A heat conducting plate 341, wherein the heat conducting plate 341 is mounted on the main heat conducting plate 320, and a secondary material passage cavity is formed inside the heat conducting plate 341; the secondary material passage cavity is connected to the material passage cavity; A plurality of side heat-conducting retractable plates 342 , wherein the plurality of side heat-conducting retractable plates 342 are evenly spaced and distributed on the heat-conducting plate 341 ; The side heat-conducting expansion plate 342 includes a heat-conducting insertion plate 3422 and a heat-conducting outer sleeve 3421 movably mounted on the heat-conducting insertion plate 3422; a material-conducting cavity is provided inside the heat-conducting insertion plate 3422, and a partition 3424 is fixed at the center of the material-conducting cavity, and the partition 3424 divides the material-conducting cavity into an inlet channel 3423 and a water outlet channel 3425; The partition 3424 is inserted into the secondary material passage cavity to separate the secondary material passage cavity, and the inlet channel 3423 and the water outlet channel 3425 are respectively connected at both ends of the partition; the partition 3424 is inserted into the interior of the thermal conductive jacket 3421 at the end away from the secondary material passage cavity; the thermal conductive jacket 3421 is fixed with a flushing guide plate 3426 on the inner wall thereof, and the flushing guide plate 3426 is provided with a wedge-shaped surface.
[0040] Therefore, in the process of the heat exchange surface expansion structure using the main heat exchange plate 320 and multiple unit heat exchange elements 340 protruding into the heat exchange shell 200, the heat source in the hot water bath first passes through the internal feed cavity of the main heat exchange plate 320 and enters the secondary feed cavity inside the heat conductive plate 341 in sequence, and then enters the inside of the entry channel 3423 through one side of the secondary feed cavity partition, enters the heat conductive jacket 3421 along the entry channel 3423, and then enters the inside of the water outlet channel 3425, and then enters the secondary feed cavity along the water outlet channel 3425, and finally is discharged through the conduit that connects the secondary feed cavity with the outside world; the heat source is realized to be quickly and comprehensively exchanged when it flows rapidly in the feed cavity, the secondary feed cavity, the entry channel 3423 and the water outlet channel 3425, thereby improving the efficiency and quality of water bath reflux extraction; When the heat source flows into the channel 3423, the wedge-shaped surface on the flushing guide plate 3426 is used to push the heat-conducting jacket 3421 to slide and expand on the heat-conducting insertion plate 3422, so as to adjust the exchange surface of the heat source by flexibly adjusting the flow rate of the heat source.
[0041] Experimental Example 1 Weigh 500 g of peony root bark, prepare a peony root bark extract based on the extraction method specifically provided in Example 6, add α-amylase, glucose oxidase and 500 mL of ethanol to the peony root bark extract, put it into a water bath reflux extraction system, collect the distillate, and then refrigerate and filter to obtain crystals.
[0042] Comparative Example 1 Weigh 500 g of peony root bark, and prepare a peony root bark extract based on the extraction method specifically provided in Example 6. The only difference from Example 6 is that in step S2 of step 2 of preparing a peony root bark solution: add peony root bark powder to deionized water and then add it to ethanol for stirring and mixing, and soak it at a temperature of 45°C for 28 min to obtain a mixed solution 1; α-amylase, glucose oxidase and 500 mL of ethanol were added to the peony root bark extract, and the extract was placed in a water bath reflux extraction system. The distillate was collected and then refrigerated and filtered to obtain crystals.
[0043] Comparative Example 2 Weigh 500 g of peony root bark, and prepare the peony root bark extract by the extraction method specifically provided in Example 6. The only difference from Example 6 is that in step S3 of preparing the peony root bark solution in step 2, "adding ethanol to the mixed solution 1 three times in a volume ratio of 2:5 under a stirring environment to obtain a mixed solution 2" is not performed; α-amylase, glucose oxidase and 500 mL of ethanol were added to the peony root bark extract, and the extract was placed in a water bath reflux extraction system. The distillate was collected and then refrigerated and filtered to obtain crystals.
[0044] Comparative Example 3 Weigh 500 g of peony root bark, and prepare a peony root bark extract by the extraction method specifically provided in Example 6, the only difference from Example 6 being that no temperature adjustment is performed in step 2 in preparing the peony root bark solution; α-amylase, glucose oxidase and 500 mL of ethanol were added to the peony root bark extract, and the extract was placed in a water bath reflux extraction system. The distillate was collected and then refrigerated and filtered to obtain crystals.
[0045] The purity of the crystals obtained in Experimental Example 1 and Comparative Examples 1-3 was analyzed by HPLC: A small amount of crystals was taken from the crystals obtained in Experimental Example 1 and Comparative Examples 1-3, and placed in vials numbered 1-4, respectively, and dissolved with 2 mL of methanol, and the dissolved solution was filtered through a 0.45 μm organic phase filter membrane, and 20 μL was injected into the chromatographic column for high performance liquid chromatography analysis [chromatographic conditions: ODS column (4.6×250 mm, Ø 5 μm); methanol + H2O (volume ratio 80:20) as the mobile phase, the mobile phase flow rate was 1.0 mL / min; UV detector, the detection wavelength was 274 nm].
[0046] Specifically, the HPLC spectrum obtained by HPLC analysis of the purity of the crystals obtained in Experimental Example 1 can be found in detail. Figure 1 ( Figure 1 HPLC spectrum of paeonol according to the extraction method provided in Example 6 for Experimental Example 1): The peak with a retention time (t) of less than 5 min is a solvent peak generated by the mismatch between the sample solvent and the mobile phase. The peak at t = 50.1 min is paeonol, and the value at the highest peak of the paeonol peak is 73 AU. Figure 1 It can be seen that the paeonol of the present invention has less impurities and high purity; Specifically, the HPLC spectrum obtained by HPLC analysis of the purity of the crystals obtained in Comparative Example 1 can be found in detail. Figure 2 ( Figure 2 The HPLC spectrum of paeonol in comparative example 1, which is completely based on the extraction method specifically provided in example 6, is obtained by first adding deionized water and then adding ethanol): the peak with a retention time (t) of less than 5 min is a solvent peak generated by the mismatch between the solvent of the sample and the mobile phase, the peak at t = 49.8 min is paeonol, and the value at the highest peak of the paeonol peak is 69 AU. Figure 2 It can be seen that the paeonol of the present invention has less impurities and high purity; Specifically, the HPLC spectrum obtained by HPLC analysis of the purity of the crystals obtained in Comparative Example 2 can be found in detail. Figure 3 ( Figure 3The HPLC spectrum of paeonol in comparative example 2, which is completely based on the extraction method specifically provided in example 6 after only three discontinuous additions of ethanol: the peak with a retention time (t) of less than 5 min is a solvent peak generated because the solvent of the sample does not match the mobile phase, the peak at t = 50 min is paeonol, and the value at the highest peak of the paeonol peak is 68.5 AU, and the analysis Figure 3 It can be seen that the paeonol of the present invention has less impurities and high purity; Specifically, the HPLC spectrum obtained by HPLC analysis of the purity of the crystals obtained in Comparative Example 3 can be found in detail. Figure 4 ( Figure 4 The HPLC spectrum of paeonol in Comparative Example 3 is obtained by completely relying on the extraction method specifically provided in Example 6 without adjusting the temperature of ethanol): the peak with a retention time (t) of less than 5 min is a solvent peak generated by the mismatch between the solvent of the sample and the mobile phase, the peak at t = 50.1 min is paeonol, and the value at the highest peak of the paeonol peak is 71.5 AU. Figure 3 It can be seen that the paeonol of the present invention has less impurities and high purity; refer to Figure 1-Figure 4 The area of the paeonol peak can be obtained by accumulating the area of the paeonol peak. Figure 1 The area of the paeonol peak in (Experimental Example 1) is the largest. Figure 4 The area of the paeonol peak in (Comparative Example 3) did not decrease much; Figure 2 (Comparative Example 1) and Figure 3 The area of the paeonol peak in (Comparative Example 2) was reduced to a certain extent; Therefore, it can be concluded that by soaking at various temperatures, ultrasonic soaking and multiple additions of ethanol, the contact can be expanded, and the ethanol can be fully utilized through appropriate temperature, contact surface and contact time, so as to lock the paeonol in the peony root bark extract to the greatest extent and avoid the loss of paeonol in the peony root bark extract.
[0047] The paeonol crystals collected in the above Experimental Example 1 and Comparative Examples 1-3 were collected respectively, and the amount of paeonol crystals in each solution and the content of paeonol were measured, and recorded in the following Table 1.
[0048] Table 1 Paeonol crystals and paeonol content
[0049] Therefore, it can be seen from Table 1 that by soaking at various temperatures, ultrasonic soaking and multiple additions of ethanol, the contact is expanded, and the ethanol is fully utilized through appropriate temperature, contact surface and contact time, so as to lock the paeonol in the peony root bark extract to the greatest extent and avoid the loss of paeonol in the peony root bark extract.
[0050] Finally, it should be noted that the above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the aforementioned embodiments, it is still possible for those skilled in the art to modify the technical solutions described in the aforementioned embodiments or to make equivalent substitutions for some of the technical features therein. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.
Claims
1. A method for extracting a peony root bark extract having a soothing effect, characterized in that: Step 1: Pretreatment of Peony Root Bark Clean the peony root bark, lay it flat in a 10-20 ℃ environment, and then let dry air with a temperature of 10-20 ℃ pass through it at a wind speed of 5.5-10.7 m / s to dry the peony root bark in the shade; then control the water content of the peony root bark to 5-10%; Step 2: Prepare peony root bark solution S1, crushing the root bark of peony root and grinding it into a powder of 80-120 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking for 20-30 minutes at a temperature of 30-50°C to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 1-3 g: 15-20 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 100-120 KHz and 50-80 W, raising the temperature of the mixed solution 1 by 60-70 °C, and placing it for 10-25 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 1-3:7-9 under stirring to obtain a mixed solution 2; S4, placing the mixed solution 2 in an ultrasonic environment of 90-100 KHz and 50-80 W, and adjusting the temperature to 30-50°C; Step 3: Water bath reflux extraction S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 1-3:2-4; S2, stirring the deionized water and the mixed solution 2 at a stirring speed of 60-90 r / min, and after stirring for 10-20 minutes, adding the mixture into a water bath reflux extraction system to perform water bath reflux extraction to obtain an oil-water mixture; Step 4: Let the oil-water mixture stand to obtain crystals, and leave the crystals to obtain the peony root bark extract.
2. The method for extracting the peony root bark extract with soothing effect according to claim 1, characterized in that: In step 1, pretreatment of peony root bark, the peony root bark is cleaned, spread flat in an environment with a temperature of 18°C, and then dry air with a temperature of 18°C is introduced at a wind speed of 8.7 m / s to dry the peony root bark in the shade; the water content of the peony root bark is controlled at 8%.
3. The method for extracting the peony root bark extract with soothing effect according to claim 1, characterized in that: In step 2, preparing the peony root bark solution, the following steps are included: S1, crushing the root bark of Paeonia suffruticosa and grinding it into a powder of 110 mesh; S2, adding peony root bark powder into ethanol, stirring and mixing, and soaking at a temperature of 45°C for 28 min to obtain a mixed solution 1; wherein the mass volume ratio of peony root bark powder to ethanol is 2 g:17 mL; S3, placing the mixed solution 1 in an ultrasonic environment of 110 KHz and 68 W, raising the temperature of the mixed solution 1 by 62 °C, and placing it for 22 min; adding ethanol to the mixed solution 1 three times in a volume ratio of 2:5 under stirring to obtain a mixed solution 2; S4. Place the mixed solution 2 in an ultrasonic environment of 198 kHz and 60 W, and adjust the temperature to 40 °C.
4. The method for extracting the peony root bark extract with soothing effect according to claim 1 or 3, characterized in that: In the step 2 of preparing the peony root bark solution, the purity of ethanol is 95%.
5. The method for extracting the peony root bark extract with soothing effect according to claim 1 or 3, characterized in that: In step S3 of preparing the peony root bark solution in step 2, ethanol is continuously added to the mixed solution 1 under a stirring environment at a rotation speed of 200 r / min and a temperature of 50°C.
6. The method for extracting the peony root bark extract with soothing effect according to claim 1, characterized in that: In step three, water bath reflux extraction, the following steps are included: S1, adding deionized water into the mixed solution 2, the volume ratio of deionized water to the mixed solution 2 being 2:3; S2. Stir the deionized water and the mixed solution 2 at a stirring speed of 80 r / min. After stirring for 18 min, add the mixture into a water bath reflux extraction system to perform water bath reflux extraction to obtain the oil-water mixture.
7. The method for extracting the peony root bark extract with soothing effect according to claim 1 or 6, characterized in that: The water bath reflux extraction system comprises: A sealing top cover, wherein the sealing top cover is provided with a material injection pipe at the top thereof, and a sealing cover is provided on the material injection pipe; the material injection pipe is used to add materials; A heat exchange shell, wherein the heat exchange shell is detachably mounted on the bottom of the sealing top cover; A heat-conducting base, which is mounted on the bottom of the heat exchange shell; an open groove is provided at the bottom of the heat exchange shell to cooperate with the heat-conducting base, and the heat-conducting base is detachably mounted on the open groove; Wherein, the heat-conducting base is provided with a heat-exchange surface expansion structure inside the heat-exchange shell; the heat-exchange surface expansion structure is used to increase the contact surface between the heat source in the hot water bath and the material inside the heat-conducting base.
8. The method for extracting the peony root bark extract with soothing effect according to claim 7, characterized in that: The heat-conducting base is provided with a sealing ridge around the heat exchange surface extension structure, and the sealing ridge is used for sealing during the detachable installation process of the heat exchange shell and the heat-conducting base; The heat exchange surface extension structure includes: A main heat conducting plate, wherein the main heat conducting plate is provided with a plurality of material penetration ports on its main body, and a material passage cavity is provided inside its main body; the material passage cavity is connected to a hot water inlet provided on the heat conducting base; A plurality of unit heat exchange elements are arranged in an array on the main heat-conducting plate, and the unit heat exchange elements are connected to the material-passing cavity.
9. The method for extracting the peony root bark extract with soothing effect according to claim 8, characterized in that: The unit heat exchange element comprises: A heat conducting plate, the heat conducting plate is mounted on the main heat conducting plate, and a secondary material passage cavity is opened inside the heat conducting plate; the secondary material passage cavity is connected to the material passage cavity; A plurality of side heat-conducting telescopic plates, wherein the plurality of side heat-conducting telescopic plates are evenly spaced and distributed on the heat-conducting plate; The side heat-conducting telescopic plate includes a heat-conducting insertion plate and a heat-conducting outer sleeve movably mounted on the heat-conducting insertion plate; a material-conducting cavity is provided inside the heat-conducting insertion plate, and a partition is fixed at the center of the material-conducting cavity, and the partition divides the material-conducting cavity into an inlet channel and a water outlet channel; The partition is inserted into the secondary material passage cavity to separate the secondary material passage cavity, and the inlet channel and the water outlet channel are respectively connected at both ends of the partition; the partition is inserted into the interior of the thermal conductive jacket at the end away from the secondary material passage cavity; the thermal conductive jacket is fixed with a flushing guide plate on its inner wall, and a wedge-shaped surface is provided on the flushing guide plate.
10. An application of the method for extracting the peony root bark extract with soothing effect according to any one of claims 1 to 9, characterized in that: The method includes extracting from the whole herb of Cynanchum chinense, a plant of the Apocynaceae family.
Citation Information
Patent Citations
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CN113855599A
Multifunctional sample pretreatment device
CN113916640A
Whitening mask essence containing peony root bark extract and preparation method thereof
CN118141727A