Preparation method of honeysuckle warm tea and product obtained thereby
By processing licorice through homogenization, PEF, and microwave combined with NADESs technology, and combining it with honey-frying and rice water to blend with honeysuckle, the problems of low licorice extraction efficiency and strong cold nature of honeysuckle were solved, and a highly effective health tea suitable for all people was prepared.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-30
- Publication Date
- 2026-03-27
AI Technical Summary
Existing licorice extraction methods suffer from environmental pollution, solvent residue, and low extraction efficiency. Furthermore, honeysuckle tea is considered to be too cooling and is not suitable for all people.
Licorice was processed using homogenization, PEF, and microwave combined with NADESs technology. Honeysuckle was then blended with honey-processing and rice water to prepare honeysuckle warm tea through a special process, which improved extraction efficiency and health benefits.
This method achieves efficient and environmentally friendly extraction of licorice components, reduces the cold nature of honeysuckle, and enhances the nutritional and health benefits of honeysuckle warm tea, making it suitable for all ages.
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Abstract
Description
TECHNICAL FIELD
[0001] The present application relates to a preparation method of honeysuckle warm tea and honeysuckle warm tea obtained according to the method, in particular to a preparation method of honeysuckle warm tea with rich efficacy and green health and the obtained product, and belongs to the technical field of traditional Chinese medicine with medicinal and edible properties. BACKGROUND
[0002] Honeysuckle is the dried flower buds or with the initial open flowers of Lonicera japonica Thunb. of Caprifoliaceae, with sweet taste and cold nature, belonging to the lung, heart and stomach channels, and having the effects of clearing heat and resolving toxicity, dispelling wind and heat. The material basis for its multiple pharmacological effects mainly includes flavonoids, organic acids, volatile oils, etc. Honeysuckle is a commonly used traditional Chinese medicine, a medicinal and edible traditional Chinese medicinal material, and a famous local medicinal material in Shandong. In recent years, it has been widely used in the field of pharmaceuticals or health foods due to its good biological activity, such as honeysuckle tea, honeysuckle beverage, etc. Honeysuckle tea is often combined with licorice, which can weaken the cold nature of honeysuckle, enhance the heat-clearing and detoxifying effect, and has no harm to the stomach.
[0003] Licorice is the dried root and rhizome of Glycyrrhiza uralensis Fisch., Glycyrrhiza glabra L. or Glycyrrhiza inflata Bat. of Leguminosae. In traditional Chinese medicine, licorice is divided into raw licorice and roasted licorice. Raw licorice is slightly cool and is good at purging fire and resolving toxicity, reducing phlegm and relieving cough, while roasted licorice is slightly warm and can tonify qi and invigorate the center. The main effective components of licorice are triterpenoids and flavonoids, etc. At present, the extraction method of effective components of licorice is relatively single, and the traditional method is often used for extraction. There is a lack of research on step-by-step extraction of heat-sensitive and non-heat-sensitive components. Traditional extraction generally uses organic solvent extraction method, and the solvents are mostly methanol and ethanol, but organic solvents are volatile, not easy to degrade, and toxic, which not only pollutes the environment, but also limits the application of licorice extract in the fields of medicine and food due to the problems of solvent residue, etc. Therefore, some extraction methods with low energy consumption, green environmental protection and high extraction rate, as well as technologies and reagents with green characteristics have gradually attracted the attention of scholars.
[0004] PEF (Pulsed Electric Field) is a green food processing technology, due to its non-thermal and non-chemical treatment characteristics, the application potential in active substance extraction has attracted attention in the industry. PEF technology mainly changes the permeability of cell membrane or causes irreversible electroporation to cell membrane through high voltage, so as to accelerate the exudation of intracellular substances of cells and increase the extraction efficiency. Compared with traditional heat treatment and chemical treatment, PEF can not only improve the yield of target substances, but also well protect the activity of target substances. NADESs (natural low eutectic solvent) is considered to be the third liquid phase existing in the organism independently of water and lipids, which has good physicochemical properties, green characteristics and excellent extraction performance, and is an ideal extraction solvent. In recent years, many scholars have applied NADESs to extract flavonoids, proteins and polysaccharides in natural products, which is expected to replace traditional organic solvents to solve the problems in the extraction process of natural compounds. In the existing research, the research on the extraction of licorice by using NADESs is relatively insufficient, and the extraction is mainly assisted by ultrasonic or microwave, such as Jia-ni Dong (RSC Adv 2021 11(59) 37649-37660) adopts the method of ultrasonic assisted NADESs to extract active compounds from compound licorice tablets; PEF is also less used in licorice, only two scholars have applied this technology to extract licorice, such as Zhao Jinghui et al. (Modern Chinese Medicine Research and Practice 2010 24(06) 50-52) studied the extraction process of licorice by high pressure PEF method using water and ethanol as extraction solvent, and Shao Suying (Chinese patent CN104664512B 2016-07-06) prepared licorice concentrate by high pressure PEF extraction, ultrasonic assisted microwave extraction and low temperature enzymolysis technology.
[0005] It can be seen that PEF and NADESs will be more in line with the trend of green development, and there are few reports on the use of NADESs and PEF to extract licorice at present, and further research is necessary. SUMMARY
[0006] In view of the present situation of honeysuckle tea, the application provides a preparation method of honeysuckle warm tea, which takes honeysuckle as the main raw material, scientifically compounding licorice extract, treating the effective components of licorice by homogenate, PEF, microwave and NADESs technology, and compounding honeysuckle and licorice extract through a special process, so that the health care effect of honeysuckle is greatly improved.
[0007] The specific technical scheme adopted by the application is as follows:
[0008] A preparation method of honeysuckle warm tea, characterized by comprising the following steps:
[0009] (1) fresh licorice is crushed, then mixed with water and put into a homogenizer to extract at least once, filtered, and the obtained filtrate is combined to obtain a homogenate;
[0010] (2) the licorice residue obtained in step (1) is mixed with water, then pulsed, filtered after the treatment, and the obtained pulsed filtrate is combined with the homogenate of step (1) and concentrated to a density of 1.02-1.08 to obtain licorice extract 1;
[0011] (3) the licorice residue obtained after pulsed treatment in step (2) is processed by honey roasting to obtain honey-processed licorice residue;
[0012] (4) the honey-processed licorice residue is mixed with a natural eutectic solvent aqueous solution, then microwave extracted three times, the supernatant of the three times of extraction is combined, and the natural eutectic solvent is recovered to obtain licorice extract 2;
[0013] (5) the honeysuckle is put into a pot to be fried for the first time with the pot temperature controlled at 45-55℃, then the pot temperature is raised to 75-85℃ for the second time, then the pot temperature is raised to 95-105℃ for the third time, and finally the pot temperature is raised to 95-105℃ for the fourth time; the licorice extract 2 is evenly sprayed on the surface of the honeysuckle during the first three times of frying, each time for 2-5 min, and the rice washing water is evenly sprayed on the surface of the honeysuckle during the fourth time of frying until the surface of the honeysuckle is slightly dry;
[0014] (6) after frying, the fried honeysuckle is soaked in licorice extract 1 for 1-2h, then taken out and dried;
[0015] (7) the honeysuckle of step (6) is placed in a steam pot to make it soft, then pressed into a cake shape on a shaping mold, then freeze-dried, sterilized and packaged to obtain the honeysuckle warm tea.
[0016] Further, the honeysuckle used in the present application can be any honeysuckle available on the market, and the first crop of large flowers of the traditional Laiyang honeysuckle variety planted in Delenchang is preferably selected. The honeysuckle is cleaned before use and then dried. The cleaning can be done with water or rice washing water, and the drying can be done naturally or by drying.
[0017] Further, in step (1), the fresh licorice is washed and crushed. Crushing is to make the effective components better precipitate, which is beneficial to subsequent extraction. When crushing, the licorice can be cut into small pieces with scissors, or crushed with a food processor, a crusher, etc.
[0018] Further, in step (1), the crushed liquorice is extracted by a homogenizer, and the extraction can be performed once, twice or more than twice, preferably twice. In each extraction, the liquorice is mixed with water, and after filtration, water is added for repeated operation. In each extraction, the mass ratio of liquorice to water is 1:4-6, the extraction temperature is 0-4℃, the extraction time is 20-25min, the power of the homogenizer is 300-320W, the homogenization time is 1.5-2.5min, and the homogenization is performed every 30s. The homogenization extraction of liquorice at low temperature can reduce the particle size of liquorice, increase the specific surface area of liquorice particles, thereby accelerating the extraction efficiency, and effectively protecting the heat-sensitive components of liquorice, ensuring the effective extraction of heat-sensitive components.
[0019] Further, in step (2), the liquorice residue obtained after step (1) is mixed with water, and then subjected to pulse treatment (PEF), and the mass ratio of liquorice residue to water is 1:4-5. Pulse treatment is a high-efficiency and green active substance extraction technology, and the combination of PEF and homogenization extraction will achieve more environmentally friendly and efficient extraction significance.
[0020] Further, in step (2), the pulse treatment conditions are as follows: the pulse field strength is 0.5-2kV / cm, the pulse number is 20-120 times (preferably 60-120 times), the pulse frequency is 4-5Hz, and the pulse width is 8-10μs / time.
[0021] Further, in step (3), the liquorice residue is processed by honey roasting, and the processing method can refer to the existing honey roasting method, for example: dilute the honey with a proper amount of boiling water to prepare a yellow-brown color, soak the liquorice residue in the yellow-brown honey and mix well, then pour the honey-soaked liquorice residue into a pan and stir-fry until the water evaporates and the color turns yellow to dark yellow, then take it out when it is not sticky, and cool it to obtain the honey-roasted liquorice residue.
[0022] Further, in step (4), the preparation method of the natural low eutectic solvent aqueous solution is as follows: mix betaine and 1,4-butanediol in a molar ratio of 1:1-1:3, continuously stir at 90-95℃ until it becomes clear and transparent, obtain the natural low eutectic solvent (NADESs), and then dilute the natural low eutectic solvent with water to obtain a natural low eutectic solvent aqueous solution with a volume fraction of 75-85%. NADESs is a new type of green solvent, which has the characteristics of low cost, environmental safety, simple operation, high sensitivity and good selectivity.
[0023] Further, in step (4), when preparing the natural low eutectic solvent aqueous solution, it is preferred to use a magnetic stirring water bath to continuously stir, which has the advantages of both magnetic stirrers and water baths, and is convenient and controllable.
[0024] Further, in step (4), the effective components of licorice are extracted by microwave-assisted NADESs technology. The microwave extraction is performed for three times, and the mass ratio of the residue of licorice to the aqueous solution of natural eutectic solvent is 1:2.5-3.5 in each extraction. After each extraction, the obtained filtrate is filtered and combined. The microwave power is 430-460 W, the microwave temperature is 45-55℃, and the extraction time is 25-35 min in the first microwave extraction; the microwave power is 430-460 W, the microwave temperature is 75-85℃, and the extraction time is 25-35 min in the second microwave extraction; and the microwave power is 430-460 W, the microwave temperature is 95-105℃, and the extraction time is 25-35 min in the third microwave extraction. Under the condition of microwave, the extraction operation with step-by-step temperature increase can make more non-thermal sensitive components with different properties be extracted.
[0025] Further, in step (5), the mass ratio of licorice extract 2 to honeysuckle sprayed on the surface of honeysuckle is 1:8-12 in the first three times of stirring. The spraying speed can be adjusted to ensure that the required licorice extract 2 is sprayed on the surface of honeysuckle within a specified time. With the stirring process, the licorice extract 2 can be evenly attached to the surface of honeysuckle and enter the interior of honeysuckle.
[0026] Further, in step (5), the mass ratio of rice washing water to honeysuckle sprayed on the surface of honeysuckle is 1:8-12 in the fourth time of stirring. The rice washing water is acidic with a pH value of 5.5-6. The rice washing water has the effects of clearing heat, removing fire, nourishing the spleen and stomach, disinfection, and decontamination. The rice washing water contains protein starch and various minerals, which can effectively protect the gastric mucosa and reduce food accumulation and indigestion. The addition of licorice extract and rice washing water during the stirring process can effectively reduce the coldness of honeysuckle and enhance the warm tea warming effect of honeysuckle.
[0027] Further, in step (5), the rice washing water is preferably rice washing water, and the mass ratio of rice to water can be selected at will. Preferably, the rice washing water is prepared by washing the rice with water, then mixing the rice and water according to a mass ratio of 1:3-5, soaking for 20-30 min, and then filtering to obtain the rice washing water.
[0028] Further, in step (5), the temperature of the pot is increased to 75-85℃ at a heating rate of 1-10℃ / min, and then the temperature of the pot is increased to 95-105℃ at a heating rate of 1-10℃ / min.
[0029] Further, in step (6), the fried honeysuckle is completely immersed in licorice extract 1 for 1-2 hours, so that the licorice extract 1 fully enters the honeysuckle. After the immersion, the honeysuckle is taken out and dried. The drying can be performed on a shaking bed, and the drying temperature is preferably 4-10℃. During the drying, the honeysuckle can be turned over to make the effective components of the licorice fully enter the honeysuckle.
[0030] Further, in step (7), the honeysuckle is first placed in a steam tank to make it soft, and then is pressed, freeze-dried and sterilized. The freeze-drying is performed by using a freeze-drying machine. The vacuum freeze-drying avoids the oxidation and decomposition of the dried material caused by high-temperature normal-pressure evaporation, and maintains the original nutrients and high effective components of the medicinal materials. The sterilization can be performed by using non-thermal sterilization technology, such as irradiation sterilization.
[0031] The honeysuckle warm tea obtained by the above method is also within the protection scope of the present application. Through the special process of the present application, the honeysuckle warm tea not only effectively improves the cold nature of the honeysuckle itself, but also combines the honeysuckle with the licorice, thereby improving the nutritional and health care effects of the honeysuckle. The honeysuckle warm tea is a kind of drink suitable for all ages, which has the effects of tonifying the spleen and invigorating qi, clearing heat and detoxifying, and antioxidant.
[0032] Compared with the prior art, the present application has the following advantages:
[0033] 1. The fresh licorice is first extracted by a homogenizer, and then is subjected to secondary extraction by PEF. The effective components of the licorice can be extracted more environmentally friendly and more efficiently, and the heat-sensitive components in the licorice are more effectively protected. Then, the licorice residues are honeyed, and the microwave extraction technology is used to extract the licorice residues by gradually increasing the temperature, using NADESs as the solvent. The medicinal components of the licorice can be fully extracted, especially some non-heat-sensitive components with different properties. After the licorice is treated by the method of the present application, the biological activity of the extract is maximized, and the extraction rate of the licorice is maximized.
[0034] 2. PEF extraction has the advantages of short time, high efficiency, low energy consumption, green environmental protection, etc., and is widely used in the extraction of bioactive components. The combination of PEF and homogenization extraction for extracting licorice can significantly improve the extraction rate of medicinal materials, reduce the extraction time, reduce the damage to effective components, and increase the precipitation of heat-sensitive effective components, compared with traditional methods.
[0035] 3. The NADESs are used to extract the licorice residues, which are non-toxic, harmless, degradable, recyclable, green, environmentally friendly, sensitive and selective.
[0036] 4. The roasting process of this invention adopts a special temperature control program, scientifically combines honeysuckle and licorice extracts, and adds a small amount of rice water for blending. Compared with conventional licorice and honeysuckle, this improves the comprehensive utilization rate of honeysuckle, reduces its cold nature, and promotes the synergistic effect of honeysuckle warm tea. It retains the original effective components of honeysuckle and increases the effective components of licorice, greatly enhancing the health benefits of honeysuckle. It is a beverage suitable for all ages with the effects of tonifying the spleen and replenishing qi, clearing heat and detoxifying, and anti-oxidation.
[0037] 5. After processing by the method of the present invention, the honeysuckle warm tea obtained retains the biological activity of the extract to the maximum extent and improves the selectivity of the target substance in the system. The content of organic acid components and luteolin glycosides changes significantly after adding licorice extract and rice water during the stir-frying process, and the free radical scavenging ability is significantly improved.
[0038] 6. The honeysuckle warming tea of this invention is especially suitable for people with heat-clearing, detoxifying, and antioxidant needs, as well as those with weak spleen and stomach, fatigue, and excessive phlegm. The honeysuckle warming tea, processed through a special process, has significantly reduced coldness and also has a good therapeutic effect on those with weak stomach and spleen who should not consume honeysuckle. Detailed Implementation
[0039] The technical solution of the present invention will be clearly and completely described below with reference to specific embodiments. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0040] In the following examples and comparative examples, the method for preparing rice water is as follows: wash rice with water once, then mix rice and water at a mass ratio of 1:4, soak for 25 minutes, and then filter to obtain rice water.
[0041] Example 1:
[0042] S1. Select the first batch of large-flowered honeysuckle of the traditional Pingyi honeysuckle variety planted at the Delunchang base, wash it with rice water, and then dry it in the sun (or oven) for later use.
[0043] S2. Fresh licorice root after washing and cutting, mixed with distilled water at a mass ratio of 1:5, put into a homogenizer with a power of 300W, homogenized at an extraction temperature of 0-4℃ for 20min, each time for 2min, homogenized every 30s, filtered with 200 mesh filter cloth, and the filtrate and residue were obtained. The residue was repeatedly homogenized once in the same way. After homogenization, the residue was mixed with 4 times the amount of distilled water and placed in a pulsed electric field (PEF) treatment chamber for pulse treatment. The electric field conditions were: pulse field strength 1.5kV / cm, pulse number 90, pulse frequency 5Hz, pulse width 8μs / time. After the pulse ended, the filtrate and residue were obtained by filtering with 200 mesh filter cloth. Finally, the filtrate obtained by homogenization and pulse treatment was mixed and concentrated to a density of 1.08, and finally licorice extract 1 and licorice residue were obtained for use;
[0044] S3. The honey was diluted with boiling water to prepare a dark yellow color. The licorice residue was soaked in the dark yellow honey and stirred evenly, then the honey-soaked licorice residue was poured into a pan and fried until the water evaporated and the color turned yellow to dark yellow. When it was not sticky, it was taken out and cooled to obtain fried licorice residue, which was ready for use;
[0045] S4. Mix betaine and 1,4-butanediol at a molar ratio of 1:2, then use a magnetic stirring water bath to continuously stir at 95℃ until a clear and transparent natural low eutectic solvent (NADESs) is formed. Dilute the NADESs with ultrapure water to form a NADESs / water (80%, v / v) solution;
[0046] S5. Mix the fried licorice residue with the NADESs / water solution at a mass ratio of 1:3 and perform microwave extraction for a total of 3 times. The first extraction was performed at a microwave power of 450W, a microwave temperature of 50℃, and an extraction time of 30min. After extraction, the filtrate and residue were obtained. The second extraction was performed on the residue, with the difference being that the microwave temperature was changed to 80℃. The third extraction was different from the first in that the microwave temperature was changed to 100℃. After extraction, the supernatant from the three extractions was combined and the NADESs was recovered to obtain licorice extract 2, which was ready for use;
[0047] S6. Put honeysuckle of step S1 in a wok, firstly control the temperature of the wok as 50℃, spray the licorice extract 2 of S5 on the honeysuckle and stir-fry for 2 min, then increase the temperature to 80℃ at a rate of 5℃ / min, spray the licorice extract 2 of S5 on the honeysuckle and stir-fry for 2 min, then increase the temperature to 100℃ at a rate of 5℃ / min, spray the licorice extract 2 of S5 on the honeysuckle and continue to stir-fry for 2 min, finally spray the rice washing water on the honeysuckle and continue to stir-fry at 100℃ until the surface is slightly dry. The mass ratio of licorice extract 2 to honeysuckle is 1:10, and the mass ratio of rice washing water to honeysuckle is 1:10.
[0048] S7. After the stir-frying, immerse the honeysuckle in the licorice extract 1 of S2 for 1.5 h, then take out and place on a shaker, dry the surface at 4℃, and turn the honeysuckle up and down 3-5 times with a wooden spatula during the period.
[0049] S8. Put the honeysuckle of S7 in a steam tank to make it soft, then place it in a shaping mold and press into a cake, then freeze-dry, sterilize and package to obtain the honeysuckle warm tea.
[0050] Example 2:
[0051] Prepare the honeysuckle warm tea according to the method of Example 1, except that in step S2, the electric field conditions are pulse field strength 0.5 kV / cm, pulse number 60 times, pulse frequency 5 Hz, and pulse width 8 μs / time.
[0052] Example 3:
[0053] Prepare the honeysuckle warm tea according to the method of Example 1, except that in step S2, the electric field conditions are pulse field strength 2 kV / cm, pulse number 120 times, pulse frequency 5 Hz, and pulse width 8 μs / time.
[0054] Example 4:
[0055] Prepare the honeysuckle warm tea according to the method of Example 1, except that in step S4, mix betaine and 1,4-butanediol at a molar ratio of 1:3.
[0056] Example 5:
[0057] Prepare the honeysuckle warm tea according to the method of Example 1, except that in step S4, mix betaine and 1,4-butanediol at a molar ratio of 1:1.
[0058] Example 6:
[0059] The honeysuckle warm tea was prepared according to the method of Example 1, except that in step S6, the honeysuckle of step S1 was placed in a wok, the wok temperature was first controlled at 45℃, the licorice extract 2 obtained in S5 was evenly sprayed on the honeysuckle and stirred for 5 min, then the temperature was raised to 75℃ at a rate of 1℃ / min, the licorice extract 2 obtained in S5 was evenly sprayed on the honeysuckle and stirred for 5 min, then the temperature was raised to 95℃ at a rate of 1℃ / min, the licorice extract 2 obtained in S5 was evenly sprayed on the honeysuckle and continued to stir for 5 min, and finally the rice washing water was evenly sprayed on the honeysuckle and continued to stir at 95℃ until the surface was slightly dry. Among them, the mass ratio of licorice extract 2 to honeysuckle in each spraying was 1:8; the mass ratio of rice washing water to honeysuckle was 1:8.
[0060] Example 7:
[0061] The honeysuckle warm tea was prepared according to the method of Example 1, except that in step S6, the honeysuckle of step S1 was placed in a wok, the wok temperature was first controlled at 55℃, the licorice extract 2 obtained in S5 was evenly sprayed on the honeysuckle and stirred for 2 min, then the temperature was raised to 85℃ at a rate of 10℃ / min, the licorice extract 2 obtained in S5 was evenly sprayed on the honeysuckle and stirred for 2 min, then the temperature was raised to 105℃ at a rate of 10℃ / min, the licorice extract 2 obtained in S5 was evenly sprayed on the honeysuckle and continued to stir for 2 min, and finally the rice washing water was evenly sprayed on the honeysuckle and continued to stir at 105℃ until the surface was slightly dry. Among them, the mass ratio of licorice extract 2 to honeysuckle in each spraying was 1:12; the mass ratio of rice washing water to honeysuckle was 1:12.
[0062] Comparative Example 1:
[0063] The honeysuckle warm tea was prepared according to the method of Example 1, except that in step S2, pulse treatment was performed first, and then homogenate extraction was performed.
[0064] Comparative Example 2:
[0065] The honeysuckle warm tea was prepared according to the method of Example 1, except that step S4 was omitted, and the NADESs / water solution in step S5 was replaced with distilled water.
[0066] Comparative Example 3:
[0067] S1. The same as Example 1;
[0068] S2. The same as Example 1;
[0069] S3. The same as Example 1;
[0070] S4. The same as Example 1;
[0071] S5. The same as Example 1;
[0072] S6. Put the honeysuckle of step S1 in a charcoal pot, first control the pot temperature to be 50℃, evenly spray distilled water on the honeysuckle and stir-fry for 2 min, then increase the temperature to 80℃ at a rate of 5℃ / min, evenly spray distilled water on the honeysuckle and stir-fry for 2 min, then increase the temperature to 100℃ at a rate of 5℃ / min, evenly spray distilled water on the honeysuckle and continue to stir-fry for 2 min, finally evenly spray rice washing water on the honeysuckle and continue to stir-fry at 100℃ until the surface is slightly dry. The mass ratio of distilled water to honeysuckle is 1:10 each time, and the mass ratio of rice washing water to honeysuckle is 1:10.
[0073] S7. Mix the licorice extract 1 and the licorice extract 2 according to a mass ratio of 1:1, after the frying is finished, immerse the honeysuckle in the mixed solution of the licorice extract, soak for 1.5 h, then take out and place on a shaker, dry the surface at 4℃, during which time use a wooden spatula to stir the honeysuckle up and down for 3-5 times;
[0074] S8. Put the honeysuckle of S7 in a steam tank to make it soft in texture, then place it in a shaping mold and press into a cake shape, then freeze-dry using a freeze-drying machine, sterilize, and package to obtain the honeysuckle warm tea.
[0075] Comparative Example 4:
[0076] S1. Select the first batch of large flowers of the Pingyi traditional honeysuckle variety planted in Delenchang, wash them with rice washing water, and then dry them (dry them in an oven) for use;
[0077] S2. Put the honeysuckle of step S1 in a charcoal pot, first control the pot temperature to be 50℃, stir-fry for 2 min, then increase the temperature to 80℃ at a rate of 5℃ / min and stir-fry for 2 min, then increase the temperature to 100℃ at a rate of 5℃ / min and stir-fry until the surface is slightly dry.
[0078] S3. After the frying is finished, place the honeysuckle on a shaker, dry the surface at 4℃, during which time use a wooden spatula to stir the honeysuckle up and down for 3-5 times;
[0079] S4. Put the honeysuckle of S3 in a steam tank to make it soft in texture, then place it in a shaping mold and press into a cake shape, then freeze-dry using a freeze-drying machine, sterilize, and package to obtain the honeysuckle warm tea.
[0080] Comparative Example 5:
[0081] Prepare the honeysuckle warm tea according to the method of Example 1, except that in step S5, microwave extraction is performed, and the extraction temperature is 100℃ for 3 times.
[0082] Comparative Example 6:
[0083] The honeysuckle warm tea was prepared according to the method of Example 1, except that in step S6, the honeysuckle of step S1 was placed in a wok, the wok temperature was controlled at 100°C, the licorice extract 2 obtained in S5 was evenly sprayed on the honeysuckle and stirred for 6 min, the mass ratio of licorice extract 2 to honeysuckle was 3:10. Finally, the rice washing water was evenly sprayed on the honeysuckle and stirred until the surface was slightly dry, the mass ratio of rice washing water to honeysuckle was 1:10.
[0084] The honeysuckle warm tea obtained in the above examples and comparative examples was evaluated, and the evaluation method is shown as follows:
[0085] 1. Determination of the content of organic acid components and osmanthus glycoside
[0086] 1.1 Determination of the content of organic acid components
[0087] 1.1.1 Preparation of the control solution
[0088] An appropriate amount of chlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B and 1,3-O-dicaffeoylquinic acid control samples were precisely weighed, placed in a brown bottle, and 75wt% methanol was added to prepare a solution of 400.00 μg / mL, 40.00 μg / mL and 20.00 μg / mL, respectively. The solution was filtered through a 0.22 μm microporous filter to obtain the control solution.
[0089] 1.1.2 Preparation of the test solution
[0090] The honeysuckle warm tea prepared in the examples and comparative examples was crushed and passed through a No. 4 sieve. 0.5 g of the crushed and sieved honeysuckle warm tea powder was precisely weighed and placed in a conical flask with a stopper. 25 mL of 75wt% methanol was precisely added, the weight was determined, and the sample was ultrasonically treated (power 500 W, frequency 40 kHz) for 30 min. The sample was cooled and weighed again. The lost weight was made up with 75wt% methanol, and the sample was shaken and filtered. The filtrate was filtered through a 0.22 μm microporous filter to obtain the test solution.
[0091] 1.1.3 Chromatographic conditions
[0092] Chromatographic column: YMC-C 18 Chromatographic column (250x4.6 mm, 5 μm); mobile phase: A was acetonitrile and B was 0.1wt% phosphoric acid; gradient elution (0-10 min, 10-15% A; 10-15 min, 15% A; 15-35 min, 15-30% A; 35-40 min, 30-90% A); flow rate: 1.0 mL / min; column temperature: 25°C; detection wavelength: 327 nm; injection volume: 10 μL.
[0093] 1.2 Determination of the content of osmanthus glycoside
[0094] 1.2.1 Preparation of the control solution
[0095] Take the lavandulatin control, accurately weigh, put it in a brown bottle, add 70wt% ethanol to make a 40ug / mL solution, filter through a 0.22um microporous filter, and get it.
[0096] 1.2.2 Preparation of test solution
[0097] Take the honeysuckle warm tea prepared in the examples and comparative examples, crush it through a No.4 sieve, accurately weigh 2g of the crushed honeysuckle warm tea powder, accurately weigh it in a conical flask with a plug, accurately add 50mL of 70wt% ethanol, weigh it, ultrasonic treat it (power 250W, frequency 35kHz) for 1h, cool it, weigh it again, make up the weight loss with 70wt% ethanol, shake it well, filter it, accurately take 10mL of the filtrate, recover the solvent to dryness, dissolve the residue with 70wt% ethanol, transfer it to a 5mL volumetric flask, add 70wt% ethanol to the mark, filter it through a 0.22um microporous filter, and get it.
[0098] 1.2.3 Chromatographic conditions
[0099] Chromatographic column: phenylsilane bonded silica gel chromatographic column (250x4.6mm, 5um) is adopted; mobile phase: A is acetonitrile and B is 0.5wt% glacial acetic acid; gradient elution (0-15min, 10-20% A; 15-30min, 20% A; 30-40min, 20-30% A); flow rate: 1.0mL / min; column temperature: 25℃; detection wavelength: 350nm; injection volume: 10uL.
[0100] 1.3 Results
[0101] The samples are determined by HPLC, and the results are shown in Table 1, the contents of chlorogenic acid, cryptochlorogenic acid, isochlorogenic acid B, 1,3-O-dicaffeoylquinic acid and lavandulatin in the honeysuckle warm tea of examples 1-7 are all better than those of comparative examples 1-6, and the content of example 1 is the highest. The results show that the honeysuckle warm tea prepared by homogenization, PEF, microwave and NADESs technology and special roasting method can obviously improve the content of effective components of medicinal materials, reduce the extraction time and reduce the damage to effective components.
[0102] Table 1 Determination results of components in honeysuckle warm tea (n=3)
[0103]
[0104]
[0105] 2. Drug resistance determination
[0106] According to the literature "50 kinds of Chinese medicine total protein content and the correlation between the cold and hot drug properties", the average total protein content of hot Chinese medicine is 2.37 times that of cold Chinese medicine. Therefore, by determining the protein content, combined with mathematical statistics, the change of drug properties can be analyzed, and the cold and hot properties of Chinese medicine can be preliminarily judged. The protein content is determined by Coomassie brilliant blue method.
[0107] 2.1 Experimental reagents
[0108] Coomassie brilliant blue, 95wt% ethanol (analytical pure), phosphoric acid (analytical pure), bovine serum albumin
[0109] 2.2 Experimental instruments
[0110] Pulverizer, electronic analytical balance, hot air drying oven, centrifuge.
[0111] 2.3 Experimental samples
[0112] Take 5g of fried honeysuckle tea, add 160mL of water, and get tea soup at 100℃ for 20min. The tea soup of the examples and the comparative examples is 13 parts, which is used as the experimental sample.
[0113] 2.4 Control sample
[0114] Take 5g of honeysuckle without any treatment, add 160mL of water, and get tea soup at 100℃ for 20min, which is used as the control sample.
[0115] 2.5 Experimental method
[0116] 2.5.1 Preparation of protein standard solution
[0117] Take 10.0mg of bovine serum albumin, dissolve with a small amount of distilled water, and dilute to 100mL to get 0.1mg / mL protein standard solution (4℃ in refrigerator).
[0118] 2.5.2 Preparation of Coomassie brilliant blue G-250 solution
[0119] Take 100mg of Coomassie brilliant blue G-250, accurately weigh, add 50mL of 95wt% ethanol (blue), stir and dissolve, then add 100mL of 85wt% phosphoric acid (blood red) and stir, finally dilute to 1000mL with distilled water (brown), stir on a magnetic heating stirrer for 4h, filter with a quantitative filter paper, and reserve.
[0120] 2.5.3 Standard curve drawing
[0121] Take 0.1 mg / mL BSA standard solution 200 μL, 300 μL, 400 μL, 600 μL, 800 μL, 1000 μL, respectively, add distilled water to 1 mL, then add 5 mL Coomassie brilliant blue G-250 solution, and determine at 595 nm when color developing for 5 min. Take protein content (X) as the abscissa and absorbance (A) as the ordinate to draw the standard curve and conduct linear regression analysis.
[0122] 2.5.4 Preparation of test solution
[0123] Take 13 portions of experimental sample tea soup 25 mL and 1 portion of control sample tea soup 25 mL respectively, centrifuge (10000 r / min) for 10 min, and then filter the supernatant to 50 mL for determination.
[0124] 2.5.5 Determination
[0125] Take 2 test tubes, add 1 mL distilled water as blank control, and take 14 test tubes, add 13 portions of experimental sample tea soup solution and 1 portion of control sample tea soup solution, add distilled water to 1 mL, then add 5 mL Coomassie brilliant blue G-250 solution, and determine absorbance at 595 nm when color developing for 5 min.
[0126] 2.6 Results
[0127] The total protein content of honeysuckle warm tea is shown in Table 2. The total protein content of honeysuckle warm tea of each example is significantly higher than that of each control, and the total protein content of the optimal treatment example 1 is the highest. It can be seen that the honeysuckle warm tea treated by the method of the application greatly reduces the cold nature of honeysuckle itself, and is especially suitable for people with weak stomach and spleen who are not suitable to eat honeysuckle.
[0128] Table 2 Determination results of total protein content in honeysuckle warm tea (n=3)
[0129]
[0130]
[0131] 3. In vitro antioxidant detection
[0132] 3.1 DPPH free radical scavenging ability
[0133] 3.1.1 Sample preparation
[0134] Take the honeysuckle warm tea prepared in the examples and comparative examples, pulverize it and pass it through a 40-mesh sieve. Take 0.01g of the pulverized and sieved honeysuckle warm tea powder, add 1mL of 80wt% methanol extract, microwave it (60℃, power 500W, frequency 40kHz) for 30min, make up to 1mL with 80wt% methanol, centrifuge at 12000rpm at room temperature for 10min, and take the supernatant for analysis.
[0135] 3.1.2 On-machine testing
[0136] ① Preheat the microplate reader for at least 30 minutes and adjust the wavelength to 517nm.
[0137] ② Different samples have different removal capabilities. Two samples can be selected for testing first. If the difference between the A determination and the A control is close to zero, the sample needs to be diluted (with 80wt% methanol extract) before testing. The dilution factor D is then substituted into the formula for calculation.
[0138] ③ Add reagents to the EP tube as shown in Table 3.
[0139] Table 3. Dosage of reagents added to EP tubes in the antioxidant activity assay.
[0140] Reagent name Test tube (μL) Control tube (μL) Blank tube (μL) Sample 150 150 80 wt% methanol 150 150 Working solution 150 150
[0141] ④ Mix well and let stand at room temperature (25℃) in the dark for 30 min; centrifuge at 12000 rpm at room temperature for 5 min, take 200 μL into a 96-well plate, and read the absorbance value A at 517 nm.
[0142] ⑤ The formula for calculating the DPPH free radical scavenging rate (K) is:
[0143]
[0144] Where A1 is the measured absorbance value;
[0145] A2 is the control absorbance value;
[0146] A0 is the blank absorbance value.
[0147] 3.2 ABTS free radical scavenging ability
[0148] 3.2.1 Sample Preparation
[0149] Take the honeysuckle warm tea prepared in the examples and comparative examples, pulverize it and pass it through a 40-mesh sieve. Take 0.05g of the pulverized and sieved honeysuckle warm tea powder, add 1mL of 80wt% methanol extract, microwave it (60℃, power 500W, frequency 40kHz) for 30min, make up to 1mL with 80wt% methanol, centrifuge at 12000rpm at room temperature for 10min, and take the supernatant for analysis.
[0150] 3.2.2 On-machine testing
[0151] ① The microplate reader is preheated for more than 30 min, and the wavelength is adjusted to 734 nm.
[0152] ② Different samples have different clearance abilities. Two samples can be selected for detection first. If A determination-A control is close to zero, the sample needs to be diluted (diluted with 80wt% methanol extraction solution) and then detected. The dilution multiple D is substituted into the formula for calculation.
[0153] ③ Add reagents to the 96-well plate as shown in Table 4.
[0154] Table 4 Dosage of reagents added to the 96-well plate for antioxidant activity detection experiment
[0155] Reagent name Test tube (μL) Control tube (μL) Blank tube (μL) Sample 10 10 Anhydrous ethanol 190 10 Working solution 190 190
[0156] ④ Mix well, and stand at room temperature (25℃) in the dark for 6 min. Read the absorbance value A at 734 nm.
[0157] ⑤ The ABTS free radical scavenging rate (K) calculation formula is:
[0158]
[0159] Wherein, A1 is the determination absorbance;
[0160] A2 is the control absorbance;
[0161] A0 is the blank absorbance.
[0162] 3.3 Results
[0163] The DPPH and ABTS free radical scavenging ability determination results of the honeysuckle warm tea are shown in Table 5 below. As can be seen from the table, the antioxidant activity of the honeysuckle warm tea of Examples 1-7 is better than that of Comparative Examples 1-6, and the antioxidant activity of Example 1 is the best. It can be seen that after being treated by the method of the present application, the honeysuckle warm tea obtained maximizes the biological activity of the extract.
[0164] Table 5 DPPH and ABTS free radical scavenging ability determination results of honeysuckle warm tea (n=3)
[0165] Sample DPPH scavenging rate (%) ABTS scavenging rate (%) Example 1 77.71±0.02 48.98±0.02 Example 2 69.61±0.01 41.98±0.02 Example 3 70.33±0.01 42.78±0.02 Example 4 74.69±0.01 46.26±0.01 Example 5 71.26±0.01 43.53±0.03 Example 6 67.71±0.02 40.98±0.03 Example 7 65.99±0.03 39.23±0.01 Comparative Example 1 62.90±0.01 35.76±0.02 Comparative Example 2 63.03±0.01 36.65±0.02 Comparative Example 3 61.17±0.00 34.12±0.01 Comparative Example 4 52.05±0.02 22.60±0.01 Comparative Example 5 60.35±0.00 33.93±0.01 Comparative Example 6 56.59±0.01 28.87±0.02
Claims
1. A preparation method of honeysuckle warm tea, characterized by comprising the following steps: The method comprises the following steps: (1) crushing fresh licorice and mixing with water, then putting into a homogenizer to extract at least once, filtering, and combining the obtained filtrate to obtain a homogenate; (2) mixing the licorice residue obtained in step (1) with water, then performing pulse treatment, filtering after the treatment, combining the obtained pulse filtrate with the homogenate of step (1), and concentrating to a density of 1.02-1.08 to obtain licorice extract 1; (3) using honey-roasting method to process the licorice residue obtained after the pulse treatment in step (2) to obtain honey-roasted licorice residue; (4) mixing the honey-roasted licorice residue with a natural eutectic solvent aqueous solution, then performing microwave extraction three times, combining the supernatants of the three times of extraction, and recovering the natural eutectic solvent to obtain licorice extract 2; (5) controlling the pot temperature to be 45-55 ℃, putting honeysuckle into the pot to perform first-time stir-frying, then increasing the pot temperature to 75-85 ℃ to perform second-time stir-frying, then increasing the pot temperature to 95-105 ℃ to perform third-time stir-frying, and finally performing fourth-time stir-frying at 95-105 ℃; during the first three times of stir-frying, spraying the licorice extract 2 evenly on the surface of the honeysuckle, each time for 2-5 min, and during the fourth-time stir-frying, spraying the rice washing water evenly on the surface of the honeysuckle until the surface of the honeysuckle is slightly dry; (6) after the stir-frying, soaking the stir-fried honeysuckle in the licorice extract 1 for 1-2 h, then taking out the honeysuckle and air-drying; (7) placing the honeysuckle of step (6) in a steam pot to make the honeysuckle soft, then placing the honeysuckle in a shaping mold to press into a cake shape, then freeze-drying, sterilizing, and packaging to obtain honeysuckle warm tea; In step (2), the mass ratio of liquorice filter residue to water is 1:4-5; the pulse treatment conditions are: pulse field intensity is 0.5-2 kV / cm, pulse number is 20-120 times, pulse frequency is 4-5 Hz, pulse width is 8-10 µ s / time; In step (4), the mass ratio of the honey-roasted licorice residue to the natural eutectic solvent aqueous solution is 1:2.5-3.5, and the natural eutectic solvent aqueous solution is prepared by mixing betaine and 1, 4-butanediol at a molar ratio of 1:1-1:3, continuously stirring at 90-95 ℃ until clear and transparent, obtaining the natural eutectic solvent, and then diluting the natural eutectic solvent with water to a volume fraction of 75-85 % to obtain the natural eutectic solvent aqueous solution; In step (4), the microwave power of the first-time microwave extraction is 430-460 W, the microwave temperature is 45-55 ℃, and the extraction time is 25-35 min; the microwave power of the second-time microwave extraction is 430-460 W, the microwave temperature is 75-85 ℃, and the extraction time is 25-35 min; the microwave power of the third-time microwave extraction is 430-460 W, the microwave temperature is 95-105 ℃, and the extraction time is 25-35 min.
2. The method of claim 1 wherein: In step (1), the homogenate extraction is performed twice.
3. The method of claim 1 or 2, wherein: In step (1), the conditions of each time of homogenate extraction are as follows: the mass ratio of licorice to water is 1:4-6, the extraction temperature is 0-4 ℃, the extraction time is 20-25 min, the power of the homogenizer is 300-320 W, the homogenization time is 1.5-2.5 min, and the interval between the homogenizations is 30 s.
4. The method of claim 1 wherein: In step (5), the mass ratio of the liquorice extract 2 sprayed onto the surface of the honeysuckle flowers to the honeysuckle flowers is 1:8-12 in the first three times of stirring, and the mass ratio of the rice washing water sprayed onto the surface of the honeysuckle flowers to the honeysuckle flowers is 1:8-12 in the fourth time of stirring.
5. The method of claim 1 or 4, wherein: In step (5), the temperature of the pot is raised to 75-85 ℃ at a temperature raising rate of 1-10 ℃ / min, and then raised to 95-105 ℃ at a temperature raising rate of 1-10 ℃ / min.
6. The honeysuckle warm tea prepared according to the preparation method of the honeysuckle warm tea in any one of claims 1-5.
Citation Information
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