Method for improving extraction transfer rate of hyperoside in semen cuscutae for health-care wine and application

Abstract

The invention relates to the technical field of extraction of traditional Chinese medicinal materials, and particularly provides a method for improving the extraction transfer rate of hyperoside in semen cuscutae for health-care wine. According to the method, the semen cuscutae medicinal material is squeezed at high temperature before extraction, on one hand, the compact structure of the semen cuscutae medicinal material is damaged through high-temperature squeezing, so that an extraction solvent can enter the semen cuscutae more easily, and the extraction transfer rate of the effective component hyperoside is close to 100%; on the other hand, grease substances in the semen cuscutae are removed through squeezing, and pollution to an ultrafiltration membrane is small during filtration, so that the filtration efficiency of the ultrafiltration membrane is remarkably improved, the loss of hyperoside is reduced, the membrane is easy to clean, and the service life of the ultrafiltration membrane can be prolonged. The used medicinal material processing method is simple and efficient, equipment is common, an extraction solvent is environment-friendly and edible, crushing or enzyme preparation adding and the like are not needed during extraction, and practicability and economical efficiency are high.

Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicine extraction, and particularly to a method for improving the extraction and transfer rate of hyperoside in dodder seeds for health care wine. Background Art

[0002] Dodder is a traditional Chinese medicine, which has the effects of tonifying the liver and kidney, benefiting essence, improving eyesight, etc., and has a wide range of applications in the field of health care wine. The 2020 edition of the Pharmacopoeia of the People's Republic of China requires hyperoside as a quality control index, indicating that hyperoside plays an important role in the efficacy of dodder. As one of the main active ingredients in dodder, hyperoside has various health care functions, such as improving cardiovascular function, antioxidant, anti-inflammatory, and can also regulate the nervous system, immune system, digestive system, etc. However, due to the hard texture and dense seed coat of dodder, it is difficult for the extraction solvent to penetrate into the seed interior. The traditional extraction method has a low extraction and transfer rate of hyperoside, resulting in the inability to fully exert the efficacy of health care wine and causing waste. There are research reports on using organic reagents combined with enzyme reagents for assisted extraction, which have problems such as the organic reagents being unsuitable as solvents for health care wine juice, complex production processes, and difficult control. In addition, for the traditional dodder extract with many impurities and poor stability after being formulated into wine, ultrafiltration membranes are usually used to remove macromolecular substances to reduce the turbidity of the feed liquid. However, due to the high oil content in dodder, during the ultrafiltration membrane filtration process, there is a large loss of hyperoside, slow separation speed, large pollution, difficult cleaning, and low membrane life.

[0003] CN201410120975.8 discloses a preparation method of dodder extract. This method uses water adjusted to pH 3 - 4 with glacial acetic acid as a solvent, and then adds cellulase or pectinase for enzymatic hydrolysis extraction, and obtains the dodder extract through concentration and drying. This method can increase the extraction rate of hyperoside in dodder by 30%, but the extraction solvent is glacial acetic acid, which is an organic solvent, not edible, and pollutes the environment. Secondly, the enzymatic hydrolysis process is used for extraction, and the process is complex. Summary of the Invention

[0004] In view of this, the purpose of the present invention is to provide a method that can effectively improve the extraction and transfer rate of hyperoside for the problem of low extraction and transfer rate of hyperoside and slow separation speed during the preparation process of dodder extract for health care wine.

[0005] The technical solution of the present invention is realized as follows: The present invention provides a method for improving the extraction and transfer rate of hyperoside in dodder seeds for health care wine, including the following steps:

[0006] Step 1: Feed the dodder raw material into a preheated press, cool after pressing, and take the pressed dodder;

[0007] Step 2: Put the squeezed dodder seeds into an extraction tank, add extraction solvent and soak them;

[0008] Step 3, heating and refluxing for 1-3 times, combining the extracts, cooling the extracts to room temperature and then coarse filtering to obtain a coarse filtrate;

[0009] Step 4, the crude filtrate is filtered through an ultrafiltration membrane to obtain an ultrafiltrate, the retentate is top-washed twice with an extraction solvent to obtain a top-wash liquid, and the ultrafiltrate and the top-wash liquid are combined to obtain an ultrafiltration membrane separation liquid;

[0010] Step 5: Determine the content of hyperoside in the extract and the ultrafiltration membrane separation liquid respectively.

[0011] In the above embodiment, the oily substances of dodder seeds are removed by squeezing, which avoids the subsequent clogging of the filtration equipment by the oil and the negative impact on the efficiency of the separation process. The squeezing method is simple and efficient, and the medicinal materials obtained after squeezing will not clog the filter screen during the extraction operation.

[0012] The extraction rate of hyperoside can be improved by soaking in an extraction solvent before reflux extraction.

[0013] In some embodiments, the preheating temperature of the press is 120-220 degrees Celsius, and the preheating time is 10-120 minutes.

[0014] In some embodiments, the pressed dodder seeds are in sheet form with a thickness of 0.1-3 mm.

[0015] In some embodiments, the extraction solvent is a 40% vol-80% vol ethanol solution.

[0016] In some embodiments, the soaking time is 2-15 hours, and the soaking temperature is 20-30°C.

[0017] In some embodiments, the extraction solvent is 4-10 times the weight of the medicinal material.

[0018] In some embodiments, the temperature of the heating reflux extraction is 40-90° C., and the extraction time is 0.5-5 h each time.

[0019] In some embodiments, the molecular weight of the ultrafiltration membrane is 10,000-50,000 Daltons, and the material of the ultrafiltration membrane is one of polyvinylidene fluoride, composite polyamide and polyether sulfone.

[0020] In some embodiments, the ultrafiltration membrane filtration temperature is 25-50° C., and the ultrafiltration membrane filtration pressure is 0.1-0.8 MPa.

[0021] In some embodiments, the extraction solvent for top wash is one time the volume of the retentate, and the top wash temperature is 25-50°C.

[0022] The present invention has the following beneficial effects compared with the prior art:

[0023] The present invention adopts a pressing method to remove the oil substances in Cuscuta chinensis, thereby avoiding the subsequent blockage of the filtration equipment by the oil and the negative impact on the efficiency of the separation process. Moreover, the pressing treatment method is simple, the pressing equipment is inexpensive, the treatment efficiency is high, and the medicinal materials obtained after pressing will not block the filter screen during the extraction operation;

[0024] Secondly, the extraction solvent adopted by the present invention is more environmentally friendly and pollution-free, and is safe and edible. The extraction process is simple and has a short cycle;

[0025] The total transfer rate of the extraction of hyperoside in Cuscuta chinensis by this method is increased from 50.8% to over 99%, and the extraction transfer rate is high. Specific Embodiments

[0026] The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. All other embodiments obtained by those of ordinary skill in the art based on the embodiments of the present invention without creative efforts shall fall within the protection scope of the present invention.

[0027] Unless otherwise defined, all technical terms and scientific terms used herein have the same meaning as commonly understood by those of ordinary skill in the technical field to which the embodiments of the present invention belong. If the definitions stated in this part are contrary to or otherwise inconsistent with the definitions stated in the patents, patent applications, published patent applications, and other publications incorporated herein by reference, the definitions listed in this part shall prevail over the definitions incorporated herein by reference.

[0028] The methods used in the following embodiments are all conventional methods unless otherwise specified. The materials, reagents, and instruments used are all conventional materials, reagents, and instruments in this field, and those skilled in the art can obtain them through commercial channels without special instructions.

[0029] When an equivalent, concentration or other value or parameter is expressed as a range, a preferred range or a range defined by a series of upper preferred values and lower preferred values, this should be understood as specifically disclosing all ranges formed by any pairing of any range upper limit or preferred value with any range lower limit or preferred value, whether or not such ranges are separately disclosed. For example, when the range "1 to 5" is disclosed, the described range should be interpreted as including the ranges "1 to 4", "1 to 3", "1 to 2", "1 to 2 and 4 to 5", "1 to 3 and 5", etc. When a numerical range is described herein, unless otherwise stated, the range is intended to include its end values and all integers and fractions within the range. In the specification and claims of this application, range limitations may be combined and / or interchanged, and if not otherwise stated, these ranges include all sub-ranges subsumed therein.

[0030] The extraction method of this application will now be further described in detail through specific examples and comparative examples. Among them, the medicinal material content of hyperin in the dodder raw materials used below is 0.3% in all cases.

[0031] Comparative Example 1

[0032] This comparative example provides a process of directly extracting without pressing and then purifying by ultrafiltration membrane filtration.

[0033] Take 10 kg of dodder raw materials, add 70% ethanol with a solvent multiple of 6 times, soak at 25°C for 12 h, then heat to 80°C and reflux extract three times, and combine to obtain 161 L of extract. The extract is cooled to 25°C, coarsely filtered, and the coarse filtrate is collected. The coarse filtrate is filtered using a Koch ultrafiltration membrane (made of polyvinylidene fluoride), with a molecular weight of 30,000, a filtration temperature of 25°C, and a filtration pressure of 0.2 MPa, to obtain 150 L of ultrafiltration membrane permeate; 10 L of retentate is backwashed 2 times with 70% ethanol with a volume of 1 times the retentate volume, and 20 L of backwash liquid is collected. The ultrafiltration permeate and the backwash liquid are combined to obtain 170 L of ultrafiltration membrane separation liquid. The operating flux of the ultrafiltration membrane filtration material is 18.4 L / h / ㎡, and the time is 4.1 h. The content of hyperin in the extract and the ultrafiltration separation liquid is detected by high performance liquid chromatography. The content of hyperin in the extract and the ultrafiltration membrane separation liquid is 110.87 mg / L and 89.57 mg / L respectively. It can be calculated that in the extract, the transfer rate of hyperin is 59.5%, from the extract to the ultrafiltration membrane separation liquid, the transfer rate of hyperin is 85.3%, and the total extraction transfer rate of hyperin is 50.8%.

[0034] Comparative Example 2

[0035] This comparative example provides a process of first pulverizing, then extracting and then purifying by ultrafiltration membrane filtration.

[0036] Take 10 kg of dodder raw materials, crush them into powder using a universal crusher, add 70% ethanol with a solvent multiple of 6 times, soak at 25°C for 12 h, then heat to 80°C and reflux extract three times, and combine to obtain 150 L of extract. Cool the extract to 25°C, filter it roughly, and collect the rough filtrate. The rough filtrate is filtered using a Koch ultrafiltration membrane (made of polyvinylidene fluoride), with a molecular weight of 30,000, a filtration temperature of 25°C, and a filtration pressure of 0.2 MPa, to obtain 140 L of ultrafiltration membrane permeate; 10 L of retentate is rinsed twice with 70% ethanol with a volume 1 time that of the retentate, and 20 L of rinse solution is collected. Combine the ultrafiltration permeate and the rinse solution to obtain 160 L of ultrafiltration membrane separation solution. The operating flux of the ultrafiltration membrane for filtering the material is 12.9 L / h / ㎡, and the time is 5.5 h. Use high-performance liquid chromatography to detect the content of hyperoside in the extract and the ultrafiltration separation solution, which are 191.40 mg / L and 142.71 mg / L respectively. In the extract, the transfer rate of hyperoside is 95.7%. From the extract to the ultrafiltration membrane separation solution, the transfer rate of hyperoside is 84.5%, and the total extraction transfer rate of hyperoside is 80.9%. However, the medicinal materials are extracted in a pulverized state. During extraction, the extraction liquid clogs the outlet, which is very unfavorable for large-scale production operations in the factory and is not ideal.

[0037] Example 1

[0038] This example provides a process of first pressing treatment, then extraction, and finally ultrafiltration membrane filtration and purification.

[0039] Turn on the oil press, set the temperature at 200°C, preheat for 120 min, then take 10.0 kg of dodder raw materials, use the oil press to press them into thin slices with a thickness of 0.2 mm, cool to room temperature, and obtain 1.0 kg of oil. Add 70% ethanol with a solvent multiple of 6 times, soak at 25°C for 12 h, then heat to 80°C and reflux extract three times, and combine to obtain 160 L of extract. Cool the extract to 25°C, filter it roughly, and collect the rough filtrate. The rough filtrate is filtered using a Koch ultrafiltration membrane (made of polyvinylidene fluoride), with a molecular weight of 30,000, a filtration temperature of 25°C, and a filtration pressure of 0.2 MPa, to obtain 150 L of ultrafiltration membrane permeate; 10 L of retentate is rinsed twice with 70% ethanol with a volume 1 time that of the retentate, and 20 L of rinse solution is collected. Combine the ultrafiltration permeate and the rinse solution to obtain 170 L of ultrafiltration membrane separation solution. The operating flux of the ultrafiltration membrane for filtering the material is 35.7 L / h / ㎡, and the time is 2.1 h. Use high-performance liquid chromatography to detect the content of hyperoside in the extract and the ultrafiltration separation solution, which are 187.31 mg / L and 175.41 mg / L respectively. In the extract, the transfer rate of hyperoside is 99.9%. From the extract to the ultrafiltration membrane separation solution, the transfer rate of hyperoside is 99.5%, and the total extraction transfer rate of hyperoside is 99.4%.

[0040] Example 2

[0041] This embodiment provides a process of first performing pressing treatment, then extraction, and finally ultrafiltration membrane filtration for purification and extraction.

[0042] Start the oil press and set the temperature at 180 °C. After preheating for 120 min, take 10.0 kg of dodder raw materials and use the oil press to press them into thin flakes with a thickness of 1.0 mm. Cool to room temperature, and 0.98 kg of oil is obtained. Add 60% ethanol with a solvent multiple of 6 times and soak at 25 °C for 12 h, then heat to 80 °C and reflux for extraction three times. Combine to obtain 161 L of extract. Cool the extract to 25 °C, perform rough filtration, and collect the rough filtrate. Filter the rough filtrate through a Koch ultrafiltration membrane (the material is composite polyamide), with a molecular weight of 50,000, a filtration temperature of 40 °C, and a filtration pressure of 0.4 MPa to obtain 151 L of ultrafiltration membrane permeate; wash the 10 L of retentate twice with 60% ethanol with a volume equal to 1 times the retentate volume, collect 20 L of washing solution, and combine the ultrafiltration permeate and the washing solution to obtain 171 L of ultrafiltration membrane separation solution. The operating flux of the ultrafiltration membrane filtration material is 32.8 L / h / ㎡, and the time is 2.3 h. Use high-performance liquid chromatography to detect the contents of hyperoside in the extract and the ultrafiltration separation solution, which are 185.96 mg / L and 175.24 mg / L respectively. In the extract, the transfer rate of hyperoside is 99.8%. From the extract to the ultrafiltration membrane separation solution, the transfer rate of hyperoside is 99.5%, and the total extraction transfer rate of hyperoside is 99.3%.

[0043] Example 3

[0044] This embodiment provides a process of first performing pressing treatment, then extraction, and finally ultrafiltration membrane filtration for purification and extraction.

[0045] Turn on the oil press, set the temperature to 160 °C, and after preheating for 120 min, take 10.0 kg of dodder raw materials, use the oil press to press them into thin slices with a thickness of 3.0 mm, cool to room temperature, and obtain 0.95 kg of oil. Add 50% ethanol with a solvent multiple of 6 times and soak at 25 °C for 12 h, then heat to 80 °C and reflux extract three times, and combine to obtain 162 L of extract. Cool the extract to 25 °C, filter it roughly, and collect the rough filtrate. The rough filtrate is filtered through a Koch ultrafiltration membrane (the material is composite polyamide), with a molecular weight of 50,000, a filtration temperature of 50 °C, and a filtration pressure of 0.3 MPa, to obtain 152 L of ultrafiltration membrane permeate; 10 L of retentate is rinsed twice with 70% ethanol with a volume of 1 times the retentate volume, and 20 L of rinsing solution is collected. Combine the ultrafiltration permeate and the rinsing solution to obtain 172 L of ultrafiltration membrane separation solution. The operating flux of the ultrafiltration membrane filtration material is 31.6 L / h / ㎡, and the time is 2.4 h. Use high performance liquid chromatography to detect the contents of hyperoside in the extract and the ultrafiltration separation solution, which are 184.44 mg / L and 175.24 mg / L respectively. In the extract, the transfer rate of hyperoside is 99.6%. From the extract to the ultrafiltration membrane separation solution, the transfer rate of hyperoside is 99.7%, and the total extraction transfer rate of hyperoside is 99.3%.

[0046] Example 4

[0047] This example provides a process of first pressing treatment, then extraction and finally ultrafiltration membrane filtration and purification extraction.

[0048] Turn on the oil press, set the temperature to 200 °C, and after preheating for 120 min, take 10.0 kg of dodder raw materials, use the oil press to press them into thin slices with a thickness of 2.0 mm, cool to room temperature, and obtain 0.97 kg of oil. Add 70% ethanol with a solvent multiple of 6 times and soak at 25 °C for 12 h, then heat to 80 °C and reflux extract three times, and combine to obtain 163 L of extract. Cool the extract to 25 °C, filter it roughly, and collect the rough filtrate. The rough filtrate is filtered through a Koch ultrafiltration membrane (the material is composite polyethersulfone), with a molecular weight of 50,000, a filtration temperature of 45 °C, and a filtration pressure of 0.4 MPa, to obtain 153 L of ultrafiltration membrane permeate; 10 L of retentate is rinsed twice with 70% ethanol with a volume of 1 times the retentate volume, and 20 L of rinsing solution is collected. Combine the ultrafiltration permeate and the rinsing solution to obtain 173 L of ultrafiltration membrane separation solution. The operating flux of the ultrafiltration membrane filtration material is 34.7 L / h / ㎡, and the time is 2.2 h. Use high performance liquid chromatography to detect the contents of hyperoside in the extract and the ultrafiltration separation solution, which are 183.50 mg / L and 175.59 mg / L respectively. In the extract, the transfer rate of hyperoside is 99.7%. From the extract to the ultrafiltration membrane separation solution, the transfer rate of hyperoside is 99.8%, and the total extraction transfer rate of hyperoside is 99.5%.

[0049] The comparison results of the above examples and comparative examples show that before reflux extraction, the primary extraction rate of hyperin in Cuscuta chinensis can be significantly improved by pressing, and at the same time, compared with the pulverization treatment method, the filtration speed of the ultrafiltration membrane can be significantly increased, thereby improving the extraction efficiency.

[0050] The above is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims

1. A method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine, characterized in that: The steps include: Step 1, feeding the dodder raw material into a preheated squeezer, cooling after squeezing, and taking the squeezed dodder; Step 2: Put the squeezed dodder seeds into an extraction tank, add extraction solvent and soak them; Step 3, heating and refluxing for 1-3 times, combining the extracts, cooling the extracts to room temperature and then coarse filtering to obtain a coarse filtrate; Step 4, the crude filtrate is filtered through an ultrafiltration membrane to obtain an ultrafiltrate, the retentate is top-washed twice with an extraction solvent to obtain a top-wash liquid, and the ultrafiltrate and the top-wash liquid are combined to obtain an ultrafiltration membrane separation liquid; Step 5: Determine the content of hyperoside in the extract and the ultrafiltration membrane separation liquid respectively.

2. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The preheating temperature of the press is 120-220 degrees Celsius, and the preheating time is 10-120 minutes.

3. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The pressed dodder is in sheet form with a thickness of 0.1-3 mm.

4. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The extraction solvent is 40% vol-80% vol ethanol solution.

5. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The soaking time is 2-15h, and the soaking temperature is 20-30℃.

6. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The extraction solvent is 4-10 times the weight of the medicinal material.

7. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The temperature of the heating reflux extraction is 40-90°C, and the extraction time each time is 0.5-5h.

8. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The molecular weight of the ultrafiltration membrane is 10,000-50,000 Daltons, and the material of the ultrafiltration membrane is one of polyvinylidene fluoride, composite polyamide and polyether sulfone.

9. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The ultrafiltration membrane filtration temperature is 25-50°C, and the ultrafiltration membrane filtration pressure is 0.1-0.8MPa.

10. The method for improving the extraction transfer rate of hyperoside in Cuscuta australis for health wine according to claim 1, characterized in that: The extraction solvent used for top washing is one times the volume of the retentate, and the top washing temperature is 25-50°C.