SICHUAN UNIWELL BIOTECHNOLOGY CO.,LTD. , https://www.uniwellbio.com
(11 State Key Laboratory of Biochemical Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100080, China;
21 Beijing Hongxianglong Biotechnology Development Co., Ltd., Beijing 100083, China)
After China's accession to WTO, Chinese medicine and natural product manufacturers must adopt advanced extraction and separation technologies in order to win the initiative. For this reason, the country has adopted extraction and separation technology as one of the key technologies for future development. In developed countries, the medicinal materials are started from the feeding, and the whole operation process is carried out in a continuous closed environment.
The degree of automation is high, and the pulverized medicinal materials are regularly put into the extraction device, and the extract is continuously discharged from the extraction tank, and the liquid medicine and the dregs are all run in the closed pipeline.
It keeps the environment clean and tidy, improves the utilization rate of the medicinal materials, and its extraction efficiency is 3 to 4 times that of the conventional method. The whole production process is controlled by computer, which avoids the instability of product quality caused by human factors, so the products are internationally competitive.
With the interdisciplinary multi-disciplinary and in-depth study of the extraction of raw materials and processes,
The new extraction technology has emerged and applied, contributing to the improvement of the quality and technical content of Chinese traditional medicine products. One of them is the circulating ultrasonic technology, which solves the engineering amplification problem of ultrasonic extraction, greatly improves the ultrasonic field strength, the utilization of ultrasonic materials and the uniformity of ultrasonic treatment of materials. Beijing Hongxianglong Biotechnology Development Co., Ltd. and China The Institute of Process Engineering of the Academy of Sciences has successfully applied cyclic ultrasonic extraction equipment to industrial production.
1 Basic principle and problems of ultrasonic extraction When high-energy ultrasonic waves act on the extraction medium, when the vibration is sparse, the medium is torn into many small holes, which are closed instantaneously and up to several thousand when closed. The instantaneous pressure of atmospheric pressure is cavitation. The strengthening effect of ultrasonic on the extraction and separation of various components is mainly due to its cavitation.
The extreme pressure generated by the bursting of tiny bubbles in the cavitation causes the rupture of the cell wall and the whole organism to be broken in an instant, shortening the breaking time, and the vibration generated by the ultrasonic waves enhances the release, diffusion and dissolution of intracellular substances.
Can significantly improve the extraction efficiency. The ultrasonic disruption process is a physical process in which no chemical reaction occurs and the biologically active material being extracted remains unchanged.
During the cavitation, the tiny bubble nuclei in the liquid oscillate, grow, shrink and collapse under the action of high-intensity ultrasonic waves, and generate high temperature and high pressure around the cavitation bubbles in a very short time of collapse. , strong shock wave and micro-jet flow above 400 kmöh, peeling off the solid surface,
The etch and pulverization creates a new active surface that increases the mass transfer surface area. The turbulence effect generated during cavitation makes the mass transfer boundary layer in the solid-liquid interface thin, resulting in a much faster reduction of the concentration gradient of solute in the interface layer than other methods. The perturbation effect caused by cavitation enhances the micropore diffusion in the solid-liquid mass transfer process, which enhances the eddy diffusion and accelerates the extraction process. The ultrasonic frequency is increased,
The extraction time is prolonged, and the energy-concentration effect generated by the ultrasonic field causes the temperature of the extract to rise. Turbulence effects, perturbation effects, interfacial effects, and energy-concentration effects are related to the frequency, power, and temperature of the system. In the natural product extraction process, the cell wall breakage, the diffusion of the solute and the equilibrium velocity are related to the ultrasonic power per unit area, and both have an effect on the extraction efficiency and the recovery rate. Therefore, low-frequency high-power ultrasound is generally used.
Although ultrasonic extraction is very effective in the preparation of small samples in the laboratory and has been widely used, especially in the processing of analytical samples, its fast and efficient characteristics have been widely recognized, but the range and intensity of the ultrasonic field limit each time. The amount of material processed, the lack of effective engineering amplification methods and methods limit its application in large-scale production.
2 Development of Cyclic Ultrasonic Extraction Technology Researchers of the State Key Laboratory of Biochemical Engineering, Institute of Process Engineering, Chinese Academy of Sciences, aiming at the problem of engineering amplification in China's current ultrasonic extraction process, in the national “863†and “Ninth Five-Year Plan†projects With the support of algae sulfate polysaccharide and artemisinin, the characteristics of various ultrasonic extractions were systematically studied. The principle of biochemical engineering and technology were used to solve the engineering amplification problems existing in traditional ultrasonic extraction. A number of patented technologies. Beijing Hongxianglong Biotechnology Development Co., Ltd. (ht tp: ööw ww. hxlbd. com) further developed a series of new high-efficiency countercurrent circulating ultrasonic extraction devices suitable for Chinese herbal medicine extraction enterprises based on the original patent technology, and applied for And obtained a number of related patents. It has been formed from a few hundred milliliters to 5 000 L
The effective volume of SY, HF, SC three series of more than 20 products, has been used by dozens of domestic units, and has won the bid in the government tender procurement.
Due to the solution of the ultrasonic extraction engineering amplification problem, the application range of ultrasonic extraction has been greatly expanded. Circulating ultrasound technology and equipment are not only suitable for the extraction of various natural products, but also for ultrasonic dispersion, emulsion preparation, sustained-release drug ultra-microcapsules and nanocapsule preparation, etc., and the application fields are extended to medicines, health products, cosmetics, foods and A number of areas such as deep processing of agricultural products.
3 Characteristics of cycle ultrasonic extraction technology and equipment The main parameters of extraction time, extraction temperature, ultrasonic power and circulation speed of the new high-efficiency cyclic ultrasonic extraction device can be set and automatically controlled. The extraction efficiency is several times to several tens of times that of conventional extraction. The extraction temperature can be reduced from 100 °C to room temperature (the SY series products can also achieve low temperature extraction), and the equipment performance has reached the international advanced level. Compared with the traditional method, the energy consumption can be saved by more than 50%, and the extraction cost can be reduced by more than 25%. Intermittent extraction and multi-stage continuous dynamic extraction, the material is run in a closed pipeline, the extract and dregs are continuously discharged, and the liquid 2 solid is continuously and automatically separated, which can realize manual, semi-automatic and fully automatic control, which can save a lot of labor and conform to GM P Claim.
Through a large number of experiments, compared with related equipment at home and abroad, the cyclic ultrasonic extraction technology and equipment have significant features and advantages, including: 1) ACT · 154 · Chinese herbal medicine Ch inese T radit ional and HerbalD rugs Vol. 37 No. 1 January 2006
X Received date: 2005207220
High rate: The extraction time is short, and the extraction time is only a fraction to a few tenths of the conventional extraction method. 2) Low extraction energy consumption: Small power ultrasonic waves can be used to crush and extract a large amount of materials, which are generally extracted at room temperature. Without high-power stirring and heating, the energy consumption can be reduced by more than 50% compared with conventional extraction methods. 3) High quality of extracted products: zui
The activity of various active ingredients is maintained to a large extent, and in particular, various heat-sensitive ingredients can achieve the purpose of improving the efficacy and reducing the dosage. At the same time, due to the short extraction time, the reduction of other useless components in the extracted product can significantly reduce the production cost of other high-end products such as single components. 4) High extraction rate of target extract: Due to the ultrasonic disruption extraction technology, the active ingredient in the medicinal material is fully released, so that the extraction rate of the target extract is improved. Even some components that are difficult to extract by conventional methods can be quickly extracted. 5) Wide range of applications: It is suitable for both volatile and non-volatile extraction media. It is suitable for experimental research, pilot test and industrial production of various natural product extractions, and is not limited by the relative molecular mass and polarity of the extract. 6) High degree of automation and easy operation: Intermittent extraction or multi-stage continuous extraction. The main parameters such as extraction time, extraction temperature and circulation speed can be set and automatically controlled, which reduces the influence of human factors on product quality and helps to ensure product quality. In the multi-stage continuous dynamic extraction, the extract and dregs operate under fully enclosed conditions, which can save a lot of labor and conform to GM P
Claim. 7) High cost performance of the product: The price of the circulating ultrasonic extraction device is much lower than that of the supercritical CO 2 extraction and import equipment. The equipment occupies a small area and does not require auxiliary facilities such as steam, thus saving investment. See Table 1 for comparison of circulating ultrasound techniques and equipment with other major ultrasonic extraction equipment.
Table 1 Comparison of circulating ultrasonic extraction equipment with other ultrasonic equipment
Table 1 Compar ison of equipmen ts between c irculation ultrason ic extraction and other ultrason ic extraction s
Comparing the project cycle ultrasonic other ultrasonic shape with the conventional extraction tank pipeline type, drag chain ultrasonic type concentrating ultrasonic, single transducer power 900 ~ 1 800W, zui high reach
2 800W. The power intensity per unit area is ten times that of divergent ultrasonic waves. It can meet the requirements of various cell wall breaking requirements. It is mainly used for ultrasonic cleaners. The power of a single transducer is small.
Generally only a few to several tens of watts, it is difficult to meet various cell breakage requirements and material contact. The energy-collecting transducer is directly in contact with the material, and the ultrasonic utilization efficiency is 100%.
All materials are in the effective range of the ultrasonic field, the material is pseudo-homogeneous, and the ultrasonic processing opportunities are equal. The ultrasonic transducers are embedded in the pipe wall, the extraction tank wall, etc., and the ultrasonic waves need to pass through the wall to the material, and the ultrasonic field only Distributed over a small portion of the circumference of the tube,
Ultrasonic utilization is low, some materials can not accept ultrasonic waves, and some of the ultrasonic field can be reversed or flowed in the direction of ultrasonic treatment. The ultrasonic field has no effect other than the mixture. The moving direction of the moving material and the ultrasonic material is perpendicular to the ultrasonic field. In the pipeline equipment, the ultrasonic wave is formed by the propelling spiral and the like, and the material is driven to form a uniform liquid-solid suspension in the circulating ultrasonic device, similar to the pseudo-average Phase, circulating through the high-intensity ultrasonic field, so that the material has the same extraction opportunity, the material pushes the power to consume the small pipeline equipment. The material moves upwards by the spiral, and the liquid depends on the high difference, due to the height difference, flow and ultrasonic vertical The relationship between the functions, some of the fine materials are difficult to reach the top, resulting in poor material mixing uniformity and excessive crushing, and high power consumption. The floor space is compact, the floor space is small, and the height is similar to that of the traditional extraction tank. Circulating speed and extraction time arbitrarily adjustable pipeline equipment to ensure sufficient ultrasonic extraction time takes a long time The pipe and the sufficient height difference, so the floor space is large, the high requirements for the plant are applicable to the volatile and non-volatile solvent extraction of various components, fully enclosed operation,
Good adaptability to a wide range of materials, especially fine materials, from 1 000
There are series of complete sets of equipment from mL to 5 000 L, which can meet the requirements of laboratory, pilot test and large-scale production and use. Pipeline equipment is generally suitable for pilot scale. It can not meet the requirements of small sample extraction in laboratory, and it is difficult to achieve large scale. And ultra-large-scale extraction, and for the application of strong volatility solvents, fine materials and other poor applications, there are dozens of actual users, from 1 000 mL to 3 000 L devices have been successfully applied, including domestic famous universities Research institutes, pharmaceutical companies, and bioengineering companies have gradually acquired other ultrasonic extraction equipments such as well-known pipeline equipment in the world. At present, the actual number of users is relatively small, and there is still a lack of industrialized large-scale production.
4 The series of circulating ultrasonic extraction equipment has been continuously developed. The circulating ultrasonic extraction equipment produced by Beijing Hongxianglong Biotechnology Development Co., Ltd. has basically formed a relatively complete product series.
It mainly includes the SY series for laboratory use, the HF series for pilot test, and the SC series for industrial production. Currently, there are nearly 20 products. There are two kinds of circulation modes: countercurrent and downstream, and the circulation speed, ultrasonic intensity, extraction temperature, etc. can be adjusted. Product users are distributed in universities, research and design institutes, production enterprises, etc. across the country. The specific products of each series are shown in Table 2.
5 Circulating ultrasonic extraction technology and equipment in the development and production of traditional Chinese medicine The first condition for extracting natural ingredients from traditional Chinese medicine is that the extract can enter the extraction medium quickly and efficiently, because the active ingredients of traditional Chinese medicine are mostly intracellular products.
It is generally necessary to destroy the raw cell wall during the extraction process. The circulating ultrasonic extraction technology device has been successfully used for the extraction of natural products from dozens of Chinese herbal medicine raw materials. Some results are shown in Table 3.
The above test results show that the circulating ultrasonic extraction device has good amplification performance, and the extraction results of the same equipment under different process conditions may be quite different, so it is necessary to optimize the process for different extraction raw materials and extracts.
Table 2 series of equipment for circulating ultrasound
Table 2 Var ious equipmen ts of c irculation
Ultrason ic extraction
Series model effective volume remarks
SY Series ST2500 500 mL Coolable and Heatable (Lab) SY21000 1 000 mL Coolable and Heatable
HF Series HF22B 2 L Electric Heating (Pilot or Production) HF25B 5 L Electric Heating
HF210B 10 L electric heating
HF220B 20 L electric heating
HF250B 50 L electric heating
HF2100B 100 L electric heating
HF2200B 200 L electric or steam heating
HF2500B 500 L electric or steam heating
HF210G 10 L extraction, extraction, electric heating
HF220G 20 L extraction, extraction, electric heating
HF250G 50 L extraction, extraction, electric heating
HF2100G 100 L extraction, extraction, electric heating
HF2200G 200 L extraction, extraction, electric or steam heating
HF2500G 500 L extraction, extraction, electric or steam heating
SC Series SC2500 500 L Electric or Steam Heating (Production) SC21000 1 000 L Steam Heating
SC23000 3 000 L steam heating
SC25000 5 000 L Steam-heated Chinese herbal medicine Ch inese T radit ional and HerbalD rugs Vol. 37 No. 1 January 2006 · 155·
Table 3 Partial results of circulating ultrasound extraction of traditional Chinese medicine
Table 3 Some results of extraction of by c irculation ultrason ic equipmen ts
Raw material extract conditions Equipment specification extraction rate Remarks Artemisia annua L. Artemisin 20 m in HF22B ≥90% Conventional 60% About Ginkgo biloba leaf flavonoids room temperature, 10 m in HF22B 82. 6% Conventional boiled for 4 h
Extraction rate at room temperature, 30 m in 88.3%
40 °C, 30 m in HF250G 91. 6% 56. 5%
Propolis flavonoids room temperature, 30 m in HF22B 41. 8% conventional 48 h is 36%
Epimedium Flavonoids 30 °C, 30 m in HF22B 87%
Licorice Flavonoids Room Temperature, 60 m in HF220B 11.5% (yield)
Sand oyster alkaloid room temperature, 30 m in HF22B 85%
Cistanche Cinnabetaine 40 ° C, 10 m in HF22B 13. 65% (yield) Boiling water reflux for 7 h is 131. 5 mgög
Phenylethanol glycoside 40 °C, 20 m in HF22B 7. 38% (yield) equivalent to extraction at 60 °C for 5 h
Epimedium icariin 30 ° C, 30 m in HF22B 90% 50% ethanol kelp sulfate polysaccharide 30 ° C, 20 m in HF22B 2. 8% (yield) equivalent to cooking 4 h
Cistanche polysaccharide 40 ° C, 10 m in HF22B 4. 69% (yield) boiling water reflux 7 h is 43. 7 mgög
Kelp sulfate polysaccharides at room temperature, 30 m in HF22B 90%, fucose ≥ 35% solvent in the pulp extraction direct purification of pepper room temperature, 40 m in HF220B absorbance of 2. 053 boiled for 8 h, absorbance of 2. 274
Cigarette factory waste benzyl alcohol, phenylethyl alcohol,
Kiwi lactone,
Large column trienolone,
The peak areas of heptanoic acid at room temperature and 30 m in SC23000 HPLC were
942, 1 021, 84, 1 607, 22
The conventional numbers are 877, 1 004, 74, respectively.
1 206, 3. 2
6 Conclusion The ultrasonic extraction technology and equipment effectively solve the problem of ultrasonic extraction engineering amplification, which lays a foundation for the application of ultrasonic extraction in large-scale production of traditional Chinese medicine. In addition, it can also be used for ultrasonic dispersion, emulsion preparation and sustained release drug super. Preparation of microcapsules and nanocapsules, etc. Due to its good use, circulating ultrasonic extraction equipment is being used by more and more universities, research institutes and manufacturing companies. Its application fields have been extended to many fields such as pharmaceuticals, health products, cosmetics, food and deep processing of agricultural products. Compared with other related technologies, it has significant technical and economic advantages, and therefore has broad application prospects.
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Circulating Ultrasound Technology and Its Application in R&D and Production of Traditional Chinese Medicine
Circulating Ultrasound Technology and Its Application in R&D and Production of Traditional Chinese Medicine Zhao Bing1, Yin Hui 2X