supercritical co2 extraction machine

Research on supercritical CO2 extraction of propolis active ingredients

The optimized conditions for the supercritical extraction of propolis are:

Extraction temperature:50 ° C,

Extraction pressure:25 MPa,

Entrainer:95% ethanol,

Solid-liquid ratio:6: 1.

Propolis was extracted under the optimal conditions, and the flavonoid content of the obtained extract was 14.8%.

Introduction

supercritical co2 extraction equipment
supercritical co2 extraction equipment

Propolis is resin (gum) collected by bees from plant spores or tree trunks, mixed with secretions from the upper glands and wax glands, and processed into a gel-like solid with an aromatic odor. It has a complex and unique chemical composition. Modern scientific research has confirmed that the chemical composition of propolis can be basically classified into more than 20 types and more than 200 single substances. These include more than thirty aromatic esters, more than thirty flavonoid compounds, and more than thirty human essential trace elements such as selenium, calcium, zinc, iron, manganese, copper, strontium, and magnesium, and nearly twenty amino acids; more than ten Aromatic acids, beeswax, terpenes, fatty acids, and fatty acid esters; several types of sterols, alcohols, aldehydes, sugars, and ketones; and a variety of phenols, steroids, enzymes, vitamins , Alkenes, hydrocarbons and other biologically active organic compounds. Obviously, propolis is a natural "small medicine storehouse" with great potential.

Propolis has become a research hotspot for scientists from all over the world for its unique medical and health benefits. At present, the traditional process of extracting propolis collagen from alcohol, which is still in use at home and abroad, is widely used at present. This process is superior to the production method of water-extracted propolis solution. The research of extracting the effective components of propolis by supercritical CO2 fluid technology is in the exploration and tackling stage. The use of supercritical CO2 fluid extraction to extract propolis flavonoids has many advantages: light yellow color, no solvent residue, safety and health, less impurities, low heavy metal content, simple process and so on. However, using supercritical fluid extraction technology, the extract is a substance that is fat-soluble and hardly soluble in alcohol, has low flavonoid content, and is gelatinous and has anti-strain activity. Under the experimental conditions, the content of flavonoids in the extract is approximately 1/5 or less of the same raw material ethanol extraction. Therefore, it can only be explained that the simple supercritical fluid extraction technology is suitable for the extraction of hue, flavor and taste food or processed food materials. It is because of the extremely low solubility of flavonoids, lactones and polysaccharides, proteins, and tannins in supercritical fluid CO2 that they need to be dissolved under high pressure. Therefore, for solutes with very low solubility in supercritical fluids, it is necessary to add a small amount of entrainer to the supercritical fluid system to change the phase behavior of the supercritical fluid system in order to achieve the purpose of greatly increasing its solubility. In view of the non-toxicity of ethanol, its solubility in SFE is large, and it is easy to use SFE for separation and other characteristics. Ethanol is selected as the preferred entrainer. Although the entrainer brings benefits to supercritical fluid extraction technology, the separation of the entrainer mixed in the extractant and the recovery of the entrainer present in the residue will increase some equipment and energy consumption. Therefore, it is very important to study the influence of the amount of entrainer and its concentration on the extraction effect. In this paper, we will carry out research on the extraction technology of flavonoids in propolis with supercritical fluid extraction technology containing entrainer, in order to achieve the purpose of low extraction temperature, few organic solvents, short time and high preservation of propolis flavonoids.

Efficacy and project significance of propolis

The biggest feature of propolis is that it is rich in flavonoids and terpenoids, especially the type and content of flavonoids. It ranks first among all natural products recognized by human beings, and the content can reach 8%. More than 20 kinds. They give propolis many wonderful and unique biological effects. At the same time, propolis is a kind of "drug-food homologous", which is an advanced product with obvious physiological and pharmacological effects. A large number of basic and clinical studies have proven that propolis has no toxic side effects on normal human life cells and is safe and reliable to eat. The complex chemical composition of propolis inevitably determines that it has magical health care effects and is a rare natural medicine.

Propolis flavonoids (PF) PF has a strong immune-enhancing activity, and is an effective ingredient in propolis to enhance the immune effect. In terms of regulating microecology, improving microcirculation, promoting wound healing and tissue regeneration, propolis has also shown extraordinary efficacy. In addition, propolis also has unique prevention and treatment effects on a variety of chronic diseases such as hyperlipidemia, hyperglycemia, hypertension, cardiovascular and cerebrovascular diseases, and cancer. These effects make propolis a bright star in human health.

Market economic benefits of propolis

Propolis is a very rare natural resource. The amount of bees collected by a bee is only 0.01 grams at a time, and the annual harvest of a large group of tens of thousands of bees is only 50-60 grams. About this amount of propolis It can ensure the health of hundreds of thousands or even millions of bees. It is a super healthy product. The world's annual output of gold is about 2500 to 2600 tons, while the global annual production of propolis raw materials is only 400 tons. Excluding impurities, only half of the really useful part is about 200 tons, which is equivalent to eleventh of the gold output. Judging from the rule of the value of the commodity as "thin is rare," the price of propolis should exceed gold. In fact, the value of propolis products in many developed countries has long overshadowed gold and platinum, and the price of pure gum per gram is as high as 300-400 yuan or more. From another perspective, health is the most precious wealth in life, and propolis can have a significant impact on human health and longevity. Therefore, it is a well-deserved "purple soft gold".

With the challenges facing China's entry into the WTO after the start of the Western Development Project, it is imperative to develop high-tech, high value-added, high-end "three high" products. Therefore, there is an urgent need to establish beekeeping bases and bee product processing bases centered on beekeeping science and technology and international standardization, with bee product processing and operating enterprises as the main body, providing technical training and guidance to bee farmers, upgrading and transforming traditional crafts, and updating Equipment, to achieve bee industry base, organization, scientific, standardization and scale, strengthen the quality control throughout the process, and regain the initiative in the international market. The development of bee products will also help Chinese agricultural products break international green trade barriers, increase the international competitiveness of Chinese agricultural products, and increase exports.

supercritical co2 extraction of propolis
supercritical co2 extraction of propolis

Experimental scheme of supercritical CO2 extraction of active ingredients in propolis

Supercritical CO2 has a density similar to that of a liquid, a large solubility, but a viscosity similar to that of a gas, and a large diffusion coefficient. The use of supercritical CO2 can extract effective components in plant tissues at a lower temperature, and is particularly suitable for the extraction of heat-sensitive components. The supercritical CO2 extraction method has a short extraction process, low extraction temperature, and a closed system. The supercritical CO2 extraction process can improve the yield of fat-soluble components of ethanol leachables, which is an effective method for the extraction and research of the chemical constituents of Chinese herbal medicines [47].

1. Experimental methods

Take an appropriate amount of propolis raw material that has been de-doped and waxed in advance, crush and pass through a 4 mesh sieve. Take the propolis powder and magnesium stearate, mix them in a tank mixer and transfer them to the extraction kettle. Turn on the plunger pump and related equipment of the supercritical CO2 extraction device, pressurize and heat CO2, and make it extract the propolis in the extractor in a supercritical fluid state.

The effects of different extraction pressure, extraction temperature, ratio of raw materials to auxiliary materials, separation pressure, separation temperature, extraction time, and flow rate on the extraction rate were investigated during the experiment.

2. Effect of extraction time on total flavonoid content in propolis extract

At an extraction temperature of 55 ° C, an extraction pressure of 25 MPa, 70% ethanol as the entrainer, and a solid-liquid ratio of 7: 1 (w / v), the propolis was extracted for 2hr, 311r, and 411r, and the extracts were measured separately. The total flavonoid content is shown in Table 2-1.

Table 2.1 Effect of extraction time on flavonoid content

Extraction time (hr)

2

3

4

Flavonoid content (g / 100g)

10.1

11.3

11.2

As can be seen from Table 2.1, the flavonoid content of the extract reached a maximum when the extraction reached 3 hr. As the extraction time continues to increase, the flavonoid content of the extract decreases. It may be that with the extension of the extraction time, the amount of other substances extracted increases, while the flavonoids no longer increase, resulting in a decrease in the mass percentage of the extract. .

3. Effect of entrainer infiltration time on total flavonoid content in propolis extract

At an extraction temperature of 55 ° C, an extraction pressure of 30 MPa, 95% ethanol as the entrainer, and a solid-liquid ratio of 5: 1 (w / v), the propolis was impregnated with the entrainer for different times, and then extracted, and then The total flavonoid content of the extract was measured, and the results are shown in Table 2.2.

Table 2-2 Effect of ethanol infiltration time on flavonoid content

Ethanol infiltration time (d)

0

1

3

Flavonoid content (g / 100g)

12.5

12.4

12.3

It can be seen from Table 2.2 that the flavonoid content of the extract is the highest without infiltration. The reason may be the infiltration of ethanol, and more of the non-flavonoid polar substances are dissolved. In the case of extraction, as the infiltration time is extended, the content of these substances gradually increases, which makes the total flavonoid content of the extract decrease.

4. orthogonal experiment optimization

Through single factor experiments, it was determined that the critical extraction of super I used the entrainer non-wetting method to extract propolis for 3hr. Relevant literature shows that only when the temperature and pressure of supercritical extraction are above 45 ° C and 20 MPa, respectively, can flavonoids be extracted more; and the excessive temperature and pressure are contrary to the experimental goals. Therefore, the temperature and pressure ranges selected in the experiment were 45 ° C to 55 ° C and 20 to 30 MPa, respectively. The amount of entrainer is referenced in the literature. The solid-liquid ratio is 5: 1 to 7: l (w / v).

Orthogonal table L9 was used to perform orthogonal experiments on the extraction temperature, extraction pressure, entrainer type, and solid-liquid ratio of several main factors in the extraction conditions of propolis.

Table 2-3 Factor levels of orthogonal experiments for propolis supercritical extraction

Factor level

A

Extraction temperature (℃)

B

Extraction pressure (MPa)

C

Entrainer type

D

Solid-liquid ratio (g / ml)

1

45

20

70% ethanol

5:1

2

50

25

95% ethanol

6:1

3

55

30

100% ethanol

7:1

 

Table 2-4 Orthogonal experiment results

Experiment No.

A

Extraction temperature(℃)

B

Extraction pressure (MPa)

C

Entrainer type

D

Solid-liquid ratio

Flavonoid content (g / 100g)

1

1

1

1

1

7.2

2

1

2

2

2

11.1

3

1

3

3

3

10.9

4

2

1

2

3

12.2

5

2

2

3

1

13.4

6

2

3

1

2

12.2

7

3

1

3

2

11.2

8

3

2

1

3

11.3

9

3

3

2

1

12.5

k1

9.733

10.200

10.233

11.033

 

k2

12.600

11.933

11.933

11.500

 

k3

11.667

11.867

11.833

11.467

 

R

2.867

1.733

1.700

0.467

 

The analysis shows that the range of A (extraction temperature) is the largest, followed by B (extraction pressure), C (entrainer type), and D (solid-liquid ratio). The major and minor factors determine the range of the range: A> B> C> D, the best combination is A2B2C2D2. Therefore, based on the comprehensive test results and the economic benefits of the manufacturing company, the optimal conditions for the optimized supercritical extraction of propolis were determined as follows: the extraction temperature was 50 ° C, the extraction pressure was 25 MPa, the entrainer was 95% ethanol, and the solid-liquid ratio was 6: 1. Propolis was extracted under the optimal conditions, and the flavonoid content of the obtained extract was 14.8%.

5. Project evaluation

This project is the physical processing of raw materials. The raw material utilization rate is high, no toxic substances are discharged, no sewage is emitted, and noise occurs within the national control standards. In the production process, there is only a small amount of packaging waste and leftover waste, such as centralized processing, landfilling, incineration, and waste disposal stations, which can not cause pollution. And propolis products have a broad market and great economic benefits, which is indeed a good project.

co2 extraction system

Related Posts

Study on Supercritical CO2 Fluid Extraction of Sardine Oil

The sardine fish oil was extracted by supercritical extraction method, and the effects of extraction pressure, extraction temperature and extraction time on the extraction of sardine fish oil were investigated to obtain the best process of supercriti..

The advantages of supercritical CO2 extraction and its application in the tobacco industry

The supercritical CO2 extraction method is used to extract valuable components such as nicotine and tobacco net oil, which can play a role of turning waste into treasure and comprehensive utilization, improving the comprehensive benefits of tobacco, ..

Supercritical Carbon Dioxide Extraction of Grape Seed Oil

Supercritical fluid is a kind of material state above the critical temperature and pressure. In this state, the properties of substances will change to some extent. Supercritical fluid extraction (SFE) applies the fact that the solubility of SFE chan..

Research Progress of Supercritical CO2 Fluid Extraction Technology in Vegetable Oil Extraction

The supercritical co2 fluid extraction refers to the fluid state when the material is above its critical temperature and pressure. This fluid has the advantages of both liquid and gas, high density, low viscosity, low surface tension, and extremely h..

Extraction of Rose Essential Oil by Supercritical CO2 Fluid

Rose extract was extracted by supercritical CO2 fluid extraction (SFE) and refined by molecular distillation (MD). The obtained rose essential oil was pale yellow, and the yield increased from 0.03% to 0.1% by traditional steam distillation. The opti..

Large scale super critical co2 extraction machine

Supercritical CO2 extraction system is used under high pressure and suitable temperature suitable to extract valuable content from material (solid or liquid), it is to change the pressure and temperature conditions of the separator tanks to let the d..