supercritical co2 extraction machine

Konjac seed oil supercritical co2 extraction process

Supercritical co2 extraction process

Laboratory equipment:HA231-50-06

Extraction pressure: 20 MPa

Extraction temperature: 60°C

Separation kettle Ⅰ pressure: 15 MPa

Separation kettle Ⅰ temperature: 50°C

Separation kettle Ⅱ pressure: 6 MPa

Separation kettle Ⅱ temperature: 45°C

Extraction time: 90 min

Abstract:

To research the optimal extraction process of supercritical CO2 extraction and analyze the component of the oil extracted from Konjac fat soluble components. Methods: using the yield of Konjac seed oil as the index, optimized supercritical CO2 extraction parameter by orthogonal experiment methodology and analysed the compounds of Konjac seed oil by GC-MS.

Results: the suitable extraction separation conditions: 28 MPa extraction pressure, extraction temperature was 60℃; Separate kettle I was15 MPa pressure, separate kettle I temperature was 50℃;Separation reactor II pressure was 6 MPa, separation reactor II temperature was 45℃; Extractiontime was 1.5 h.

Conclusion: Compared with the ethanol impregnation, supercritical CO2 extraction has the advantages of high extraction yield, short extraction time, fatty oil clear advantages, there was a big difference between the two kinds of components.

Foreword:

Konjac is a tuber of Amorphophalluskonjac, a herbaceous plant belonging to the genus Amorphaceae. It has the functions of lowering blood lipids, lowering blood pressure, lowering blood sugar, detoxification, beauty, health care and other functions.

Konjac seed oil supercritical co2 extraction process
Konjac seed oil supercritical co2 extraction process

It is mainly produced in the tropical and subtropical regions of the eastern hemisphere. China is one of the origins and has a wide distribution in various provinces in the south of China. At present, the research on konjac is mainly focused on the study of its plant ecology, cultivation and major components, but the development of konjac fatty oil has been reported less, and the extracts have special odor.

The author's first research on the supercritical CO2 extraction process and composition analysis of konjac fatty oil is of great significance to the further comprehensive development and industrialization of konjac.

1 Experimental materials

Konjac medicinal materials, purchased in Yichang, Hubei;

Commercial Konjac Extract (Chengdu Xifu Biotechnology Co., Ltd.);

Ethyl acetate, dichloromethane (chromatographic grade), anhydrous ether, acetone (analytical grade), anhydrous sodium sulfate (analytical grade) (Tianjin Fuyu Fine Chemical Co., Ltd.);

CO2 (purity: 99.9%, Guangdong Shunde Furen Gas Co., Ltd.). 2 Experimental methods

  3. Orthogonal design for process parameter optimization

There are many factors that affect the efficiency of supercritical CO2 extraction. Based on the single factor pre-test, the author determines the extraction time. For the main factors affecting the extraction efficiency, the extraction pressure, temperature, and the pressure and temperature of the separation kettle I, L16 (4 ) 5 Orthogonal experiment design, taking the yield of konjac fatty oil as an index, and conducting experiments to optimize the extraction process conditions. The factor level setting is shown in the table

 

A

B

C

D

 

Extraction pressure

MPa

Extraction temperature

Separation kettle Ⅰ pressure

MPa

Separation kettle Ⅰ temperature

1

18

45

9

45

2

23

50

12

50

3

28

55

15

55

4

33

60

18

60

4. Extraction process of konjac fatty oil

Weigh a certain amount of pre-granulated medicinal materials each time and put them into the extraction kettle, heat the extraction kettle, separation kettle I, separation kettle II, and refrigerate the cold machine and storage tank. When the temperature reaches the requirements of the experiment, open the carbon dioxide gas cylinder, pressurize the extraction kettle and the separation kettle with a high-pressure pump. When the pressure reaches the value required by the experiment, close the carbon dioxide, open the circulation valve, and perform the extraction cycle. , Discharge from separate kettle Ⅰ and Ⅱ respectively. After the extraction, the II extracts were combined and separated, weighed, and the yield was calculated according to the following formula.

5. Preparation method of test article

Take about 10mg of supercritical CO2 extraction, ethanol impregnation extraction and commercially available fatty oil, accurately weighed, make up to 10ml with anhydrous ether, add a small amount of anhydrous sodium sulfate to remove water, and pass through a 0.45μm microporous filter membrane, that is, Got.

6. result

 From the visual analysis table, it can be seen that the influence order of the four factors on the yield of konjac fatty oil is C> A> D> B, and the factor C has a significant effect on the yield. The best combination of factors and levels is A3B4C3D2, that is, the optimal process conditions for supercritical CO2 extraction of konjac ceramide are: pressure of the extraction kettle 28MPa, temperature of the extraction kettle 60 ℃, pressure of the separation kettle Ⅰ 15MPa, temperature 50 ℃ Kettle II pressure was 6 MPa, temperature was 45 ° C, and extraction time was 90 min.

In order to verify the above results, the optimal extraction process conditions were used for verification tests. Results The average yield of konjac fatty oil was 1.086%, which was consistent with the orthogonal results, which indicated that the process conditions after orthogonal tests were feasible.

 

 

 

 

Gap Analysis Table

 

 

 

 

factor

Sum of squared deviations

Degrees of freedom

FCritical value

Saliency

 

 

Extraction pressure

0.013

3

1.857

9.280

 

 

 

Extraction temperature

0.006

3

0.857

9.280

 

 

 

Separation kettle Ⅰ pressure

0.455

3

65.000

9.280

*

 

 

Separation kettle Ⅰ temperature

0.011

3

1

9.280

 

 

 

误差

0.01

3

 

 

 

 

summary

The optimal process conditions for supercritical CO2 extraction of konjac fatty oil are: extraction kettle pressure 28MPa, extraction kettle temperature 60 ℃, separation kettle I pressure 15MPa, temperature 50 ℃, separation kettle II pressure 6MPa, temperature 45 ℃, extraction time 90min . Under this condition, the oil recovery rate is 1.086%, the sample is clear, and the ceramide content is higher than that of ethanol impregnation. This process can be used to extract konjac ceramide.

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