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Supercritical CO2 fluid extraction of angelica oil

Angelica

Angelica is the dry root of the Umbelliferae Angelica sinensis.

Pharmacology

Modern pharmacological studies have shown that the volatile oil components of angelica have the effects of inhibiting platelet arachidonic acid metabolism, alleviating myocardial ischemia, inhibiting uterine smooth muscle contraction, etc., and has a wide range of pharmacological effects in anti-asthmatic, central depression, analgesia, and immune function enhancement. active.

Extract Angelica Oil

The supercritical CO2 extraction of angelica oil has higher extraction rate and lower extraction temperature than traditional steam distillation extraction of angelica oil, and can store a large amount of thermally unstable and easily oxidized components, which overcomes the high temperature, time-consuming, and time-consuming requirements of steam distillation. The shortcomings of easy variation in composition.

Extraction test

The orthogonal test method was used to study the production process of supercritical CO2 extraction to obtain angelica oil. In addition, volatile oil has strong volatility, is unstable when exposed to light and heat, and is easily lost and deteriorated.

In order to effectively prevent the above problems in the preparation process and improve the efficacy and stability of the drug, this experiment used Lin cyclodextrin (8-CD) to clathrate the supercritical extract of Angelica sinensis and prepare the clathrate by grinding method. The inclusion rate is an index to evaluate the pros and cons of the process, so as to select the best inclusion process.

Extraction process

Supercritical CO2 extraction of angelica oil, take the crude powder of angelica medicinal material (320g each time) in a 1L extraction kettle.

Adjust the extraction temperature, extraction pressure, analysis temperature, and analysis pressure. After the pressure and temperature reach the set conditions, the cyclic extraction is started.

During the extraction process, the carbon dioxide flow rate was 22L/h, and the extraction time was 2h.

Collect the extract, weigh it, and calculate the extraction rate.

Grinding preparation

Preparation of Angelica Oil β-CD Inclusion Compound by Grinding Method According to the pre-test results, weigh an appropriate amount of β-CD into a mortar, add a certain amount of water, and grind evenly.

Dissolve 1g of Angelica oil in 5mL of absolute ethanol, slowly add it to a mortar, continue to grind for a certain period of time, filter with suction, dry at low temperature, and then rinse with petroleum ether 3 times (25mL each time).

After evaporating the petroleum ether, vacuum drying at 40°C for 4 hours to constant weight to obtain (β-CD inclusion compound, weighed and set aside.

Take the dried β-CD inclusion compound, accurately weigh it, determine the angelica oil content, and calculate the inclusion rate.

Scale-up test

The optimal extraction conditions determined by the orthogonal test results of supercritical CO2 extraction of angelica oil were: the extraction temperature was 40°C, the extraction pressure was 15MPa, the analysis temperature was 50°C, and the separation pressure was 6MPa.

Carry out the scale-up test according to the best extraction conditions, take 1.6kg of crude angelica powder in a 5L extraction kettle, and repeat the test. The extraction rate of angelica oil is 1.88%, 1.78%, 1.86%, and the average extraction rate is 1.84%. It shows that the process conditions are basically stable and feasible.

Process parameters

Pulverization degree:40 mesh
Extraction pressure: 24 MPa
Extraction temperature: 60°C
Separation pressure I: 12 MPa
Separation I temperature: 40°C
Separation pressure II: 8 MPa
Separation II temperature: 40°C
Extraction time: 90 min