CN105713732A - Extraction method of star anise oil - Google Patents

Abstract

The invention provides a method for extracting star anise oil. The present invention adopts the process of steam distillation first and then ethanol extraction. In this method, the fennel oil remaining in star anise after steam distillation is extracted by ethanol extraction, so as to realize the dual extraction of effective components of star anise. At the same time, steam distillation can effectively remove impurities in star anise, so that the purity of fennel oil obtained by ethanol extraction in the later stage can be improved, and the inherent defects of organic solvent extraction can be overcome. The method can significantly increase the yield of star anise oil, and obtain better-quality anise oil, and is low in cost and convenient in implementation, and is suitable for industrial scale production.

Description

A kind of extraction method of star anise oil

technical field

The invention belongs to the technical field of natural product extraction, in particular to a method for extracting star anise oil.

Background technique

"Compendium of Materia Medica" records that star anise is the dried and mature fruit of magnolia plant star anise. It has the effects of dispelling wind and regulating qi, harmonizing stomach, warming yang and dispersing cold, regulating qi and relieving pain. In traditional Chinese medicine, it is often used for stomach cold vomiting, kidney deficiency, low back pain and cold colic Abdominal pain etc. Fennel oil can be extracted from its dried fruit and branches and leaves. The most important active ingredient in star anise oil is trans-anethole, also known as anisole, with molecular formula C ₁₀ H ₁₂ O, which is a colorless transparent or light yellow liquid. It has an anise-like aroma and sweet taste, and has been widely used in food production and processing fields such as candy, beverages, and alcoholic flavors. Scientific research has shown that it also has spectrum antibacterial activity and can effectively scavenge DPPH-free radicals. Peristalsis, relief of cough caused by bronchitis and other medicinal value.

At present, there are many extraction methods for star anise oil. Traditional extraction methods include steam distillation, simultaneous distillation extraction, organic solvent extraction, etc. New methods developed in recent years include microwave extraction and supercritical _CO2 extraction. Wait. But on the whole, steam distillation is still the most widely used extraction method because of its good stability, low extraction cost and simple extraction method, but the yield of this method is relatively low; The new technology of volatile oil extraction developed in the 1960s has the outstanding feature of combining the steam distillation of the sample and the solvent extraction of the fraction into one, with fewer extraction steps, but this method requires special equipment with special design and complex structure ; And though the organic solvent extraction method can improve the productive rate of star anise oil to a certain extent, the gained extract has many impurities, and is not easy to separate and purify. In recent years, the emerging microwave extraction method and supercritical CO ₂ extraction method have high requirements on equipment. Although the yield and purity of star anise oil have been improved to a certain extent, the equipment is expensive and not suitable for large-scale industrial production. Therefore how to find a kind of extraction process with low cost, easy implementation, and higher fennel oil yield and purity has become a difficult problem in front of the majority of scientific research workers. At the same time, this process comprehensively compares various extraction methods, and improves and combines the process flow to a certain extent, adopts the process of first steam distillation and then ethanol extraction, and explores the best process conditions, although The price of 95% ethanol is relatively high, but the ethanol can be recovered and recycled here without increasing the production components. Therefore, it is a kind of convenient implementation, which can significantly improve the extraction efficiency, and can make full use of various components in the star anise. Process of active ingredients.

Contents of the invention

Aiming at the above-mentioned deficiencies in the prior art, the present invention provides a method for extracting fennel oil by combining steam distillation and organic solvent extraction. The method can significantly increase the yield of star anise oil and obtain better-quality fennel oil. At the same time, the extraction method is low in cost and easy to implement, and is suitable for industrial scale production.

In order to achieve the above object, the present invention adopts the following technical solutions:

A method for extracting star anise oil, comprising the following steps:

(1) Baking and drying the star anise until the water content is 2%-7%, and then pulverizing it into a powder of 60-70 mesh;

(2) Add water and mix the star anise powder obtained in step (1), and the mass ratio of the added water to the star anise powder is 8-12:1;

(3) Distill the star anise powder-water mixture obtained in step (2) by steam distillation, the distillation temperature is 80-120° C., and the distillation time is 2-5 hours to remove the impurities of the distillation and collect the distillate;

(4) Add analytically pure sodium chloride to the distillate obtained in step (3) until white sodium chloride solid appears in the distillate, and after promoting the oil-water layer, collect the upper oil layer to obtain fennel essential oil;

(5) Collect the star anise powder extracted by steam distillation in step (3), after drying again, carry out Soxhlet extraction with ethanol as a solvent, the extraction temperature is 60°C-90°C, and the extraction time is 4- 6 hours to get the extract;

(6) Recover the ethanol in the extract of step (5) to obtain the fennel extract oil.

Preferably, in step (1), the star anise is baked and dried to a water content of 3%-5%.

Preferably, the mass ratio of water and star anise powder added in step (2) is 9-11:1.

Preferably, the distillation temperature in step (3) is 90-110° C., and the distillation time is 3-4 hours.

Preferably, the extraction temperature in step (5) is 70-80° C., and the extraction time is 3-5 hours.

Preferably, the ethanol concentration in step (5) is 75%-95%.

Preferably, the extraction method of above-mentioned star anise oil, comprises the following steps:

(1) Baking and drying the star anise until the water content is 4%, and then pulverizing it into a 60-mesh powder;

(2) Add water and mix the star anise powder obtained in step (1), and the mass ratio of the added water to the star anise powder is 10:1;

(3) Distill the star anise powder-water mixture obtained in step (2) by steam distillation, the distillation temperature is 105° C., and the distillation time is 4 hours to remove the impurities of the distillation and collect the distillate;

(4) Add analytically pure sodium chloride to the distillate obtained in step (3) until white sodium chloride solid appears in the distillate, and after promoting the oil-water layer, collect the upper oil layer to obtain fennel essential oil;

(5) the star anise powder extracted through steam distillation in step (3) is collected, after drying again, carry out Soxhlet extraction with 95% ethanol as solvent, extraction temperature is 78 ℃, and extraction time is 4.5 hours, get the extract;

(6) Recover the ethanol in the extract of step (5) to obtain the fennel extract oil.

Compared with the prior art, the present invention has significant advantages in that:

(1) The present invention adopts the technology of first steam distillation and then ethanol extraction to operate, the technology is simple, convenient to implement, and does not need expensive equipment.

(2) Compared with the traditional extraction method, the yield of the present invention is significantly improved. After the steam distillation, the fennel oil remaining in the star anise is extracted through the ethanol extraction method, so as to realize the secondary extraction and utilization of the effective components of the star anise; at the same time, the steam distillation Impurities in star anise can be effectively removed, so that the purity of fennel oil obtained through ethanol extraction in the later stage can be significantly improved.

(3) The present invention does not add any toxic and harmful solvents to prevent harmful chemical residues to the human body and environmental pollution during processing. At the same time, the ethanol used in the ethanol extraction method can be recovered and recycled, saving resources and effectively reducing The production cost is suitable for industrial mass production applications.

Description of drawings

Fig. 1 is the gas chromatogram of the star anise essential oil that embodiment 1 steam distillation obtains;

Fig. 2 is the gas chromatogram of the star anise extract oil that embodiment 1 Soxhlet extraction obtains;

Fig. 3 is the gas chromatogram of the star anise essential oil that comparative example 1 steam distillation obtains;

Fig. 4 is the gas chromatogram of the star anise extract oil that comparative example 2 Soxhlet extraction obtains;

Fig. 5 is the gas chromatogram of the star anise extract oil that comparative example 3 Soxhlet extraction obtains;

Fig. 6 is the gas chromatogram of the star anise essential oil that comparative example 3 steam distillation obtains;

Fig. 7 is the gas chromatogram of the star anise oil obtained by the simultaneous distillation and extraction method in Comparative Example 4.

detailed description

The present invention will be further described in conjunction with the examples. It should be noted that the following descriptions are only for explaining the present invention and not limiting its content.

Example 1

Take the star anise fruit, bake and dry until the water content is 2%, pass through a 60-mesh sieve after being crushed by a pulverizer, weigh 100g of star anise powder with an electronic scale, add 1200mL of water, mix the two, and place it in the steam receiver of the steam distillation device. Start distillation in the bottle, the distillation temperature is 80°C, the distillation time is 5h, remove the impurities in the distillation, collect the effluent, add analytically pure sodium chloride until white sodium chloride solid appears in the water phase, separate the oil and water, absorb In the upper oil layer, 5.74g of star anise essential oil was obtained, which was stored in a brown bottle for later use, and the yield was 5.74%. The water phase in the steam receiving bottle in the steam distillation device was discarded, and the residue in the lower layer was collected and directly poured into a tray for drying. Collect and dry the residue to obtain 71g, place it in the extraction tube of a Soxhlet extractor, add 70% ethanol to extract until it is submerged in the siphon tube, extract at 60°C for 6 hours, collect the effluent, and recover the ethanol to obtain star anise extract Extract 13g of oil and store it in a brown bottle for future use. The yield is 18.31%. Gas chromatography is used to detect the material components of star anise essential oil and star anise extract oil. The test results are shown in Figure 1 and Figure 2. The essential oil contains 82.7% of anisehole, and the extract oil contains 31.2% of anisehole.

Example 2

Take the star anise fruit, bake and dry until the water content is 5%, pass through a 60-mesh sieve after being crushed by a pulverizer, weigh 200g of star anise powder with an electronic scale, add 2200mL of water, mix the two, and place it in the steam receiver of the steam distillation device. Start distillation in the bottle, the distillation temperature is 90°C, the distillation time is 3h, remove the impurities in the distillation, collect the effluent, add analytically pure sodium chloride until white sodium chloride solid appears in the water phase, separate the oil and water, absorb In the upper oil layer, 11.62g of star anise essential oil was obtained, which was stored in a brown bottle for later use, and the yield was 5.81%. The water phase in the steam receiving bottle in the steam distillation device was discarded, and the residue in the lower layer was collected and directly poured into a tray for drying. Collect and dry the residue to obtain 141g, place it in the extraction tube of a Soxhlet extractor, add 80% ethanol to extract until it does not pass through the siphon tube, extract at 70°C for 5 hours, collect the effluent, and recover the ethanol to obtain star anise extract Extract 26.4g of oil and store it in a brown bottle for future use. The yield is 18.72%. The composition of star anise essential oil and star anise extract oil is detected by gas chromatography. It can be known that the essential oil contains 81.3% anethole, and the extract oil contains 30.7% anethole.

Example 3

Take the star anise fruit, bake and dry until the water content is 4%, pass through a 60-mesh sieve after being crushed by a pulverizer, weigh 150g of star anise powder with an electronic scale, add 1500mL of water, mix the two, and place it in the steam receiver of the steam distillation device. Start distillation in the bottle, the distillation temperature is 105°C, and the distillation time is 4h. Remove the impurities in the distillation, collect the effluent, add analytically pure sodium chloride until white sodium chloride solid appears in the water phase, separate the oil and water, and absorb In the upper oil layer, 8.83g of star anise essential oil was obtained, which was stored in a brown bottle for later use, and the yield was 5.89%. The water phase in the steam receiving bottle in the steam distillation device was discarded, and the residue in the lower layer was collected and directly poured into a tray for drying. Collect and dry the residue to obtain 108g, place it in the extraction tube of a Soxhlet extractor, add 95% ethanol to extract until it is submerged in the siphon tube, extract at 78°C for 4.5 hours, collect the liquid, and recover the ethanol to obtain star anise 20.48g of the extracted oil was stored in a brown bottle for future use, and the yield was 18.96%. The composition of star anise essential oil and star anise extract oil is detected by gas chromatography. It can be known that the essential oil contains 82.9% of anisehole, and the extract oil contains 30.6% of anisehole.

Example 4

Take the star anise fruit, bake and dry until the water content is 3%, pass through a 70-mesh sieve after being crushed by a pulverizer, weigh 100g of star anise powder with an electronic scale, add 900mL of water, mix the two, and place it in the steam receiver of the steam distillation device. Start distillation in the bottle, the distillation temperature is 120°C, and the distillation time is 2h. Remove the impurities in the distillation, collect the effluent, add analytically pure sodium chloride until white sodium chloride solid appears in the water phase, separate the oil and water, and absorb In the upper oil layer, 5.92g of star anise essential oil was obtained, which was stored in a brown bottle for later use, and the yield was 5.92%. The water phase in the steam receiving bottle in the steam distillation device was discarded, and the residue in the lower layer was collected and directly poured into a tray for drying. Collect and dry the residue to obtain 72g, place it in the extraction tube of a Soxhlet extractor, add 75% ethanol to extract until it does not pass through the siphon tube, extract at 80°C for 5 hours, collect the effluent, and recover the ethanol to obtain star anise extract Extract 13.62g of oil and store it in a brown bottle for future use, the yield is 18.92%. The composition of star anise essential oil and star anise extract oil is detected by gas chromatography. It can be seen that the essential oil contains 82.9% of anisehole, and the extract oil contains 30.9% of anisehole.

Example 5

Take the star anise fruit, bake and dry until the water content is 7%, pass through a 70-mesh sieve after being crushed by a pulverizer, weigh 200g of star anise powder with an electronic scale, add 1600mL of water, mix the two, and place it in the steam receiver of the steam distillation device. Start distillation in the bottle, the distillation temperature is 100°C, and the distillation time is 3.5h. Remove the impurities in the distillation, collect the effluent, add analytically pure sodium chloride until white sodium chloride solid appears in the water phase, and separate the oil and water. Absorb the upper oil layer to obtain 11.52g of star anise essential oil, put it in a brown bottle and save it for later use, the yield is 5.76%, discard the water phase in the steam receiving bottle in the steam distillation device, collect the residue in the lower layer and pour it directly into the tray for drying , collect and dry the residue to obtain 143g, put it in the extraction tube of Soxhlet extractor, add 70% ethanol to extract until it has not passed the siphon tube, extract at 90°C for 4 hours, collect the liquid, and recover the ethanol to obtain star anise 26.75g of the extracted oil was stored in a brown bottle for future use, and the yield was 18.75%. The composition of star anise essential oil and star anise extract oil is detected by gas chromatography. It can be seen that the essential oil contains 82.4% of anisehole, and the extract oil contains 31.3% of anisehole.

Comparative example 1

Take the star anise fruit, bake and dry until the water content is 2%, pass through a 60-mesh sieve after being crushed by a pulverizer, weigh 100g of star anise powder with an electronic scale, add 1200mL of water, mix the two, and place it in the steam receiver of the steam distillation device. Start distillation in the bottle, the distillation temperature is 80°C, the distillation time is 5h, remove the impurities in the distillation, collect the effluent, add analytically pure sodium chloride until white sodium chloride solid appears in the water phase, separate the oil and water, absorb In the upper oil layer, 5.72g of star anise essential oil was obtained, which was stored in a brown bottle for later use, and the yield was 5.72%. %.

But compared with Example 1, Comparative Example 1 only uses the steam distillation method, then the fennel oil remaining in the star anise cannot be extracted, and the total yield is not high.

Comparative example 2

Take the star anise fruit, bake and dry until the water content is 2%, pass through a 60-mesh sieve after being pulverized by a pulverizer, weigh 100g of star anise powder with an electronic scale, place it in the extraction tube of a Soxhlet extractor, add 70% ethanol to extract to Submerged in a siphon, extracted at 60°C for 6 hours, collected the effluent, and recovered ethanol to obtain 21.5 g of star anise extract oil, which was stored in a brown bottle for later use, with a yield of 21.5%. The components of the star anise extract oil were detected by gas chromatography, and the test results are shown in Figure 4, the extract oil contained 36.7% anethole.

Compared with Example 1, Comparative Example 2 only uses ethanol as a solvent for Soxhlet extraction, and its yield and the anethole component contained in the extracted oil have a small increase, but the total yield is still not as good as that of Example 1, and using Gas chromatography detection and analysis shows that the components in the extracted oil are very complex, and there are a large number of unidentified substances, which means that there are many types of impurities and high content, which is very unfavorable for further separation and purification of active components of fennel oil.

Comparative example 3

Take the star anise fruit, bake and dry until the water content is 2%, pass through a 60-mesh sieve after being pulverized by a pulverizer, weigh 100g of star anise powder with an electronic scale, place it in the extraction tube of a Soxhlet extractor, add 70% ethanol to extract to Submerged in a siphon, extracted at 60°C for 6 hours, collected the effluent, and recovered ethanol to obtain 22.3 g of star anise extract oil, which was stored in a brown bottle for later use, with a yield of 22.3%. The components of the star anise extract oil were detected by gas chromatography, and the test results are shown in Figure 5. The extract oil contained 36.2% anethole. Collect the star anise residue and pour it directly into the tray for drying. After collecting and drying the residue to obtain 59g, add 708mL of water, mix the two, place it in the steam receiving bottle in the steam distillation device and start distillation. The distillation temperature is 80°C. The time is 5 hours, remove the impurities in the distillation, collect the slip-out liquid, add analytically pure sodium chloride until white sodium chloride solid appears in the water phase, separate the oil and water, absorb the upper oil layer, and obtain 1.03 g of star anise essential oil, which is placed in Store it in a brown bottle for later use, and the yield is 1.74%. The star anise essential oil is detected by gas chromatography for its composition. The test results are shown in Figure 6. The essential oil contains 72.8% of anethole.

Compared with Example 1, first use ethanol as solvent to carry out Soxhlet extraction, and then carry out steam distillation, then the yield and purity of fennel oil in the later stage steam distillation method are all significantly reduced, and it is the same as Comparative Example 2. Steam distillation and direct Soxhlet extraction will result in many types of impurities in the extracted volatile oil and high content, which is very unfavorable for the further separation and purification of the effective components of fennel oil.

Comparative example 4

Take the star anise fruit, bake and dry until the water content is 2%, pass through a 60-mesh sieve after being pulverized by a pulverizer, weigh 100g of star anise powder with an electronic scale, add 1200mL of water, and place it on one end of the simultaneous distillation extraction apparatus, and place it in the other end of the simultaneous distillation extraction apparatus Add 70% ethanol, then distill and extract at the same time for 10 hours, and recover the ethanol solvent to obtain 6.72 g of star anise oil. The star anise oil is detected by gas chromatography. The test results are shown in Figure 7. It can be seen that anise oil contains anethole 82.5%

Compared with Implementation 1, the total yield of fennel oil by simultaneous distillation and extraction is not high, and the purity does not increase significantly. In fact, the essence of the simultaneous distillation extraction method is that the sample has only been subjected to steam distillation, and the volatile fractions are dissolved in the extractant. Specifically, in this comparative example, star anise has been subjected to steam distillation, and volatile components such as fennel oil It is distilled and then volatilized to the condensation tube and then dissolved in ethanol to complete the extraction process. The raw material star anise itself does not directly contact ethanol, which is essentially different from the present application.

Although the specific implementation of the present invention has been described above in conjunction with the examples, it is not intended to limit the protection scope of the present invention. Those skilled in the art should understand that on the basis of the technical solution of the present invention, those skilled in the art do not need to pay creative work Various modifications or variations that can be made are still within the protection scope of the present invention.

Claims (7)

1. the extracting method of an Oleum Anisi Stellati, it is characterised in that comprise the following steps:

(1) anise baking is dried to water content at 2%-7%, then smashes into the powder of 60-70 order；

(2) add water mixing by step (1) gained anise powder, is added water and the mass ratio of anistree powder is 8-12:1；

(3) adopting steam distillation that step (2) gained anise powder water mixed liquid is distilled, vapo(u)rizing temperature is 80-120 DEG C, and distillation time is 2-5 hour, removes the impurity of distillation, collects distillation；

(4) in gained distillation in step (3), add analytical pure sodium chloride to distillation and white solid sodium chloride occurs, collect upper strata oil reservoir after promoting profit layering and obtain fennel essential oil；

(5) being collected by the anistree powder extracted through vapor distillation in step (3), after after drying, carry out soxhlet type using ethanol as solvent, extraction temperature is 60 DEG C-90 DEG C, and extraction times is 4-6 hour, obtains extract；

(6) ethanol in recycling step (5) extract obtains Fructus Foeniculi extract oil.

2. the extracting method of a kind of Oleum Anisi Stellati as claimed in claim 1, it is characterised in that in step (1), anise is bakeed and be dried to water content 3%-5%.

3. the extracting method of a kind of Oleum Anisi Stellati as claimed in claim 1, it is characterised in that added water in step (2) and the mass ratio of anistree powder is 9-11:1.

4. the extracting method of a kind of Oleum Anisi Stellati as claimed in claim 1, it is characterised in that in step (3), vapo(u)rizing temperature is 90-110 DEG C, distillation time is 3-4 hour.

5. the extracting method of a kind of Oleum Anisi Stellati as claimed in claim 1, it is characterised in that in step (5), extraction temperature is 70-80 DEG C, extraction times is 3-5 hour.

6. the extracting method of a kind of Oleum Anisi Stellati as claimed in claim 1, it is characterised in that concentration of alcohol described in step (5) is 75%-95%.

7. the extracting method of a kind of Oleum Anisi Stellati as claimed in claim 1, it is characterised in that the extracting method of above-mentioned Oleum Anisi Stellati, comprises the following steps:

(1) anise baking is dried to water content 4%, then smashes into the powder of 60 orders；

(2) add water mixing by step (1) gained anise powder, is added water and the mass ratio of anistree powder is 10:1；

(3) adopting steam distillation that step (2) gained anise powder water mixed liquid is distilled, vapo(u)rizing temperature is 105 DEG C, and distillation time is 4 hours, removes the impurity of distillation, collects distillation；

(4) in gained distillation in step (3), add analytical pure sodium chloride to distillation and white solid sodium chloride occurs, collect upper strata oil reservoir after promoting profit layering and obtain fennel essential oil；

(5) being collected by the anistree powder extracted through vapor distillation in step (3), after after drying, carry out soxhlet type using 95% ethanol as solvent, extraction temperature is 78 DEG C, and extraction times is 4.5 hours, obtains extract；

(6) ethanol in recycling step (5) extract obtains Fructus Foeniculi extract oil.