CN112063458A - Method for extracting cinnamon essential oil by using eutectic solvent - Google Patents
Method for extracting cinnamon essential oil by using eutectic solvent Download PDFInfo
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- CN112063458A CN112063458A CN202011115053.XA CN202011115053A CN112063458A CN 112063458 A CN112063458 A CN 112063458A CN 202011115053 A CN202011115053 A CN 202011115053A CN 112063458 A CN112063458 A CN 112063458A
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- cinnamon
- essential oil
- eutectic solvent
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- 241000723347 Cinnamomum Species 0.000 title claims abstract description 52
- 235000017803 cinnamon Nutrition 0.000 title claims abstract description 49
- 239000000341 volatile oil Substances 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002904 solvent Substances 0.000 title claims abstract description 23
- 230000005496 eutectics Effects 0.000 title claims abstract description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims abstract description 10
- 238000004821 distillation Methods 0.000 claims abstract description 8
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 239000001763 2-hydroxyethyl(trimethyl)azanium Substances 0.000 claims description 9
- 235000019743 Choline chloride Nutrition 0.000 claims description 9
- SGMZJAMFUVOLNK-UHFFFAOYSA-M choline chloride Chemical compound [Cl-].C[N+](C)(C)CCO SGMZJAMFUVOLNK-UHFFFAOYSA-M 0.000 claims description 9
- 229960003178 choline chloride Drugs 0.000 claims description 9
- 229960004063 propylene glycol Drugs 0.000 claims description 6
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 239000000370 acceptor Substances 0.000 claims 3
- 150000001298 alcohols Chemical class 0.000 claims 1
- 238000003760 magnetic stirring Methods 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims 1
- 238000000605 extraction Methods 0.000 abstract description 20
- 235000013305 food Nutrition 0.000 abstract description 7
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 238000001256 steam distillation Methods 0.000 abstract description 5
- 230000003078 antioxidant effect Effects 0.000 abstract description 4
- 239000002608 ionic liquid Substances 0.000 abstract description 4
- 230000003647 oxidation Effects 0.000 abstract description 4
- 238000007873 sieving Methods 0.000 abstract description 4
- 239000003963 antioxidant agent Substances 0.000 abstract description 3
- 239000008367 deionised water Substances 0.000 abstract description 3
- 229910021641 deionized water Inorganic materials 0.000 abstract description 3
- 239000003814 drug Substances 0.000 abstract description 3
- 239000002537 cosmetic Substances 0.000 abstract description 2
- 238000000199 molecular distillation Methods 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 238000000194 supercritical-fluid extraction Methods 0.000 abstract description 2
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 238000007789 sealing Methods 0.000 description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 5
- 235000010323 ascorbic acid Nutrition 0.000 description 4
- 229960005070 ascorbic acid Drugs 0.000 description 4
- 239000011668 ascorbic acid Substances 0.000 description 4
- 150000003254 radicals Chemical class 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- HHEAADYXPMHMCT-UHFFFAOYSA-N dpph Chemical compound [O-][N+](=O)C1=CC([N+](=O)[O-])=CC([N+]([O-])=O)=C1[N]N(C=1C=CC=CC=1)C1=CC=CC=C1 HHEAADYXPMHMCT-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 235000013599 spices Nutrition 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 230000002292 Radical scavenging effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000013641 positive control Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 241000218195 Lauraceae Species 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 235000008429 bread Nutrition 0.000 description 1
- 230000030833 cell death Effects 0.000 description 1
- 230000003915 cell function Effects 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 235000020774 essential nutrients Nutrition 0.000 description 1
- 239000000374 eutectic mixture Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention discloses a method for extracting cinnamon essential oil by using a eutectic solvent. And crushing the cinnamon blocks by a crusher to obtain crude cinnamon powder. And (4) sieving the coarse cinnamon powder by a sieve of 80 meshes to obtain cinnamon fine powder. Reacting the cinnamon fine powder and the eutectic solvent at a mass ratio of 1: 4-1: 8 at a temperature of 50-90 ℃ for 5-25 min. And then adding 200ml of deionized water, performing steam distillation, wherein volatile components in the cinnamon essential oil can form an azeotrope with water and are evaporated along with steam, and collecting the volatile oil obtained by distillation. The invention adopts the eutectic solvent, has low cost, is green, safe and pollution-free. The problem of high price of the imidazole ionic liquid is avoided, and the problem of solvent residue in the extraction of the organic solvent is avoided. The invention has simple process and convenient operation, and avoids the limitation of equipment in the methods of supercritical fluid extraction, molecular distillation and the like. The cinnamon essential oil extracted by the method can shorten the extraction period, obtain higher extraction rate, has good oxidation resistance, is a potential natural antioxidant, and has development potential in the fields of food, medicine and cosmetics.
Description
Technical Field
The invention relates to an extraction method of deep eutectic solvent cinnamon essential oil, and belongs to the technical field of essential oil processing.
Background
Cinnamon, also known as cinnamon and cinnamon, is an important spice, is commonly used as an additive, is a traditional Chinese medicine material, is certified by the FDA as a generally recognized safe food (GRAS), and is commonly used all over the world. Cinnamon plants belong to the family lauraceae, evergreen trees, and are suitably living in warm and humid conditions, mainly in subtropical regions such as india, cambodia, china, and the like. The planting of cinnamon in China is mainly concentrated in Guangxi, Guangdong, Yunnan, Fujian and other places, and the yield of cinnamon in China can account for 80 percent of the world cinnamon yield, and belongs to the world of cinnamon production. Cinnamon is commonly used in the food industry to improve or accentuate the taste of food. The cinnamon essential oil can be used as a preparation spice of products such as beverages, candies and the like, and can also be used as a natural preservative of bread and cake products. Cinnamon essential oil has antioxidant properties and can reduce oxidation reactions in biological systems. Excessive production of free radicals can cause redox imbalance, interfere with cell functions, and can lead to cell death seriously. Spice plants such as cinnamon have long been recognized as natural antioxidants and the use of essential oils in food products has become a means of increasing the shelf life of the food product and reducing waste and nutrient loss (inhibition and retardation of oxidation). The eutectic solvent is a eutectic mixture formed by two or three components in proportion through the interaction of hydrogen bonds. The ionic liquid has the similar properties to the traditional ionic liquid, and has the advantages of low raw material price, simple preparation, safety, no toxicity or low toxicity. Choline chloride has been used for decades in the agrochemical (essential nutrient) and pharmaceutical industries and is a good choice for the eutectic solvent component.
The conventional extraction method of steam distillation has the problems of low extraction efficiency and long extraction time, and practical development and utilization of the extraction method are limited. The new extraction method is developed, the extraction efficiency of the cinnamon essential oil is improved, the comprehensive development of cinnamon resources is facilitated, and the production benefit is improved.
Disclosure of Invention
The invention aims to provide a method for extracting essential oil from cinnamon by using a eutectic solvent, and the method adopts the eutectic solvent, is low in cost, green, safe and pollution-free. The problem of high price of the imidazole ionic liquid is avoided, and the problem of toxicity of extraction of an organic solvent is avoided. The invention has simple process and convenient operation, and avoids the limitation of equipment in the methods of supercritical fluid extraction, molecular distillation and the like. The cinnamon essential oil extracted by the method can shorten the extraction period, obtain higher extraction rate, has good oxidation resistance, is a potential natural antioxidant, and has development potential in the fields of food, medicine and cosmetics.
The technical scheme of the invention is as follows:
1) crushing the dried cinnamon rolls into small pieces, crushing by using a crusher, sieving by using a 80-mesh sieve, transferring to a container, sealing by using a sealing film, and storing in a dryer.
2) Choline chloride, 1, 2-propylene glycol and water are put into a round-bottom flask according to a certain proportion, and are continuously heated and stirred to prepare uniform and stable liquid.
3) Mixing the above cortex Cinnamomi powder with eutectic solvent containing choline chloride/1, 2-propylene glycol at ratio of 1: 4-8, at 50-80 deg.C for 5-25min, and extracting in situ flask under heating and stirring.
4) After extraction, 200ml of deionized water is added for steam distillation extraction, and the volatile oil obtained by distillation is collected.
5) The eutectic solvent can be choline chloride/1, 2-propylene glycol, choline chloride/glucose, lactic acid/glucose, etc.
Compared with the prior art, the invention has the following advantages:
the used eutectic solvent is simple and easy to synthesize and has low raw material price; the extraction process is simple, the operation is convenient, the extraction period is shortened, the extraction efficiency is improved, and the problems of time consumption and low extraction rate of the traditional process are solved.
Drawings
FIG. 1 is a graph showing the comparison of the radical scavenging rate of cinnamon essential oil extracted by eutectic solvent and cinnamon essential oil extracted by conventional water distillation
Detailed Description
The technical scheme of the invention is explained in detail through specific embodiments. The technical content described in the embodiment is illustrative and not restrictive, and the scope of the invention should not be limited thereto.
Example 1
1) Crushing the dried cinnamon rolls into small pieces, crushing the cinnamon rolls by a crusher, sieving the crushed cinnamon rolls by a 80-mesh sieve, transferring the cinnamon rolls into a container, sealing the container by a sealing film, and storing the cinnamon rolls in a dryer for later use.
2) Choline chloride, 1, 2-propylene glycol and water are put into a round-bottom flask according to a certain proportion, and are continuously heated and stirred to prepare uniform and stable liquid.
3) Adding appropriate amount of cortex Cinnamomi powder and eutectic solvent of choline chloride/1, 2-propylene glycol into round bottom flask, and magnetically stirring at 70 deg.C for 10 min.
4) Extracting with eutectic solvent, adding 200ml deionized water, distilling for 50min, and collecting
5) Collecting the volatile oil obtained by distillation.
Comparative example 1
Comparative example 1 is a conventional steam distillation extraction method, as follows:
1) crushing the dried cinnamon rolls into small pieces, crushing the cinnamon rolls by a crusher, sieving the crushed cinnamon rolls by a 80-mesh sieve, transferring the cinnamon rolls into a container, sealing the container by a sealing film, and storing the cinnamon rolls in a dryer for later use.
2) Extracting the cinnamon powder prepared in the step 1) by steam distillation for 2 hours, and collecting the volatile oil obtained by distillation.
Test examples
The yields of essential oils of example 1 and comparative example 1 were calculated, and the radical clearance of example 1 and comparative example 1 was measured using the DPPH method.
The antioxidant properties of cinnamon essential oil were determined using DPPH method. 10mg/ml, 20mg/ml, 30mg/ml, 40mg/ml, 50mg/ml ascorbic acid solution, the ethanol solution of the essential oil of example 1, and the ethanol solution of the essential oil of comparative example 1 were prepared, respectively, using absolute ethanol as a solvent, with ascorbic acid solution as a positive control. Respectively mixing 1ml of sample solution with 2ml of DPPH solution with the concentration of 0.5mmol/l, violently shaking for 30s to make the mixture uniform, standing in the shade at room temperature for 40min, measuring the absorbance value at 517nm, and calculating the free radical clearance.
The results of the yield of essential oil are shown in table 1.
TABLE 1 yield of essential oils
As can be seen from Table 1, the method for extracting essential oil from cinnamon of the present invention has high yield of essential oil.
Explanation of the drawings
FIG. 1 is a graph comparing the radical clearance. Trend graphs of the clearance of cinnamon essential oil extracted in example 1 and comparative example 1 with ascorbic acid as a positive control. Ascorbic acid has a constant radical scavenging effect, and the clearance of essential oils increases with increasing concentration for both methods. And compared with the essential oil obtained in the comparative example 1, the essential oil obtained in the example 1 has higher clearance rate than the essential oil obtained in the comparative example 1, and shows relatively better oxidation resistance.
Claims (6)
1. A method for extracting cinnamon essential oil from cinnamon plants by using a eutectic solvent is characterized in that: extracting cinnamon essential oil from cinnamon plants using a eutectic solvent. The process flow comprises the following steps: adding the processed cinnamon powder into a eutectic solvent according to a certain proportion, reacting for a period of time at a certain temperature, then transferring to a large container, performing water distillation again, and collecting to obtain cinnamon essential oil.
2. The method of claim 1, wherein: the cinnamon roll is firstly dried, crushed and sieved, and the particle size of cinnamon powder is 80 meshes.
3. The method of claim 1, wherein: the eutectic solvent is formed by combining a hydrogen bond donor and a hydrogen bond acceptor, and two or more components are heated according to a certain proportion to form a mixture. Quaternary ammonium salt type hydrogen bond acceptors such as choline chloride, and hydrogen bond acceptors such as alcohols. Choline chloride, 1, 2-propylene glycol and water are put into a round-bottom flask according to a certain proportion, and are continuously heated and stirred to prepare uniform and stable liquid.
4. The method of claim 1, wherein: the mass ratio of eutectic solvent and cortex Cinnamomi powder is 1: 4-8, the temperature is 50-90 deg.C, and the time is 5-25min, and magnetic stirring is used to heat and stir in round bottom flask. Then, an appropriate amount of water was added to conduct water distillation.
5. The method of claim 1, wherein: the water distillation time is 10-90 min.
6. The method of claim 1, wherein the water and essential oil form an azeotrope, and the water carries the essential oil out of the azeotrope and the essential oil is collected by passing the essential oil through a condenser.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011115053.XA CN112063458A (en) | 2020-10-19 | 2020-10-19 | Method for extracting cinnamon essential oil by using eutectic solvent |
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| CN202011115053.XA CN112063458A (en) | 2020-10-19 | 2020-10-19 | Method for extracting cinnamon essential oil by using eutectic solvent |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725091A (en) * | 2021-01-04 | 2021-04-30 | 陕西国际商贸学院 | Method for extracting wormwood essential oil by microwave-assisted eutectic solvent and application of wormwood essential oil |
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2020
- 2020-10-19 CN CN202011115053.XA patent/CN112063458A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112725091A (en) * | 2021-01-04 | 2021-04-30 | 陕西国际商贸学院 | Method for extracting wormwood essential oil by microwave-assisted eutectic solvent and application of wormwood essential oil |
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Application publication date: 20201211 |