CN103805341A - Extraction method of orange peel essential oil - Google Patents
Extraction method of orange peel essential oil Download PDFInfo
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- CN103805341A CN103805341A CN201210460934.4A CN201210460934A CN103805341A CN 103805341 A CN103805341 A CN 103805341A CN 201210460934 A CN201210460934 A CN 201210460934A CN 103805341 A CN103805341 A CN 103805341A
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- essential oil
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- reticulata blanco
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Abstract
The invention relates to an extraction method of orange peel essential oil, and belongs to the field of essential oil preparation. The extraction method of the orange peel essential oil comprises carrying out steam distillation on the raw material followed by microwave processing, and refining the orange peel essential oil by supercritical CO2. By combining the steam distillation method and the supercritical extraction method, the oil yield of orange peel can be effectively improved, and the oil yield improves by about 20% compared with the traditional steam distillation method. Meanwhile, the purity of the orange peel essential oil is enhanced, and food-grade orange peel essential oil can be obtained.
Description
Technical field
The present invention relates to a kind of extracting method of tangerine essential oil, belong to essential oil preparation field.
Background technology
Peel of Citrus reticulata Blanco, refer to the citrous pericarp of a class, comprise sweet orange class, wide skin citrus, lemon class, shaddock class, there is clearing heat and detoxicating, the dry effect of relieving inflammation or internal heat, dispel, its essential oil is the combination that contains the compound with strong aromatic odour, contain a large amount of terpenoid substances, can be used as a kind of spices that uses, for the processing of the numerous food such as beverage.
The process for purification of spices is mainly by steam distillation, supercritical extraction and organic solvent extractionprocess.
Steam distillation is by utilizing high-temperature water vapor to make the spices of the oily method of separating with water vapor of vaporizing, isolated steam is carried out carrying out oily water separation after condensation, obtaining essential oil.The extraneous solvent contamination of the method, can obtain the essential oil product that purity is higher, but its rate of recovery is lower.Provide the yield of essential oil though be widely used at present the extraction liquid after essential oil refluxes by extraction method, but essential oil in these extraction liquids only circulates in system, and be the effective yield of raising essential oil.
Thereby organic solvent extractionprocess is to utilize spices different solubility in different organic solvents to select suitable organic solvent that spices is separated, conventional solvent is ethanol etc., but it is evident that, in the process of Separation of Organic and essential oil, tend to residual a small amount of solvent in essential oil, cause essential oil pollution in various degree.
Supercritical extraction is to utilize temperature, pressure to carry out the extraction of spices as solvent higher than the fluid of stagnation point.Because supercutical fluid had both had mobility and the solvability of fluid, there is again the good diffustivity of gas simultaneously.In the time there is comparatively faint variation in ambient conditions, can cause the noticeable change of supercutical fluid, the extraction that utilizes supercutical fluid to carry out spices can obtain the high and free of contamination spices essential oil of purity, and conventional supercutical fluid is supercritical CO
2.But supercritical extraction price is comparatively expensive.
Summary of the invention
The object of this invention is to provide a kind of extracting method of essential oil, a kind of extracting method of tangerine essential oil is specifically provided, improve the purity of tangerine essential oil, obtain the tangerine essential oil of food grade.
The object of this invention is to provide a kind of extracting method of tangerine essential oil.
An extracting method for tangerine essential oil, comprises following processing step:
1. raw material processing: the peel of Citrus reticulata Blanco of removing white cortex is carried out to crushed after being dried to 200nm, the peel of Citrus reticulata Blanco particle of pulverizing is dissolved in non-polar solvent, gained peel of Citrus reticulata Blanco solution is carried out to microwave treatment until peel of Citrus reticulata Blanco particle dissolves completely;
2. distillation: by step 1. gained peel of Citrus reticulata Blanco solution be placed in steam still and distill processing, must contain the steam of tangerine essential oil;
3. condensation: the step steam that 2. gained contains tangerine essential oil is carried out to condensation process, collect tangerine essential oil;
4. non-polar solvent reclaims: the non-polar solvent in distiller is reclaimed;
5. refining: to utilize supercritical CO
2to step 3. gained tangerine essential oil refine extraction treatment.
In the extracting method of tangerine essential oil of the present invention, originally receive technician and should know during described step is 1. repeatedly pulverizing after the peel of Citrus reticulata Blanco drying treatment of fresh harvesting, sieve, to the median size of peel of Citrus reticulata Blanco particle be below 200nm.Peel of Citrus reticulata Blanco particle through lyophilize processing can further be pulverized grinding, be crushed to nano-scale particle can be farthest dissolved in solvent, thereby more easy aromatoising substance in particle is taken away.
In the extracting method of tangerine essential oil of the present invention, preferred steps 1.: the peel of Citrus reticulata Blanco of removing white cortex carry out crushed after being dried to 50 ~ 150nm.
In the extracting method of tangerine essential oil of the present invention preferred steps 1. in non-polar solvent be vegetables oil.
In the extracting method of tangerine essential oil of the present invention preferred steps 1. in peel of Citrus reticulata Blanco particle be 1g:20 ~ 100ml with the ratio of non-polar solvent.
In the extracting method of tangerine essential oil of the present invention preferred steps 1. microwave treatment conditions be: microwave power 400 ~ 800W, microwave time 5 ~ 15min.
In the extracting method of tangerine essential oil of the present invention, preferred steps 2.: solution is placed in steam still and distills processing, and the pressure of distiller is 5 ~ 10Mpa, distillation time 1h ~ 6h.
In the extracting method of tangerine essential oil of the present invention, preferably distillation number of times is 1 ~ 5 time, and distillation time summation is 1h ~ 6h.
In the extracting method of tangerine essential oil of the present invention, preferred steps 5.: utilize supercritical CO
2to step 3. gained tangerine essential oil refine extraction treatment, supercritical CO
2flow is 10 ~ 50L/h, pressure 10 ~ 20Mpa, 40 ~ 80 ℃ of temperature, time 1 ~ 6h.
The further preferred following technical proposals of the extracting method of tangerine essential oil of the present invention:
1. raw material processing: the peel of Citrus reticulata Blanco of removing white cortex carry out crushed after being dried to 50 ~ 150nm, the peel of Citrus reticulata Blanco particle of pulverizing is dissolved in non-polar solvent, peel of Citrus reticulata Blanco particle is 1g:20 ~ 100ml with the ratio of non-polar solvent, gained peel of Citrus reticulata Blanco solution is carried out to microwave treatment until peel of Citrus reticulata Blanco particle dissolves completely, microwave treatment conditions is: microwave power 400 ~ 800W, microwave time 5 ~ 15min;
2. distillation: by step 1. gained peel of Citrus reticulata Blanco solution be placed in steam still and distill processing, the pressure of distiller is 5 ~ 10Mpa, distilling number of times is 1 ~ 5 time, distillation time summation is 1h ~ 6h, must contain the steam of tangerine essential oil;
3. condensation: the step steam that 2. gained contains tangerine essential oil is carried out to condensation process, collect tangerine essential oil;
4. non-polar solvent reclaims: the non-polar solvent in distiller is reclaimed;
5. refining: to utilize supercritical CO
2to step 3. gained tangerine essential oil refine extraction treatment, supercritical CO
2flow is 10 ~ 50L/h, pressure 10 ~ 20Mpa, 40 ~ 80 ℃ of temperature, time 1 ~ 6h.
Most preferably following technical proposals of the extracting method of tangerine essential oil of the present invention:
1. raw material processing: the peel of Citrus reticulata Blanco of removing white cortex is carried out to crushed after being dried to 100nm, the peel of Citrus reticulata Blanco particle of pulverizing is dissolved in non-polar solvent, peel of Citrus reticulata Blanco particle is 1g:50ml with the ratio of non-polar solvent, gained peel of Citrus reticulata Blanco solution is carried out to microwave treatment until peel of Citrus reticulata Blanco particle dissolves completely, microwave treatment conditions is: microwave power 400W, microwave time 10min;
2. distillation: by step 1. gained peel of Citrus reticulata Blanco solution be placed in steam still and distill processing, the pressure of distiller is 5Mpa, distilling number of times is 5 times, distillation time summation is 3h, must contain the steam of tangerine essential oil;
3. condensation: the step steam that 2. gained contains tangerine essential oil is carried out to condensation process, collect tangerine essential oil;
4. non-polar solvent reclaims: the non-polar solvent in distiller is reclaimed;
5. refining: to utilize supercritical CO
2to step 3. gained tangerine essential oil refine extraction treatment, supercritical CO
2flow is 25L/h, pressure 10Mpa, temperature 50 C, time 2h.
Another object of the present invention is to provide the tangerine essential oil of being prepared by aforesaid method.
The invention has the beneficial effects as follows: the extracting method of tangerine essential oil provided by the invention adopts microwave method, vapor distillation method and supercritical extraction to combine, and can effectively improve the oil yield of peel of Citrus reticulata Blanco, and its oil yield of more traditional vapor distillation method has improved approximately 20%.Meanwhile, improve the purity of tangerine essential oil, obtain the tangerine essential oil of food grade, because supercritical extraction is only applied in the purification step in extraction of essential oil, therefore to a certain degree reduced process costs.Utilize the tangerine essential oil that the inventive method makes to can be used for multiple fields such as food interpolation.
Embodiment
Following non-limiting example can make the present invention of those of ordinary skill in the art's comprehend, but does not limit the present invention in any way.
Embodiment 1
1. raw material processing: the grapefruit peel of removing white cortex is carried out to crushed after being dried to 100nm, the grapefruit peel particle of pulverizing is dissolved in non-polar solvent, grapefruit peel particle is 1g:50ml with the ratio of non-polar solvent, gained grapefruit peel solution is carried out to microwave treatment until grapefruit peel particle dissolves completely, microwave treatment conditions is: microwave power 400W, microwave time 10min;
2. distillation: by step 1. gained grapefruit peel solution be placed in steam still and distill processing, the pressure of distiller is 5Mpa, distilling number of times is 5 times, distillation time summation is 3h, must contain the steam of grapefruit peel essential oil;
3. condensation: the step steam that 2. gained contains grapefruit peel essential oil is carried out to condensation process, collect grapefruit peel essential oil;
4. non-polar solvent reclaims: the non-polar solvent in distiller is reclaimed;
5. refining: to utilize supercritical CO
2to step 3. gained grapefruit peel essential oil refine extraction treatment, supercritical CO
2flow is 25L/h, pressure 10Mpa, temperature 50 C, time 2h.
Claims (10)
1. an extracting method for tangerine essential oil, comprises following processing step:
1. raw material processing: the peel of Citrus reticulata Blanco of removing white cortex is carried out to crushed after being dried to 200nm, the peel of Citrus reticulata Blanco particle of pulverizing is dissolved in non-polar solvent, gained peel of Citrus reticulata Blanco solution is carried out to microwave treatment until peel of Citrus reticulata Blanco particle dissolves completely;
2. distillation: by step 1. gained peel of Citrus reticulata Blanco solution be placed in steam still and distill processing, must contain the steam of tangerine essential oil;
3. condensation: the step steam that 2. gained contains tangerine essential oil is carried out to condensation process, collect tangerine essential oil;
4. non-polar solvent reclaims: the non-polar solvent in distiller is reclaimed;
5. refining: to utilize supercritical CO
2to step 3. gained tangerine essential oil refine extraction treatment.
2. method according to claim 1, is characterized in that: described step 1.: undertaken crushed after being dried to 50 ~ 150nm by removing the peel of Citrus reticulata Blanco of white cortex.
3. method according to claim 1, is characterized in that: described step 1. middle non-polar solvent is vegetables oil.
4. method according to claim 1, is characterized in that: described step 1. middle peel of Citrus reticulata Blanco particle is 1g:20 ~ 100ml with the ratio of non-polar solvent.
5. method according to claim 1, is characterized in that: described step 1. microwave treatment conditions is: microwave power 400 ~ 800W, microwave time 5 ~ 15min.
6. method according to claim 1, is characterized in that: described step 2.: solution is placed in steam still and distills processing, and the pressure of distiller is 5 ~ 10Mpa, distillation time 1h ~ 6h.
7. method according to claim 6, is characterized in that: described distillation number of times is 1 ~ 5 time, and distillation time summation is 1h ~ 6h.
8. method according to claim 1, is characterized in that: described step 5.: utilize supercritical CO
2to step 3. gained tangerine essential oil refine extraction treatment, supercritical CO
2flow is 10 ~ 50L/h, pressure 10 ~ 20Mpa, 40 ~ 80 ℃ of temperature, time 1 ~ 6h.
9. according to the method described in the arbitrary claim of claim 1 ~ 8, it is characterized in that:
1. raw material processing: the peel of Citrus reticulata Blanco of removing white cortex carry out crushed after being dried to 50 ~ 150nm, the peel of Citrus reticulata Blanco particle of pulverizing is dissolved in non-polar solvent, peel of Citrus reticulata Blanco particle is 1g:20 ~ 100ml with the ratio of non-polar solvent, gained peel of Citrus reticulata Blanco solution is carried out to microwave treatment until peel of Citrus reticulata Blanco particle dissolves completely, microwave treatment conditions is: microwave power 400 ~ 800W, microwave time 5 ~ 15min;
2. distillation: by step 1. gained peel of Citrus reticulata Blanco solution be placed in steam still and distill processing, the pressure of distiller is 5 ~ 10Mpa, distilling number of times is 1 ~ 5 time, distillation time summation is 1h ~ 6h, must contain the steam of tangerine essential oil;
3. condensation: the step steam that 2. gained contains tangerine essential oil is carried out to condensation process, collect tangerine essential oil;
4. non-polar solvent reclaims: the non-polar solvent in distiller is reclaimed;
5. refining: to utilize supercritical CO
2to step 3. gained tangerine essential oil refine extraction treatment, supercritical CO
2flow is 10 ~ 50L/h, pressure 10 ~ 20Mpa, 40 ~ 80 ℃ of temperature, time 1 ~ 6h.
10. a tangerine essential oil of being prepared by method described in claim 1.
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| CN201210460934.4A CN103805341A (en) | 2012-11-15 | 2012-11-15 | Extraction method of orange peel essential oil |
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| CN201210460934.4A CN103805341A (en) | 2012-11-15 | 2012-11-15 | Extraction method of orange peel essential oil |
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Cited By (16)
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|---|---|---|---|---|
| CN104004592A (en) * | 2014-06-11 | 2014-08-27 | 湖南鑫利生物科技有限公司 | Method for simultaneously extracting essential oil and pectin from fresh citrus peels |
| CN104130864A (en) * | 2014-07-16 | 2014-11-05 | 湖北中烟工业有限责任公司 | Preparation method of sweet orange flavor for cigarettes |
| CN104403801A (en) * | 2014-12-19 | 2015-03-11 | 杨玉峰 | Method for extracting orange peel essential oil with surfactant aqueous solution |
| CN104593152A (en) * | 2015-01-26 | 2015-05-06 | 福建农林大学 | Method for supercritical CO2 fluid extraction of mango peel essence |
| CN105087153A (en) * | 2015-09-02 | 2015-11-25 | 广州绿萃生物科技有限公司 | Dried tangerine peel oil extracting method |
| CN105886121A (en) * | 2014-11-14 | 2016-08-24 | 上海霖成生物科技有限公司 | Preparation method of high-quality citrus essential oil |
| CN106244330A (en) * | 2016-08-26 | 2016-12-21 | 云南养瑞科技集团有限公司 | The preparation method of a kind of Pericarpium Citri Reticulatae quintessence oil and the application in Medicated cigarette thereof |
| CN106978257A (en) * | 2017-05-12 | 2017-07-25 | 贺州学院 | The extracting method of navel orange pericarp essential oil |
| CN107987968A (en) * | 2017-11-25 | 2018-05-04 | 防城港市润禾农林科技有限公司 | It is a kind of to be used to extract the aromatic oil processing technology that essence processing uses |
| CN108753464A (en) * | 2018-06-20 | 2018-11-06 | 江西思派思香料化工有限公司 | It is a kind of transfer and extracting natural perfume method and device |
| CN109517664A (en) * | 2018-12-18 | 2019-03-26 | 河南中烟工业有限责任公司 | A kind of width skin orange peel powder, preparation method and its application in cigarette filter rod |
| CN109549410A (en) * | 2016-08-12 | 2019-04-02 | 张太平 | A kind of fiber promoting sleep |
| CN110623009A (en) * | 2019-09-30 | 2019-12-31 | 广西壮族自治区农业科学院 | Sugarcane vinegar fragrance fumigant and preparation method thereof |
| CN111621365A (en) * | 2020-06-04 | 2020-09-04 | 成都泰罗科技有限公司 | Zanthoxylum essential oil and extraction process thereof |
| CN111676097A (en) * | 2020-06-01 | 2020-09-18 | 蓝彤生物科技(吉林)有限公司 | Extraction method of ginseng essential oil |
| CN112980585A (en) * | 2021-03-26 | 2021-06-18 | 江西科技师范大学 | Method for extracting orange peel essential oil |
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2012
- 2012-11-15 CN CN201210460934.4A patent/CN103805341A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104004592A (en) * | 2014-06-11 | 2014-08-27 | 湖南鑫利生物科技有限公司 | Method for simultaneously extracting essential oil and pectin from fresh citrus peels |
| CN104004592B (en) * | 2014-06-11 | 2016-04-13 | 湖南鑫利生物科技有限公司 | A kind of method simultaneously extracting essential oil and pectin from fresh peel of Citrus reticulata Blanco |
| CN104130864A (en) * | 2014-07-16 | 2014-11-05 | 湖北中烟工业有限责任公司 | Preparation method of sweet orange flavor for cigarettes |
| CN105886121A (en) * | 2014-11-14 | 2016-08-24 | 上海霖成生物科技有限公司 | Preparation method of high-quality citrus essential oil |
| CN104403801A (en) * | 2014-12-19 | 2015-03-11 | 杨玉峰 | Method for extracting orange peel essential oil with surfactant aqueous solution |
| CN104593152A (en) * | 2015-01-26 | 2015-05-06 | 福建农林大学 | Method for supercritical CO2 fluid extraction of mango peel essence |
| CN105087153B (en) * | 2015-09-02 | 2018-08-07 | 广州绿萃生物科技有限公司 | A kind of extracting method of Oleum Citri Reticulatae |
| CN105087153A (en) * | 2015-09-02 | 2015-11-25 | 广州绿萃生物科技有限公司 | Dried tangerine peel oil extracting method |
| CN109549410A (en) * | 2016-08-12 | 2019-04-02 | 张太平 | A kind of fiber promoting sleep |
| CN106244330A (en) * | 2016-08-26 | 2016-12-21 | 云南养瑞科技集团有限公司 | The preparation method of a kind of Pericarpium Citri Reticulatae quintessence oil and the application in Medicated cigarette thereof |
| CN106978257A (en) * | 2017-05-12 | 2017-07-25 | 贺州学院 | The extracting method of navel orange pericarp essential oil |
| CN107987968A (en) * | 2017-11-25 | 2018-05-04 | 防城港市润禾农林科技有限公司 | It is a kind of to be used to extract the aromatic oil processing technology that essence processing uses |
| CN108753464A (en) * | 2018-06-20 | 2018-11-06 | 江西思派思香料化工有限公司 | It is a kind of transfer and extracting natural perfume method and device |
| CN109517664A (en) * | 2018-12-18 | 2019-03-26 | 河南中烟工业有限责任公司 | A kind of width skin orange peel powder, preparation method and its application in cigarette filter rod |
| CN110623009A (en) * | 2019-09-30 | 2019-12-31 | 广西壮族自治区农业科学院 | Sugarcane vinegar fragrance fumigant and preparation method thereof |
| CN110623009B (en) * | 2019-09-30 | 2021-09-14 | 广西壮族自治区农业科学院 | Sugarcane vinegar fragrance fumigant and preparation method thereof |
| CN111676097A (en) * | 2020-06-01 | 2020-09-18 | 蓝彤生物科技(吉林)有限公司 | Extraction method of ginseng essential oil |
| CN111621365A (en) * | 2020-06-04 | 2020-09-04 | 成都泰罗科技有限公司 | Zanthoxylum essential oil and extraction process thereof |
| CN112980585A (en) * | 2021-03-26 | 2021-06-18 | 江西科技师范大学 | Method for extracting orange peel essential oil |
| CN112980585B (en) * | 2021-03-26 | 2022-08-26 | 江西科技师范大学 | Method for extracting orange peel essential oil |
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Application publication date: 20140521 |