CN105087153A - Dried tangerine peel oil extracting method - Google Patents
Dried tangerine peel oil extracting method Download PDFInfo
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- CN105087153A CN105087153A CN201510554377.6A CN201510554377A CN105087153A CN 105087153 A CN105087153 A CN 105087153A CN 201510554377 A CN201510554377 A CN 201510554377A CN 105087153 A CN105087153 A CN 105087153A
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Abstract
The invention provides a dried tangerine peel oil extracting method. According to the method, dried tangerine peels are ground to 80-100 meshes by a liquid nitrogen grinder, a dried tangerine peel raw material is obtained, and the moisture content is controlled to range from 15% to 25%; the dried tangerine peel raw material is extracted by the aid of propane and butane mixed alkane at the temperature of 25-35 DEG C and under the pressure of 0.2-0.5 MPa for 30-40 min; the extracted dried tangerine peel raw material is subjected to extraction by the aid of supercritical CO2 again at the temperature of 50-65 DEG C and under the pressure of 10-20 MPa for 50-70 min, and dried tangerine peel oil is obtained through resolution and separation. The method is used for extracting the dried tangerine peel oil, the extraction ratio is higher than 6.4%, the dried tangerine peel oil is rich in functional components, contains more than 62% of polymethoxyflavonoids, has the bright yellow and transparent color, has the pure and strong fragrance and is free of the irritating odor and the biting taste, and the retention degree of the original flavor of the dried tangerine peels is high.
Description
Technical field
The present invention relates to a kind of extraction process of Oleum Citri Reticulatae, particularly relate to that a kind of functional ingredient enriches, polymethoxyflavone class substances content is high, color and luster is bright orange, fragrance pure dense, have no irritating odor, without the extracting method of sharp flavor, Oleum Citri Reticulatae that dried orange peel original local flavor reservation degree is high.
Background technology
Dried orange peel is the dry pericarp of maturation of Rutaceae citrus plant tangerine and mutation thereof.Dried orange peel has the functions such as regulating qi-flowing for strengthening spleen, appetite-stimulating indigestion-relieving, eliminating dampness and eliminating phlegm, hypotensive, reducing blood-fat, and has significant health value, and medical, edible is with a long history, dark liking by domestic and international consumers in general.Oleum Citri Reticulatae is the main composition of dried orange peel, research shows Oleum Citri Reticulatae mainly containing the material such as volatile component and flavonoid (particularly polymethoxyflavone) such as terpenes, Flavonoid substances have anticancer, anti-inflammatory, anti-oxidant, reduce the multiple pharmacological effect such as cholesterol.
Oleum Citri Reticulatae in the market mainly adopts the single methods such as milling process, organic solvent method, supercritical fluid extraction to extract, and DNA extration is single, shortage coupling.The Oleum Citri Reticulatae foreign matter content that milling process obtains is comparatively large, color and luster is dim, quality is general; The Oleum Citri Reticulatae functional component kind that organic solvent method obtains is abundant not, fragrance is strong not, even there is the risk of dissolvent residual; And directly adopt supercritical CO
2the Oleum Citri Reticulatae that extraction process obtains, with strong sharp flavor and irritating smell, can not retain the original local flavor of dried orange peel largely.In addition, before extracting, dried orange peel is generally based on mechanical disintegration, and rub during pulverizing easy heat production, and the volatile aroma component of dried orange peel and functional mass are very easily run off.And functional active components enriches, original local flavor reserving degree is high, fragrance is pure, the bright clear Oleum Citri Reticulatae product of color and luster does not also occur in the market.
Bai Weidong is the flavonoid compound that Extraction medium is extracted in Xinhui tangerine peel with ethanolic soln in the research of Extraction Process of Total Flavones " in the Xinhui tangerine peel ", and under optimum extraction process, Xinhui tangerine peel flavones yield is only 0.80%.
Huang Jingsheng is at " supercritical CO
2extraction Pericarpium Citri Reticulatae volatile oil and chemical composition analysis " in have studied supercritical CO
2the processing condition of extraction Pericarpium Citri Reticulatae volatile oil, in gained Pericarpium Citri Reticulatae volatile oil, polymethoxyflavone content is 33.6%.
Zhou Guohai adopts low temperature continuous phase transistion abstraction technique to utilize butane to extract volatile oil from dried orange peel in " the low temperature continuous phase transistion extraction of Pericarpium Citri Reticulatae volatile oil and specificity analysis ", and polymethoxyflavone class material is only containing 10.6%.
Chinese patent disclosed " a kind of method of continuous phase transistion extraction Oleum Citri Reticulatae " (201310096857.3), adopt propane, butane, high-purity Trimethylmethane, Tetrafluoroethane, one among sulfur hexafluoride and liquefied petroleum gas (LPG) is as solvent, continuous phase transistion cycling extraction technology is adopted to extract Oleum Citri Reticulatae, but because adopt 50 DEG C of-60 DEG C of drying modes to control the moisture of dried orange peel raw material, adopt cut mechanically pulverizing and granularity is bigger, and solvent single and lack combination, the Oleum Citri Reticulatae extracted is yellow to reddish-brown semi-solid paste, color and luster is bright and thoroughly clear not, in oven dry and crushing process, aroma component rate of loss is slightly high, polymethoxyflavone class substances content is also lower, functional component is abundant not.
Chinese patent disclosed " a kind of Pericarpium Citri Reticulatae extract and its preparation method and application " (201110023489.0) provides a kind of Pericarpium Citri Reticulatae extract, and this extract is through supercritical CO
2extraction prepares, and this extract contains flavonoid and ter penoids, can effective function of spleen and stomach regulating function, has effect of weight reducing.But this extract directly extracts from dried orange peel raw material and obtains, dried orange peel raw material is not through pre-treatments such as past sharp flavor, decolourings, the extract color and luster obtained is darker, also there is larger sharp flavor and irritating smell, fragrance is lighter and pure not, dried orange peel original local flavor reservation degree is lower, is unfavorable for the application in food or functional food.
Chinese patent application disclosed " a kind of Pericarpium Citri Reticulatae extract and its preparation method and application " (201110023459.X) provide a kind of Pericarpium Citri Reticulatae extract, and it is through supercritical CO
2or water extraction or organic solvent extraction obtain, its extracting mode is single, lack integrated coupling etc. to repeat to extract, dried orange peel raw material is not through pre-treatments such as removal of impurities, the extract obtained has certain effect, but it is not high to there is more impurity, active constituent content, and utilize poisonous organic solvent as methyl alcohol extract time, there is the risk of certain dissolvent residual and the hidden danger of food safety in product.
Summary of the invention
The object of the invention is to solve the deficiency in existing Oleum Citri Reticulatae extraction process, provide that a kind of functional ingredient enriches, polymethoxyflavone class substances content is high, color and luster is bright orange, fragrance pure dense, have no irritating odor, without sharp flavor, its extraction process of Oleum Citri Reticulatae that dried orange peel original local flavor reservation degree is high.
For achieving the above object, embodiment of the present invention are: a kind of extraction process of Oleum Citri Reticulatae, comprises the following steps:
(1) dry, pulverizing: utilize liquid nitrogen pulverizer, tangerine peel powder is broken to 80 ~ 100 orders, obtain dried orange peel raw material, controls water content in 15% ~ 25% simultaneously.
(2) subcritical mixed alkanes removal of impurities, decolouring, removal sharp flavor and pungency volatile matter: utilize propane, butane mixed alkanes, 25 ~ 35 DEG C, under 0.2 ~ 0.5MPa, 30 ~ 40min is extracted to dried orange peel raw material, described dried orange peel raw material and mixed alkanes bulking value proportioning be 1:3 ~ 5, in described propane, butane mixed alkanes, the volume ratio of propane and butane is 1:1 ~ 3.
(3) supercritical CO
2extract: the dried orange peel raw material after extracting in (2) is used supercritical CO again
2extracting, temperature 50 C ~ 65 DEG C, pressure 10 ~ 20MPa, extraction time 50 ~ 70min, obtaining Oleum Citri Reticulatae through resolving separation.
As optimization, in step (1), dried orange peel raw material controls water content in 15%.
As optimization, in step (2), described dried orange peel raw material and mixed alkanes bulking value proportioning be 1:3, in propane butane mixed alkanes, the volume ratio of propane and butane is 1:3, under Extracting temperature 25 DEG C, pressure 0.5MPa, extraction time 40min.
As optimization, in step (3), Extracting temperature 50 DEG C, pressure 20MPa, extraction time 50min.
The present invention for extracting Oleum Citri Reticulatae, extraction yield more than 6.4%, its functional ingredient is abundant, bright orange clear, the fragrance of polymethoxyflavone class substances content more than 62%, color pure strong, have no irritating odor, high without sharp flavor, dried orange peel original local flavor reservation degree.
Advantage of the present invention is:
1, adopt liquid nitrogen pulverizer to carry out drying, pulverizing to dried orange peel, the loss of the volatile functional component of dried orange peel in drying, disintegrating process can be reduced.
2, adopt subcritical mixed alkanes to carry out pre-treatment to dried orange peel raw material, the object of effective removal of impurities, decolouring, removal sharp flavor and pungency volatile matter can be reached.
3, by the dried orange peel raw material supercritical CO after process
2extract, the Oleum Citri Reticulatae functional ingredient obtained be abundant, polymethoxyflavone class substances content is high, bright orange clear, the fragrance of color pure strong, have no irritating odor, high without sharp flavor, dried orange peel original local flavor reservation degree.
4, the extraction agent used is as alkane, CO
2be all that safe nontoxic food extracts auxiliary agent, extract the not residual hazardous and noxious substances of the Oleum Citri Reticulatae obtained thus, security is high, product are of fine quality.
Accompanying drawing explanation
Fig. 1 is the dried orange peel oil volatility functional component GCMS collection of illustrative plates that the present invention obtains, and compares with Fig. 3, and the functional mass of the Oleum Citri Reticulatae that known the present invention obtains comparatively speaking abundant species, content is high.
Fig. 2 be dried orange peel raw material without alkane treatment, and directly use supercritical CO
2the volatility functional component GCMS collection of illustrative plates of the dried orange peel extracted.
Fig. 3 is the ultraviolet-visible light full wavelength scanner figure of the Oleum Citri Reticulatae that the present invention obtains.
Embodiment
Embodiment 1:
Get a certain amount of dried orange peel, utilize liquid nitrogen pulverizer, tangerine peel powder is broken to 100 orders, control water content in 15% simultaneously, obtain dried orange peel raw material.Get the dried orange peel raw material of 8.055kg, utilize mixed alkanes (propane: butane=1:1), dried orange peel raw material and mixed alkanes bulking value proportioning be 1:4,25 DEG C, under 0.5MPa, extract 35min.By the dried orange peel raw material supercritical CO after extraction
2extract, control temperature is 50 DEG C, pressure is 20MPa, extraction time is 50min, Oleum Citri Reticulatae 0.554kg is obtained through resolving separation, this Oleum Citri Reticulatae color is bright orange, fragrance pure strong, have no irritating odor, high without sharp flavor, dried orange peel original local flavor reservation degree, functional ingredient enriches, and ultraviolet spectrophotometer method records polymethoxyflavone class substances content 65.71%.
Embodiment 2:
Get a certain amount of dried orange peel, utilize liquid nitrogen pulverizer, tangerine peel powder is broken to 90 orders, control water content in 20% simultaneously, obtain dried orange peel raw material.Get the dried orange peel raw material of 7.876kg, utilize mixed alkanes (propane: butane=1:2), dried orange peel raw material and mixed alkanes bulking value proportioning be 1:5,30 DEG C, under 0.4MPa, extract 30min.By the dried orange peel raw material supercritical CO after extraction
2extract, control temperature is 60 DEG C, pressure is 15MPa, extraction time is 60min, Oleum Citri Reticulatae 0.503kg is obtained through resolving separation, this Oleum Citri Reticulatae color is bright orange, fragrance pure strong, have no irritating odor, high without sharp flavor, dried orange peel original local flavor reservation degree, functional ingredient enriches, and ultraviolet spectrophotometer method records polymethoxyflavone class substances content 62.43%.
Embodiment 3:
Get a certain amount of dried orange peel, utilize liquid nitrogen pulverizer, tangerine peel powder is broken to 80 orders, control water content in 20% simultaneously, obtain dried orange peel raw material.Get the dried orange peel raw material of 7.567kg, utilize mixed alkanes (propane: butane=1:3), dried orange peel raw material and mixed alkanes bulking value proportioning be 1:3,35 DEG C, under 0.2MPa, extract 40min.By the dried orange peel raw material supercritical CO after extraction
2extract, control temperature is 65 DEG C, pressure is 10MPa, extraction time is 70min, Oleum Citri Reticulatae 0.489kg is obtained through resolving separation, this Oleum Citri Reticulatae color is bright orange, fragrance pure strong, have no irritating odor, high without sharp flavor, dried orange peel original local flavor reservation degree, functional ingredient enriches, and ultraviolet spectrophotometer method records polymethoxyflavone class substances content 67.85%.
Embodiment 4:
Get a certain amount of dried orange peel, utilize liquid nitrogen pulverizer, tangerine peel powder is broken to 80 orders, control water content in 20% simultaneously, obtain dried orange peel raw material.Get the dried orange peel raw material of 8.012kg, utilize mixed alkanes (propane: butane=1:3), dried orange peel raw material and mixed alkanes bulking value proportioning be 1:3,35 DEG C, under 0.3MPa, extract 40min.By the dried orange peel raw material supercritical CO after extraction
2extract, control temperature is 55 DEG C, pressure is 10MPa, extraction time is 65min, Oleum Citri Reticulatae 0.537kg is obtained through resolving separation, this Oleum Citri Reticulatae color is bright orange, fragrance pure strong, have no irritating odor, high without sharp flavor, dried orange peel original local flavor reservation degree, functional ingredient enriches, and ultraviolet spectrophotometer method records polymethoxyflavone class substances content 64.28%.
Claims (4)
1. an extracting method for Oleum Citri Reticulatae, is characterized in that, comprises the following steps:
(1) utilize liquid nitrogen pulverizer, tangerine peel powder is broken to 80 ~ 100 orders, obtain dried orange peel raw material, control water content in 15% ~ 25% simultaneously;
(2) propane, butane mixed alkanes is utilized, 25 ~ 35 DEG C, under 0.2 ~ 0.5MPa, 30 ~ 40min is extracted to dried orange peel raw material, described dried orange peel raw material and mixed alkanes bulking value proportioning be 1:3 ~ 5, in described propane, butane mixed alkanes, the volume ratio of propane and butane is 1:1 ~ 3;
(3) the dried orange peel raw material after extraction in (2) is used supercritical CO again
2extracting, temperature 50 C ~ 65 DEG C, pressure 10 ~ 20MPa, extraction time 50 ~ 70min, obtaining Oleum Citri Reticulatae through resolving separation.
2. the extracting method of Oleum Citri Reticulatae according to claim 1, is characterized in that, in step (1), dried orange peel raw material controls water content 15%.
3. the extracting method of Oleum Citri Reticulatae according to claim 1, it is characterized in that, in step (2), described dried orange peel raw material and mixed alkanes bulking value proportioning be 1:3, in propane butane mixed alkanes, the volume ratio of propane and butane is 1:3, under Extracting temperature 25 DEG C, pressure 0.5MPa, extraction time 40min.
4. the extracting method of Oleum Citri Reticulatae according to claim 1, is characterized in that, in step (3), and Extracting temperature 50 DEG C, pressure 20MPa, extraction time 50min.
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| CN110029015A (en) * | 2019-04-12 | 2019-07-19 | 福州帅宝生物科技有限公司 | A kind of extracting method of coix seed oil |
| CN110240968A (en) * | 2019-06-08 | 2019-09-17 | 深圳市喜云实业有限公司 | A kind of extraction process of pollen pini absolute oil |
| CN111149874A (en) * | 2020-01-11 | 2020-05-15 | 长沙围度美容服务有限公司 | A weight reducing oil containing tea leaf extract |
| CN114832051A (en) * | 2022-05-17 | 2022-08-02 | 仁和全域(上海)大健康研究院有限公司 | Guangchenpi oil composition and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110029015A (en) * | 2019-04-12 | 2019-07-19 | 福州帅宝生物科技有限公司 | A kind of extracting method of coix seed oil |
| CN110240968A (en) * | 2019-06-08 | 2019-09-17 | 深圳市喜云实业有限公司 | A kind of extraction process of pollen pini absolute oil |
| CN111149874A (en) * | 2020-01-11 | 2020-05-15 | 长沙围度美容服务有限公司 | A weight reducing oil containing tea leaf extract |
| CN114832051A (en) * | 2022-05-17 | 2022-08-02 | 仁和全域(上海)大健康研究院有限公司 | Guangchenpi oil composition and preparation method and application thereof |
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