CN103045354A - Method for extracting seabuckthorn fruit by supercritical CO2 - Google Patents

Method for extracting seabuckthorn fruit by supercritical CO2 Download PDF

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Publication number
CN103045354A
CN103045354A CN 201210459506 CN201210459506A CN103045354A CN 103045354 A CN103045354 A CN 103045354A CN 201210459506 CN201210459506 CN 201210459506 CN 201210459506 A CN201210459506 A CN 201210459506A CN 103045354 A CN103045354 A CN 103045354A
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Prior art keywords
fructus hippophae
extraction
supercritical
extracting
plant milk
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CN 201210459506
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Chinese (zh)
Inventor
赵志侃
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SHANXI WUTAISHAN SEA-BUCKTHORN PRODUCT Co Ltd
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SHANXI WUTAISHAN SEA-BUCKTHORN PRODUCT Co Ltd
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Priority to CN 201210459506 priority Critical patent/CN103045354A/en
Publication of CN103045354A publication Critical patent/CN103045354A/en
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Abstract

The invention relates to an extraction method of plant fruits, and particularly relates to a method for extracting seabuckthorn fruits by supercritical CO2. The method for extracting the seabuckthorn fruits by the supercritical CO2 solves a technical problem related to extraction and utilization of nutrient substances of the seabuckthorn fruits, and comprises the following steps of: a. drying and crushing the seabuckthorn fruits and then placing into an extraction kettle; b. injecting the supercritical CO2 into the extraction kettle, and extracting for 3.5-4.5 hours under the condition that the temperature is 45-55 DEG C, the pressure is 1.2-2.0MPa and the CO2 flow is 0.10-0.15L/min; and c. conveying CO2 flow with dissolved plant extracts of the seabuckthorn fruits into a separation kettle to separate the plant extracts of the seabuckthorn fruits, and compressing the CO2 and then conveying the CO2 into the extraction kettle for cycle use. According to the method for extracting the plant extracts of the seabuckthorn fruits by the supercritical CO2, the content of vitamin E in the extracted plant extracts of the seabuckthorn fruits is 100mg/100g.

Description

Supercritical CO 2The method of extraction Fructus Hippophae
Technical field
The present invention relates to a kind of fruit extracting process, specifically a kind of supercritical CO 2The method of extraction Fructus Hippophae.
Background technology
Sea-buckthorn has another name called vinegar willow, Hei Ci and acid thorn etc., is a kind of anti-do cold, Salt And Alkali Tolerance, impoverishment tolerant, extremely strong perennial shrub or dungarunga fruit tree of vitality.Sea-buckthorn is the precious nonwood forest trees that contains in the world the natural complex most species at present, and its ascorbic content is higher than bright jujube and Kiwifruit far away, thereby is described as the treasure-house of natural complex.
The plant milk extract of Fructus Hippophae is comprised of multiple beneficial lipid acid such as palmitinic acid, physetoleic acid, stearic acid, oleic acid, linolic acid, linolenic acid, wherein unsaturated fatty acids is up to 70%, and the indispensable vitamin A of carotenoid and vitamin-E and various trace elements such as human body in the Oleum Hippophae, selenium, magnesium, zinc, iron, manganese equal size are also higher.The shortcomings such as present extraction process has organic solvent residual, and extraction efficiency is not high, loss of effective components is larger.
200910263590.6 method of from seabuckthorn fruit peel, extracting β-carotene.A kind of method of extracting β-carotene from seabuckthorn fruit peel of the present invention comprises the steps: 1) the sea-buckthorn branch of step of preparing fruit peel after to the squeezing sea buckthorn juice carry out roughing, dries, screens and to get seabuckthorn fruit peel; 2) extraction step is carried out SCF-CO 2 to the seabuckthorn fruit peel that extracts; Its processing condition are: 42.5 ℃~45 ℃ of extraction temperature, extracting pressure 25MPa~30MPa, time 2.5h; 3) get red-brown oily liquids seabuckthorn fruit peel oil, oil yield is 8.0%.Contain higher β-carotene composition in this seabuckthorn fruit peel oil.
Summary of the invention
The present invention provides a kind of supercritical CO in order to solve the technical problem of Fructus Hippophae nutritive substance extraction and application 2The method of extraction Fructus Hippophae.
Technical scheme of the present invention is a kind of supercritical CO 2The method of extraction Fructus Hippophae, step is as follows:
A, will put into extraction kettle after the Fructus Hippophae drying and crushing;
B, with the CO of supercritical state 2Injecting extraction kettle, is 45~55 ℃ in temperature, and pressure is 1.2~2.0Mpa, CO 2Flow velocity is: under the condition of 0.10~0.15L/min, extract 3.5~4.5 hours;
C, be dissolved with the CO of Fructus Hippophae plant milk extract 2Fluid enters separating still, the Fructus Hippophae plant milk extract is separated CO by regulating 48~60 ℃ of temperature and pressure 2.0Mpa~3.0Mpa 2Gas enters after compression extraction kettle and recycles.
Above-mentioned supercritical CO 2The extraction Fructus Hippophae obtains the method for plant milk extract, wherein, and described supercritical CO 2The preferred temperature of extraction is 50 ℃, and pressure is 1.7Mpa, CO 2Flow velocity is 0.12L/min.
Above-mentioned SCF-CO 2 Fructus Hippophae obtains the method for plant milk extract, and wherein, described drying is carried out in temperature is lower than 80 ℃ baking oven, and dry 1.5~2 hours, the Fructus Hippophae moisture content after the drying was lower than 10%.
Above-mentioned supercritical CO 2The method of extraction Fructus Hippophae plant milk extract, the content of the vitamin-E in the Fructus Hippophae plant milk extract of extraction gained reaches 100mg/100g.
Supercritical CO of the present invention 2The method that the extraction Fructus Hippophae obtains plant milk extract first with the Fructus Hippophae drying and crushing, has overcome because the Fructus Hippophae appearance is hard CO before extracting 2Fluid can't penetrate its appearance and the incomplete defective of extraction that causes, has increased Fructus Hippophae and CO 2The contact area of fluid was pulverized Fructus Hippophae 40 mesh sieves simultaneously, and its granularity is just so that CO 2Fluid is circulate in extraction process, contacts more fully with Fructus Hippophae, thereby has further improved the extraction efficiency of Fructus Hippophae plant milk extract.
Supercritical CO of the present invention 2The extraction Fructus Hippophae obtains CO used in the method for plant milk extract 2Purity is more than or equal to 99%, CO 2Be rare gas element, can operate at normal temperatures, can effectively prevent oxidation and the decomposition of thermo-sensitivity composition and chemically unstable composition, utilize CO 2Be in the large character of the high-density, low viscosity and the spread coefficient that have under the supercritical state and extract effective constituent in the Fructus Hippophae, then will be dissolved in CO in the method that heats up with step-down 2Solute in the fluid separates, and plays the dual function of extracting and distilling, and can finish a leaching process in 2.5~4 hours.The method operational cycle is short, extraction efficiency is high, can avoid the residual of organic solvent simultaneously, in addition, because CO 2Cheap and easy to get, general recyclable about 80%, saved the energy, simultaneously because CO 2Without incendivity, use safety and environmentally safe.
Supercritical CO of the present invention 2The method technique that the extraction Fructus Hippophae obtains plant milk extract is simple, easy to operate, greatly improved production efficiency, Fructus Hippophae with the method extraction obtains plant milk extract, avoided the residual of organic solvent, shortened extraction time, improve the extraction efficiency of Fructus Hippophae, especially greatly improved the content of vitamin-E in the Fructus Hippophae plant milk extract.The content of the vitamin-E in the Fructus Hippophae plant milk extract of extraction gained reaches 100mg/100g, and effect of extracting is obvious.
Embodiment
Plant milk extract check (high performance liquid chromatography)
Instrument and reagent: effect liquid phase chromatogram instrument, vitamin-E standard model.
Sample determination
(1) configuration vitamin-E standard model solution, the drawing standard curve.
(2) configuration sample solution.
(3) use liquid chromatograph, press the chromatographic condition operation, obtain chromatographic peak area.Peak area according to each point on the typical curve calculates with external standard method.
(4) result calculates
The content X of vitamin-E 2Represent (%) with massfraction
Formula:
Figure DEST_PATH_IMAGE001
In the formula: X 2: the content of the total vitamin-E of sample (%)
m St: the quality of standard substance (g)
m i: the quality of sample (g)
P St: the content of vitamin-E standard substance (%)
A i: the peak area of vitamin-E in the sample
A St: the peak area of vitamin-E in the standardized solution
Embodiment 1, the present invention's supercritical CO 2The extraction Fructus Hippophae obtains the method for plant milk extract, and wherein, the step of described method is as follows:
Fructus Hippophae was dried by the fire 2 hours in 80 ℃ baking oven, and the Fructus Hippophae water content after the drying is 10%, and dried Fructus Hippophae was pulverized 40 mesh sieves, and the Fructus Hippophae after then will sieving is put into supercritical extraction reactor and extracted.Be 45 ℃ in temperature, pressure is 2.0Mpa, CO 2Flow velocity is under the condition of 0.10L/min, extracts 4 hours, and the Fructus Hippophae plant milk extract is dissolved in supercritical CO 2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making 2Fructus Hippophae plant milk extract in the fluid is separated CO 2Recycle.The content of the vitamin-E in the Fructus Hippophae plant milk extract of extraction gained is:
Figure 541836DEST_PATH_IMAGE002
Embodiment 2, Fructus Hippophae was dried by the fire 1.5 hours in 80 ℃ baking oven, the Fructus Hippophae water content after the drying is 10%, and dried Fructus Hippophae was pulverized 40 mesh sieves, and the Fructus Hippophae after then will sieving is put into supercritical extraction reactor and extracted.Be 55 ℃ in temperature, pressure is 1.2Mpa, CO 2Flow velocity is under the condition of 0.15L/min, extracts 2.5 hours, and the Fructus Hippophae plant milk extract is dissolved in supercritical CO 2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making 2Fructus Hippophae plant milk extract in the fluid is separated CO 2Recycle.The content of the vitamin-E in the Fructus Hippophae plant milk extract of extraction gained is: 100mg/100g.
Embodiment 3, Fructus Hippophae was dried by the fire 1.5 hours in 80 ℃ baking oven, the Fructus Hippophae water content after the drying is 10%, and dried Fructus Hippophae was pulverized 40 mesh sieves, and the Fructus Hippophae after then will sieving is put into supercritical extraction reactor and extracted.Be 50 ℃ in temperature, pressure is 1.7Mpa, CO 2Flow velocity is under the condition of 0.12L/min, extracts 3 hours, and the Fructus Hippophae plant milk extract is dissolved in supercritical CO 2In the fluid, enter in the separating still, be dissolved in supercritical CO through overregulating temperature and pressure, making 2Fructus Hippophae plant milk extract in the fluid is separated CO 2Recycle.The content of the vitamin-E in the Fructus Hippophae plant milk extract of extraction gained is: 101mg/100g.
 
Here description of the invention and application is illustrative, is not to want that therefore, the present invention is not subjected to the restriction of present embodiment with scope restriction of the present invention in the above-described embodiments, and the technical scheme that the replacements such as any employing obtain is all in the scope of protection of the invention.

Claims (4)

1. supercritical CO 2The method of extraction Fructus Hippophae is characterized in that step is as follows:
A, will put into extraction kettle after the Fructus Hippophae drying and crushing;
B, with the CO of supercritical state 2Injecting extraction kettle, is 45~55 ℃ in temperature, and pressure is 1.2~2.0Mpa, CO 2Flow velocity is: under the condition of 0.10~0.15L/min, extract 3.5~4.5 hours;
C, be dissolved with the CO of Fructus Hippophae plant milk extract 2Fluid enters separating still, the Fructus Hippophae plant milk extract is separated CO by regulating 48~60 ℃ of temperature and pressure 2.0Mpa~3.0Mpa 2Gas enters after compression extraction kettle and recycles.
2. supercritical CO according to claim 1 2The method of extraction Fructus Hippophae is characterized in that described supercritical CO 2The preferred temperature of extraction is 50 ℃, and pressure is 1.7Mpa, CO 2Flow velocity is 0.12L/min.
3. supercritical CO according to claim 1 2The method of extraction Fructus Hippophae is characterized in that described drying is carried out in temperature is lower than 80 ℃ baking oven, dry 1.5~2 hours, the Fructus Hippophae moisture content after the drying was lower than 10%.
4. supercritical CO according to claim 1 2The method of extraction Fructus Hippophae is characterized in that Fructus Hippophae was pulverized 40 mesh sieves.
CN 201210459506 2012-11-15 2012-11-15 Method for extracting seabuckthorn fruit by supercritical CO2 Pending CN103045354A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105419938A (en) * 2015-12-28 2016-03-23 贵州航天乌江机电设备有限责任公司 Refining method of sea buckthorn oil
CN108434182A (en) * 2018-04-09 2018-08-24 内蒙古宇航人高技术产业有限责任公司 A kind of supercritical CO2The method that fluid extraction technology extracts Leaves of Hippophae L polyphenol
CN114042144A (en) * 2021-11-17 2022-02-15 山西五台山沙棘制品有限公司 Platycodon grandiflorum and almond paste and preparation method thereof
CN115251389A (en) * 2022-06-23 2022-11-01 南昌蜂芝缘健康科技有限公司 Ganoderma lucidum spore oil sea-buckthorn soft capsule and preparation method thereof

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105419938A (en) * 2015-12-28 2016-03-23 贵州航天乌江机电设备有限责任公司 Refining method of sea buckthorn oil
CN108434182A (en) * 2018-04-09 2018-08-24 内蒙古宇航人高技术产业有限责任公司 A kind of supercritical CO2The method that fluid extraction technology extracts Leaves of Hippophae L polyphenol
CN114042144A (en) * 2021-11-17 2022-02-15 山西五台山沙棘制品有限公司 Platycodon grandiflorum and almond paste and preparation method thereof
CN115251389A (en) * 2022-06-23 2022-11-01 南昌蜂芝缘健康科技有限公司 Ganoderma lucidum spore oil sea-buckthorn soft capsule and preparation method thereof

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Application publication date: 20130417