CN102071099B - Process for quickly breaking cell walls of Chinese wolfberry seeds and extracting seed oil - Google Patents
Process for quickly breaking cell walls of Chinese wolfberry seeds and extracting seed oil Download PDFInfo
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- CN102071099B CN102071099B CN 201110004255 CN201110004255A CN102071099B CN 102071099 B CN102071099 B CN 102071099B CN 201110004255 CN201110004255 CN 201110004255 CN 201110004255 A CN201110004255 A CN 201110004255A CN 102071099 B CN102071099 B CN 102071099B
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Abstract
The invention relates to a process for quickly breaking cell walls of Chinese wolfberry seeds and extracting seed oil. The process comprises the following steps of: (1) breaking the cell walls of the Chinese wolfberry seeds: crushing the cleaned and dried Chinese wolfberry seeds and filling into an extraction kettle; introducing CO2 into the extraction kettle; raising the pressure in the extraction kettle to the pressure of between 40 and 45MPa at normal temperature and keeping for 10 to 15 minutes; closing air inlet valves at the two ends of the extraction kettle; and reducing the pressure in the extraction kettle to atmospheric pressure in 1 to 5 minutes to obtain the wall-broken Chinese wolfberry seeds; and (2) filling the wall-broken Chinese wolfberry seeds obtained in the step (1) in the extraction kettle; introducing the CO2 at the same time; extracting under a supercritical condition for 60 to 70 minutes; and performing two-stage separation under reduced pressure to obtain the Chinese wolfberry seed oil. The process is simple and environmentally-friendly and is low in cost; the extraction time can be greatly shortened, so the oil yield reaches the maximum value in a shortest time; and the process can be widely applied to advanced development and production preparation of various functional unsaturated fatty acid medicaments and health foods thereof.
Description
Technical field
The present invention relates to the matrimony vine manufacture field, relate in particular to the quick broken wall of matrimony vine seed cell and seed oil extraction process.
Background technology
The matrimony vine seed is the byproduct in matrimony vine processing, accounts for 3% of whole grain, and processing 1t fresh fruit can get matrimony vine seed 30kg.To be the matrimony vine seed form through the methods such as squeezing or extraction are refining Boxthorn Seed Oil, contains a large amount of unsaturated fatty acidss, V in oil
EAnd phosphatide.Lycium-seed-oil also has medical care effect except edibleness is arranged, can be used for the assisting therapy to cardiovascular and cerebrovascular diseases such as hypertension, hyperlipidemia, atherosclerosiss.
Supercritical CO
2Fluid extraction (SFE-CO
2) technology is widely used in the fields such as medicine, food, chemical industry.This technique has easy to operate, and CO
2Nontoxic, tasteless, cheap and easy to get, nonflammable, no solvent residue but also can fully keep its activity in the natural product that not only can guarantee to extract.The report of supercritical extraction seed oil is a lot, but the extraction research of Boxthorn Seed Oil is reported seldom, mainly concentrates on theoretical numerical simulation and simple experiment of single factor research.Adopt fixedly other factors, the single factor investigation method that changes a factor is determined processing condition, and the interaction between can not the investigation factor also is difficult to the interaction relation between a plurality of analog values of investigation and factor simultaneously.Response surface method (response surface methodology, RSM) can adopt the funtcional relationship between a plurality of factors of quadratic regression equation match and a plurality of response value, seeks optimal processing parameter by the regression equation analysis.
Overcritical (SC) abstraction technique is to utilize the high-solvency of natural product under the SC state, and this feature extraction of low dissolving power under non-SC state and separate targets composition.But SC-CO
2A kind of non-polar solvent, during some composition in extracting natural product, CO
2Extraction efficiency can be strong because of its polarity, molecular weight is large, greatly reduced by factors such as related substance combinations.
Summary of the invention
Technical problem to be solved by this invention is to provide the quick broken wall of matrimony vine seed cell and the seed oil extraction process that a kind of percentage extraction is high, production cost is low.
For addressing the above problem, the quick broken wall of a kind of matrimony vine seed cell of the present invention and seed oil extraction process comprise the following steps:
(1) matrimony vine seed cell wall breaking is processed: after the matrimony vine seed of clean dry is crushed to granularity and is 20～60 orders, put into extraction kettle; Pass into CO to extraction kettle
2, after at normal temperatures the pressure in extraction kettle being elevated to 40～45MPa, keep 10～15min; Then close the air intake valve at extraction kettle two ends, make pressure drop in extraction kettle to normal atmosphere in 1～5min, obtain the matrimony vine seed after broken wall;
(2) the matrimony vine seed after the broken wall of described step (1) gained is packed in extraction kettle, pass into simultaneously CO
2, be that 28.5～30.0Mpa, temperature are that 40.2 ℃～45.0 ℃, the consumption of the entrainment agent ethanol every 100g of matrimony vine seed after by broken wall adds 6.88～8.45mL, CO at extraction kettle pressure
2Flow is to extract 60～70min under the super critical condition of 20～50L/h, namely gets Boxthorn Seed Oil after two-stage decompression separation.
Ethanol mass concentration in described step (2) is 95%.
Two-stage decompression separation in described step (2) refers to take pressure as 5～7Mpa, temperature as 40～50 ℃ as the one-level decompression separation, take pressure as 4～5Mpa, temperature separates as second depressurized as 30～40 ℃.
The present invention compared with prior art has the following advantages:
1, the present invention is first to supercritical CO
2The extraction Boxthorn Seed Oil is studied, on affect percentage extraction parameters be optimized, thereby determined optimum extraction process, belong to domestic the first.
2, the present invention carries out the extraction of seed oil by the mode of the matrimony vine seed first being carried out broken wall and then extracting, and not only greatly reduces extraction time, but also has effectively improved oil yield.
As can see from Figure 1, through the successful of overcritical broken wall treatment, after matrimony vine seed broken wall, (B) is more serious than (A) cell wall rupture before broken wall, thereby is conducive to the extraction of next step seed oil.
In order further to investigate overcritical broken wall to the impact of oil yield, we broken wall treatment with contrasting of broken wall treatment not, as can be seen from Figure 2 just can reach maximum oil yield through the sample 60min of broken wall treatment, and undressedly need to reach maximum value more than the time of 150min.Therefore can find out that overcritical broken wall treatment not only can reduce extraction time greatly, can also improve oil yield.
3, present device is simple, and is easy and simple to handle, with short production cycle, industrial consumption is few, production cost is low, is easy to industrial promotion and application, can accomplish scale production.
4, be carbonic acid gas because the present invention extracts fluid used, this safe fluid, reliable, inexpensive, be easy to get, therefore, production cost is low, and can not cause industrial pollution, belongs to environment-friendly production process.
5, to extract temperature relatively low due to the present invention, therefore, effectively protects two keys of unsaturated fatty acids not oxidated, thereby more fully keep its nutrition and physiologically active, also improved product quality simultaneously.
6, the present invention can be widely used in deep development and the manufacture of various functional unsaturated fatty acids medicines and protective foods thereof.
Description of drawings
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in further detail.
Fig. 1 is (B) electron-microscope scanning picture after (A) and broken wall before matrimony vine seed broken wall.
Fig. 2 is that the matrimony vine seed is through broken wall treatment and the not oil yield contrast of broken wall treatment.Wherein
Be matrimony vine seed broken wall treatment,
Be matrimony vine seed broken wall treatment not.
Embodiment
The embodiment 1 quick broken wall of matrimony vine seed cell and seed oil extraction process comprise the following steps:
(1) matrimony vine seed cell wall breaking is processed: after the matrimony vine seed of clean dry is crushed to granularity and is 20 orders, put into extraction kettle; Pass into CO to extraction kettle
2, after at normal temperatures the pressure in extraction kettle being elevated to 40MPa, keep 15min; Then close the air intake valve at extraction kettle two ends, make pressure drop in extraction kettle to normal atmosphere in 1min, obtain the matrimony vine seed after broken wall.
(2) the matrimony vine seed after the broken wall of step (1) gained is packed in extraction kettle, pass into simultaneously CO
2, be that 28.5Mpa, temperature are that 40.2 ℃, the consumption of entrainment agent ethanol (mass concentration is 95%) the every 100g of matrimony vine seed after by broken wall adds 6.88mL, CO at extraction kettle pressure
2Flow is to extract 70min under the super critical condition of 50L/h, namely gets Boxthorn Seed Oil after two-stage decompression separation, and oil yield is 21.02%.
Wherein: two-stage decompression separation refers to take pressure as 5Mpa, temperature as 40 ℃ as the one-level decompression separation, take pressure as 4Mpa, temperature separates as second depressurized as 30 ℃.
The embodiment 2 quick broken walls of matrimony vine seed cell and seed oil extraction process comprise the following steps:
(1) matrimony vine seed cell wall breaking is processed: after the matrimony vine seed of clean dry is crushed to granularity and is 60 orders, put into extraction kettle; Pass into CO to extraction kettle
2, after at normal temperatures the pressure in extraction kettle being elevated to 45MPa, keep 10min; Then close the air intake valve at extraction kettle two ends, make pressure drop in extraction kettle to normal atmosphere in 5min, obtain the matrimony vine seed after broken wall.
(2) the matrimony vine seed after the broken wall of step (1) gained is packed in extraction kettle, pass into simultaneously CO
2, be that 30.0Mpa, temperature are that 45.0 ℃, the consumption of entrainment agent ethanol (mass concentration is 95%) the every 100g of matrimony vine seed after by broken wall adds 8.45mL, CO at extraction kettle pressure
2Flow is to extract 60min under the super critical condition of 20L/h, namely gets Boxthorn Seed Oil after two-stage decompression separation, and oil yield is 18.8%.
Wherein: two-stage decompression separation refers to take pressure as 7Mpa, temperature as 50 ℃ as the one-level decompression separation, take pressure as 5Mpa, temperature separates as second depressurized as 40 ℃.
The embodiment 3 quick broken walls of matrimony vine seed cell and seed oil extraction process comprise the following steps:
(1) matrimony vine seed cell wall breaking is processed: after the matrimony vine seed of clean dry is crushed to granularity and is 40 orders, put into extraction kettle; Pass into CO to extraction kettle
2, after at normal temperatures the pressure in extraction kettle being elevated to 43MPa, keep 12min; Then close the air intake valve at extraction kettle two ends, make pressure drop in extraction kettle to normal atmosphere in 3min, obtain the matrimony vine seed after broken wall.
(2) the matrimony vine seed after the broken wall of step (1) gained is packed in extraction kettle, pass into simultaneously CO
2, be that 29.0Mpa, temperature are that 42.0 ℃, the consumption of entrainment agent ethanol (mass concentration is 95%) the every 100g of matrimony vine seed after by broken wall adds 7.50mL, CO at extraction kettle pressure
2Flow is to extract 65min under the super critical condition of 35L/h, namely gets Boxthorn Seed Oil after two-stage decompression separation, and oil yield is 19.3%.
Wherein: two-stage decompression separation refers to take pressure as 6Mpa, temperature as 45 ℃ as the one-level decompression separation, take pressure as 4.5Mpa, temperature separates as second depressurized as 35 ℃.
Claims (1)
1. the quick broken wall of matrimony vine seed cell and seed oil extraction process comprises the following steps:
(1) matrimony vine seed cell wall breaking is processed: after the matrimony vine seed of clean dry is crushed to granularity and is 20～60 orders, put into extraction kettle; Pass into CO to extraction kettle
2, after at normal temperatures the pressure in extraction kettle being elevated to 40～45MPa, keep 10～15min; Then close the air intake valve at extraction kettle two ends, make pressure drop in extraction kettle to normal atmosphere in 1～5min, obtain the matrimony vine seed after broken wall;
(2) the matrimony vine seed after the broken wall of described step (1) gained is packed in extraction kettle, pass into simultaneously CO
2, be that 28.5～30.0Mpa, temperature are that 40.2 ℃～45.0 ℃, the consumption of the entrainment agent ethanol every 100g of matrimony vine seed after by broken wall adds 6.88～8.45mL, CO at extraction kettle pressure
2Flow is to extract 60～70min under the super critical condition of 20～50L/h, namely gets Boxthorn Seed Oil after two-stage decompression separation; Described ethanol mass concentration is 95%; Described two-stage decompression separation refers to take pressure as 5～7Mpa, temperature as 40～50 ℃ as the one-level decompression separation, take pressure as 4～5Mpa, temperature separates as second depressurized as 30～40 ℃.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710295A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Wolfberry fruit wall breaking treatment fluid |
Families Citing this family (4)
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|---|---|---|---|---|
| CN103215119B (en) * | 2013-04-19 | 2014-08-20 | 云南绿宝香精香料股份有限公司 | Preposed oil cell disruption process of producing aromatics by cubcritical fluid low-temperature extraction equipment |
| CN103704688B (en) * | 2013-12-13 | 2016-08-24 | 广西科技大学 | A kind of Food-grade natural Lycium seed breaking cellular wall dissociates additive |
| CN103690678B (en) * | 2013-12-13 | 2016-05-18 | 广西科技大学 | A kind of matrimony vine seed broken wall pretreating reagent |
| CN110892988B (en) * | 2019-12-10 | 2023-11-17 | 大连工业大学 | Wall breaking method for acerola cherry |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103710295A (en) * | 2013-12-13 | 2014-04-09 | 广西科技大学 | Wolfberry fruit wall breaking treatment fluid |
| CN103710295B (en) * | 2013-12-13 | 2015-11-11 | 广西科技大学 | A kind of matrimony vine seed broken wall treatment liquid |
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