CN1594520A - Method for supercritical extraction of balsam pear oil using carbon dioxide - Google Patents

Method for supercritical extraction of balsam pear oil using carbon dioxide Download PDF

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Publication number
CN1594520A
CN1594520A CN 200410027723 CN200410027723A CN1594520A CN 1594520 A CN1594520 A CN 1594520A CN 200410027723 CN200410027723 CN 200410027723 CN 200410027723 A CN200410027723 A CN 200410027723A CN 1594520 A CN1594520 A CN 1594520A
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China
Prior art keywords
cylinder
balsam pear
melon seed
bitter melon
extraction
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CN 200410027723
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Chinese (zh)
Inventor
张萍
陈立新
苏菲
郭宁平
李无畏
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BEIHAI ANTAI BIO-TECH Co Ltd
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BEIHAI ANTAI BIO-TECH Co Ltd
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Priority to CN 200410027723 priority Critical patent/CN1594520A/en
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Abstract

The invention discloses a method for supercritical extraction of balsam pear oil using carbon dioxide, which is aimed at solving the problems of solvent recovery and solvent residual for the conventional solvent method employed in balsam pear oil extraction. The method for supercritical extraction of balsam pear oil can be carried out at normal temperature.

Description

Extract the method for balsam pear oil with carbon dioxide upercritical fluid extraction
Technical field
The present invention relates to a kind ofly from plant seed or plant the method for extracting effective components the benevolence, be specifically related to from bitter melon seed, extract the method for balsam pear oil.
Background technology
Balsam pear (monordica charantia L.) has another name called balsam pear, golden lichee, balsam pear etc., is the annual climing property herbaceous plant of Curcurbitaceae Momordica.Originate in India, be distributed widely in the torrid zone, subtropics and area, temperate zone.Ground such as successor's Yunnan Province of China the etc. during Southern Song Dynasty was just eaten by the southerner to Ming Dynasty's middle and later periods morely, still cultivated morely for south China so far, and northern area is progressively cultivated and eaten more widely in recent years.Its meat of balsam pear is tender and crisp, and bitter taste is moderate, be melon in the highest a kind of of Vitamin C content, also have clearing heat and detoxicating, make eye bright, effects such as relieving summer-heat, diuresis, therefore liked by people.Along with balsam pear is revealed gradually in the pharmacological action of aspect such as immune, antitumor, antibiotic, hypoglycemic, people increased day by day to the demand of balsam pear in recent years.For adapting to the needs of market economic development, strengthen research and development to the balsam pear product, people are except studying balsam pear meat, bitter melon seed benevolence has also been carried out more research, because people are except giving over to seed in the past, bitter melon seed all abandons mostly, be not used, very unfortunate.The bitter melon seed purposes is very extensive, and the every fruit of balsam pear contains seed 20-30 grain, seed peltate tawny, and the kind skin is thicker, and therefore bitter melon seed benevolence, caused people's extensive attention to its development and use with nourishing functions such as edible and blood lipid-reducing blood sugar-decreasings.People are to the effect further research again of balsam pear and bitter melon seed benevolence in recent years, and find that bitter melon seed benevolence also has following effect: 1, the activated protein of bitter melon seed benevolence has anticancer propagation and deactivation cancer cells; 2, the effective active composition that contains AIDS virus resisting in the bitter melon seed benevolence, bitter melon seed benevolence have three kinds of albumen mass-energy with physiologically active to stop the synthetic of virus of AIDS DNA, suppress the infection and the growth of virus of AIDS; 3, bitter melon seed benevolence has stronger restraining effect to bacterium, and the antibacterial experiment that the domestic medical college that has carries out with balsam pear extract and seed benevolence proves that gram-positive cocci, gram bacillus, gram negative bacillus are all had anti-microbial effect preferably; 4, bitter melon seed benevolence has the function that adjusting exempts to control, the test that relevant researchist carries out shows, balsam pear Normal juice and balsam pear extract all have obvious enhancement to leukocytic phagocytic activity in the content of the serum coagulation antibody titre of normal mouse, serum lysozyme, the blood, illustrate that bitter melon seed benevolence has comprehensive promotion and regulating effect to normal immune function of mice.
At present bitter melon seed benevolence extraction of active ingredients open source literature there are some reports, as (1), " separation and purification of bitter melon seed ribosome deactivation protein and Study on Antioxidant Activities " [author] Fu Ming brightness Tian Jie, biology department of University Of Shantou, [periodical name] Chinese biochemical drug magazine .2002,23 (3)), [digest] bitter melon seed is through pulverizing, the extracting of 50mmol/L acetate, ammonium sulfate precipitation, after steps such as cationic exchange and gel column chromatography are further purified, measure the physico-chemical property of two kinds of ribosome inactivating proteins of gained, obtaining protein and a kind of small molecular weight protein that a kind of molecular weight is 29.6kD behind the purifying. the ribosome inactivating protein that separation and purification goes out two kinds of different molecular weights from bitter melon seed is sugar-protein, and has certain anti-oxidant activity.(2) biology department of " separation and purification of bitter melon seed ribosome deactivation protein and Study on Antioxidant Activities " [author] Fu Ming brightness Tian Jie [mechanism] University Of Shantou, [periodical name] Chinese biochemical drug magazine .2002,23 (3) .[digests] purpose improves the extraction process of bitter melon seed ribosome deactivation protein, and its anti-oxidant activity studied.The method bitter melon seed is through pulverizing, the extracting of 50mmol/L acetate, ammonium sulfate precipitation, after steps such as cationic exchange and gel column chromatography are further purified, measure the physico-chemical property of two kinds of ribosome inactivating proteins of gained, obtain protein and a kind of small molecular weight protein that a kind of molecular weight is 29.6kD as a result behind the purifying, both suppress 50% protein synthesis concentration and are respectively 4.3 * 10 in acellular system -6, 1.4 * 10 -6Mol/L, sugar degree is respectively 4.83%, 1.82%, and class superoxide-dismutase (SOD) activity is respectively 79.05,17.25u/mg.The pure product SOD activity of positive control is 1267u/mg.The ribosome inactivating protein that conclusion separation and purification from bitter melon seed goes out two kinds of different molecular weights is sugar-protein, and has certain anti-oxidant activity.(3), Chinese patent, application number: 99816804, oil from balsam pear, Preparation Method And The Use (Pushpa Khanna, India New Delhi,), the present invention relates to be suitable for being locally applied to body of mammals and be used as anti-inflammatory, arthritis, a kind of novel oil that extracts from balsam pear of vasodilation and Wound healing agent, described oil mainly comprises capric acid 0.7-1.2 weight %, lauric acid 0.6-1 weight %, palmitinic acid 4.2-5.0 weight %, stearic acid 59-62 weight %, oleic acid 13-15 weight %, ortho acid 3-5 weight %, linolic acid 8-10 weight % and other nd less important sour 6-8 weight %; And the method for producing this oil.The method steps of extract oil is as follows from the balsam pear seed: 1, in the runner milling that is fit to dry seed is worn into fine powder; 2, handle crushed seeds with non-polar solvent mixture; 3, this mixture was at room temperature kept 48 hours so that separate fuel-displaced; 4, adopt separating funnel from clear liquid, to collect oil; 5, with the mixture of non-polar solvent reflux step 4 gained arbitrarily to remove last trace amount; 6, by precipitating this salt and impurity wherein comes purifying oil.Wherein the non-polar solvent of Cai Yonging can comprise acetone and be selected from the aromatic hydrocarbons of benzene, hexane, sherwood oil and ether and the mixture of aliphatic hydrocarbon.(4), the volatile component of balsam pear flesh and seed research, happy growing tall, Fu Honglei, applied chemistry system of East China Institute Of Technology, Fuzhou Shi first hospital, [periodical name] forest chemical engineering communication .2003,37 (3)), use volatile component and relative content thereof that gas-chromatography and mass spectrometry method (GC-MS) are measured balsam pear flesh and seed.Find that the balsam pear flesh has 23 above compositions, has identified 12 compositions wherein; Bitter melon seed has 12 above compositions, has identified 8 compositions wherein, and has determined the relative content of each composition with normalization method.The volatility chemical composition of bitter melon seed still less, content is concentrated relatively, 16 carbonic acid and 16 ethyl-carbonates account for 33.79%, 32.89%, ten eight carbonic acid respectively and 18 ethyl-carbonates account for 4.16%, 6.32% respectively.(5) the proteic separation of bitter melon seed, purifying and Antioxidation Effects (Fu Minghui thereof, biology department of University Of Shantou, medicine biotechnology .2001,8 (5)), bitter melon seed is through pulverizing extracting, ammonium sulfate precipitation, step purifying such as cationic exchange and gel filtration chromatography obtain a kind of albumen, SDS-PAGE and IEF are shown as single band, relative molecular mass 28000, PI8.9-9.0, this albumen quasi-SOD activity is 16.71U/mgpr.(6) Chinese patent<application number〉02134773<denomination of invention Momordi glucose-reducing polypeptide<applicant Beihai Haiyu Agricultural Development Co., Ltd, the 4th buildings, Building 88, Haiyu Community, Haicheng District, Beihai City, Guangxi Zhuang Autonomous Region<digest〉disclosed by the invention be Momordi glucose-reducing polypeptide.It is to utilize bitter melon seed benevolence to be raw material, the activeconstituents that extracts, it prepares with following method: bitter melon seed is shelled, clean then and dry, pulverize, use organic solvent degreasing again, the bitter melon seed benevolence powder vacuum-drying after the degreasing, use alkaline extraction again, this moment, the ratio of powder water was 1 prior to adding pure water in the dry bitter melon seed benevolence powder: 6-10, and adding the adjusting PH with base value is 9.5-9.6, get supernatant liquor after leaving standstill, in supernatant liquor, add acid, and adjust pH is 2.5-3.5, then has precipitation to separate out, obtain throw out after the filtration, throw out cleans with pure water, and crushed after being dried is called in appropriate amount of purified water and lyophilize.The present invention is easily absorbed by human body, but Regular Insulin in the human activin reaches the purpose that reduces blood sugar for human body, and the diabetic subject is had certain function of health care.(7) separation of lipid acid and physiological action research in the bitter melon seed (in Changchun etc., Siping Normal College etc., the distant academic periodical of pine: natural science edition .1995 (2)), take by weighing dry bitter melon seed 80 grams, make solvent with anhydrous diethyl ether, put in 50 ℃ of waters bath with thermostatic control the backflow extracting 48 hours, reclaim ether with the Soxhlet extraction apparatus, promptly get bitter melon seed crude fat, and the physiological action of bitter melon seed crude fat is studied.Contain a large amount of fat in the bitter melon seed, show through experimentation on animals, balsam pear fat has obvious reducing blood lipid, so the research and development bitter melon seed, it is significant therefrom to extract PUFA.The separation of lipid acid and physiological action research in the bitter melon seed (in Changchun etc., Siping Normal College etc., the distant academic periodical of pine: natural science edition .1995 (2)), take by weighing dry bitter melon seed 80 grams, make solvent with anhydrous diethyl ether, put in 50 ℃ of waters bath with thermostatic control the backflow extracting 48 hours, reclaim ether with the Soxhlet extraction apparatus, promptly get bitter melon seed crude fat, and the physiological action of bitter melon seed crude fat is studied.Contain a large amount of fat in the bitter melon seed, show through experimentation on animals, balsam pear fat has obvious reducing blood lipid, so the research and development bitter melon seed, it is significant therefrom to extract PUFA.
From above-mentioned disclosed document, recognize, extracting balsam pear oil at present from bitter melon seed all is to adopt solvent method (comprising the aromatic hydrocarbons of acetone, hexanaphthene, hexane, acetate, sherwood oil and ether or the mixture of aliphatic hydrocrbon etc.) usually, this method exists solvent recuperation and product to have the dissolvent residual problem, the leaching process that has is complicated, and oily yield is lower.
Summary of the invention
The inventor has invented a kind of the needs with the method for organic solvent from balsam pear seed extraction balsam pear oil through research and exploration, the balsam pear oil recovery rate height that this method is extracted, and the noresidue solvent, technological process is simple.
Technical scheme of the present invention is as follows:
Balsam pear oil of the present invention extracts from bitter melon seed with carbon dioxide supercritical extraction method, and extracting method comprises the steps:
1, with bitter melon seed shelling, shell and stay benevolence, bitter melon seed benevolence is cleaned dry then, after crushed clean bitter melon seed benevolence powder;
2, set the temperature of extraction cylinder, two splitter cylinder (I, II);
3, the barrel that a certain amount of bitter melon seed benevolence powder will be housed is put into the extraction cylinder;
4, start the carbonic acid gas recycle system, regulate the pressure of extraction cylinder, two splitter cylinder (I, II);
When 5, the temperature of cylinder to be extracted, splitter cylinder (I, II) and pressure reach set(ting)value, the opening entry time;
6, regularly emit balsam pear oil from the splitter cylinder drain hole, weighing, record;
7, separate that bitter melon seed benevolence powder that balsam pear oil obtains later on can be further used for preparing bitter gourd polypeptide or as protein powder.
The above-described method of extracting balsam pear oil with carbon dioxide supercritical extraction method, in the temperature course of setting extraction cylinder and two splitter cylinder, the temperature of extraction cylinder is 32 ℃~40 ℃, and the temperature of splitter cylinder I is 50 ℃~55 ℃, and the temperature of splitter cylinder II is 40 ℃~45 ℃.
The above-described method of extracting balsam pear oil with carbon dioxide supercritical extraction method, in the pressure of regulating extraction cylinder, two splitter cylinder (I, II), the pressure of extraction is 35MPa~40MPa, and splitter cylinder I pressure is 5.0MPa~6.0MPa, and splitter cylinder II pressure is 4.0MPa~5.0MPa.
Above-described method with carbon dioxide supercritical extraction method extraction balsam pear oil, the time of extraction is 6-16 hour.
Balsam pear of the present invention oil purposes: promoting blood circulation and removing blood stasis, the anti-inflammatory analgetic of the property of medicine is used for the myalgia and the Wound healing agent of sacroiliitis, rheumatoid arthritis, spondylitis, diabetic subject's leg and hand.Also can be used as the pharmaceutical industry raw material, perhaps the raw material of daily-use chemical industry, foodstuff additive.
Extract the method for balsam pear oil compares with existing solvent method, outstanding substantive distinguishing features of the present invention and obvious improvement are: extracting balsam pear oil with carbon dioxide supercritical extraction method can carry out at normal temperatures, and carbonic acid gas is nontoxic, noresidue, the source of the gas steady sources can be recycled, and extraction process is simple, the extraction efficiency height, do not need through complicated loaded down with trivial details leaching process, the cost of suitability for industrialized production is low, implements easily.
Embodiment
Embodiment 1: gets an amount of dry bitter melon seed, the bitter melon seed shell sloughed, get Semen Momordicae Charantiae benevolence with peeler, and decon, cleaning, normal temperature is dry down, pulverizes, and obtains greater than 40 purpose Semen Momordicae Charantiae powder.Connect the supercritical extraction device power supply (DPS), open cold cycling switch and heater switch, the temperature of setting the extraction cylinder is 32 ℃, the temperature of splitter cylinder I is 50 ℃, the temperature of splitter cylinder II is 40 ℃, pour the Semen Momordicae Charantiae powder of having pulverized into barrel and put into the extraction cylinder, start the carbonic acid gas recycle system, the pressure of regulating the extraction cylinder is 35MPa, and the pressure of splitter cylinder I is 5.5MPa, and the pressure of splitter cylinder II is 4.0MPa, cylinder to be extracted, splitter cylinder (I, when temperature II) and pressure reach set(ting)value, pick up counting, balsam pear oil promptly can separate from splitter cylinder I, again material and carbonic acid gas is imported splitter cylinder II, every interval one hour emits balsam pear oil once from the splitter cylinder drain hole, carbonic acid gas recycles, and through 6 hours extraction, percentage extraction reached 96%.
Embodiment 2: gets an amount of dry bitter melon seed, the bitter melon seed shell sloughed, get Semen Momordicae Charantiae benevolence, and decon, cleaning, normal temperature is dry down, at freezing and pulverizing below 30 ℃, obtains greater than 40 purpose Semen Momordicae Charantiae powder.Connect the supercritical extraction device power supply (DPS), open cold cycling switch and heater switch, the temperature of setting the extraction cylinder is 36 ℃, the temperature of splitter cylinder I is 55 ℃, the temperature of splitter cylinder II is 45 ℃, pour the Semen Momordicae Charantiae powder of having pulverized into barrel and put into the extraction cylinder, start the carbonic acid gas recycle system, the pressure of regulating the extraction cylinder is 38MPa, and the pressure of splitter cylinder I is 5.0MPa, and the pressure of splitter cylinder II is 5.0MPa, cylinder to be extracted, splitter cylinder (I, when temperature II) and pressure reach set(ting)value, pick up counting, balsam pear oil promptly can separate from splitter cylinder I, again material and carbonic acid gas is imported splitter cylinder II, every interval one hour emits balsam pear oil once from the splitter cylinder drain hole, carbonic acid gas recycles, and through 10 hours extraction, percentage extraction reached more than 98.5%.
Embodiment 3: gets an amount of dry bitter melon seed, the bitter melon seed shell sloughed, get Semen Momordicae Charantiae benevolence, and decon, cleaning, normal temperature is dry down, at freezing and pulverizing below 30 ℃, obtains greater than 40 purpose Semen Momordicae Charantiae powder.Connect the supercritical extraction device power supply (DPS), open cold cycling switch and heater switch, the temperature of setting the extraction cylinder is 40 ℃, the temperature of splitter cylinder I is 53 ℃, the temperature of splitter cylinder II is 42 ℃, pour the Semen Momordicae Charantiae powder of having pulverized into barrel and put into the extraction cylinder, start the carbonic acid gas recycle system, the pressure of regulating the extraction cylinder is 40MPa, and the pressure of splitter cylinder I is 6.0MPa, and the pressure of splitter cylinder II is 4.5MPa, cylinder to be extracted, splitter cylinder (I, when temperature II) and pressure reach set(ting)value, pick up counting, balsam pear oil promptly can separate from splitter cylinder I, again material and carbonic acid gas is imported splitter cylinder II, every interval one hour emits balsam pear oil once from the splitter cylinder drain hole, carbonic acid gas recycles, and through 16 hours extraction, percentage extraction reached more than 98.7%.

Claims (4)

1, a kind of method of extracting balsam pear oil from bitter melon seed is characterized in that: described balsam pear oil extracts and extracts from bitter melon seed with carbon dioxide supercritical extraction method, and extracting method comprises the steps:
(1) with bitter melon seed shelling, shell and stay benevolence, bitter melon seed benevolence is cleaned dry then, after crushed clean bitter melon seed benevolence powder;
(2) set the temperature that extracts cylinder, two splitter cylinder (I, II);
(3) barrel that a certain amount of bitter melon seed benevolence powder will be housed is put into the extraction cylinder;
(4) start the carbonic acid gas recycle system, regulate the pressure of extraction cylinder, two splitter cylinder (I, II);
When (5) temperature of cylinder to be extracted, splitter cylinder (I, II) and pressure reach set(ting)value, the opening entry time;
(6) regularly emit balsam pear oil from the splitter cylinder drain hole, weighing, record;
In the temperature course of above-described setting extraction cylinder and two splitter cylinder, the temperature of extraction cylinder is 32 ℃~40 ℃, and the temperature of splitter cylinder I is 50 ℃~55 ℃, and the temperature of splitter cylinder II is 40 ℃~45 ℃;
Above-described the pressure of extraction is 35MPa~40MPa in the pressure of regulating extraction cylinder, two splitter cylinder (I, II), and splitter cylinder I pressure is 5.0MPa~6.0MaP, and splitter cylinder II pressure is 4.0MPa~5.0MPa.
2, the method for extracting balsam pear oil from bitter melon seed according to claim 1, it is characterized in that: the time of carbon dioxide upercritical fluid extraction is 6-12 hour.
3, the method for extracting balsam pear oil from bitter melon seed according to claim 1 is characterized in that: separate that bitter melon seed benevolence powder that balsam pear oil obtains later on is further used for preparing bitter gourd polypeptide or as protein powder.
4, the purposes of balsam pear oil as claimed in claim 1, it is characterized in that myalgia and the Wound healing agent of balsam pear oil, perhaps as the application of industrial raw material at promoting blood circulation and removing blood stasis or anti-inflammatory analgetic, sacroiliitis, rheumatoid arthritis, spondylitis, diabetic subject's leg and hand.
CN 200410027723 2004-06-22 2004-06-22 Method for supercritical extraction of balsam pear oil using carbon dioxide Pending CN1594520A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103436354A (en) * 2013-09-11 2013-12-11 江苏丘陵地区镇江农业科学研究所 Method for extracting Trichosanthes kirilowii Maxim seed oil
CN104605136A (en) * 2015-02-02 2015-05-13 王�锋 Preparation method of balsam pear polypeptide
CN105132146A (en) * 2015-09-24 2015-12-09 全椒县尹氏油脂有限公司 Extraction method of bitter melon seed oil
CN105434502A (en) * 2015-12-07 2016-03-30 安徽理工大学 External washing medicine for treating children's prickly heat and preparation method thereof
CN105623844A (en) * 2016-03-23 2016-06-01 深圳市先康达生物科技有限公司 Balsam pear seed oil, extraction method therefor and application thereof
CN106692258A (en) * 2016-12-21 2017-05-24 陈绍良 Medical application of bitter guard and bitter guard extract
CN109699756A (en) * 2017-02-02 2019-05-03 中创寰宇生物科技有限责任公司 Use of balsam pear seed oil for producing a composition for simulating sports effects

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103436354A (en) * 2013-09-11 2013-12-11 江苏丘陵地区镇江农业科学研究所 Method for extracting Trichosanthes kirilowii Maxim seed oil
CN104605136A (en) * 2015-02-02 2015-05-13 王�锋 Preparation method of balsam pear polypeptide
CN105132146A (en) * 2015-09-24 2015-12-09 全椒县尹氏油脂有限公司 Extraction method of bitter melon seed oil
CN105434502A (en) * 2015-12-07 2016-03-30 安徽理工大学 External washing medicine for treating children's prickly heat and preparation method thereof
CN105434502B (en) * 2015-12-07 2019-08-06 安徽理工大学 A kind of Wash-out medicine and preparation method thereof for treating children's prickly heat
CN105623844A (en) * 2016-03-23 2016-06-01 深圳市先康达生物科技有限公司 Balsam pear seed oil, extraction method therefor and application thereof
CN106692258A (en) * 2016-12-21 2017-05-24 陈绍良 Medical application of bitter guard and bitter guard extract
CN109699756A (en) * 2017-02-02 2019-05-03 中创寰宇生物科技有限责任公司 Use of balsam pear seed oil for producing a composition for simulating sports effects

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