CN103416733A - Glucosinolate extract from fresh broccoli and preparation method thereof - Google Patents
Glucosinolate extract from fresh broccoli and preparation method thereof Download PDFInfo
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- CN103416733A CN103416733A CN2012101632122A CN201210163212A CN103416733A CN 103416733 A CN103416733 A CN 103416733A CN 2012101632122 A CN2012101632122 A CN 2012101632122A CN 201210163212 A CN201210163212 A CN 201210163212A CN 103416733 A CN103416733 A CN 103416733A
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Abstract
A glucosinolate extract from fresh broccoli and a preparation method thereof relate to the technical field of extraction techniques of natural products. The preparation method comprises the following steps: 1. raw material processing; 2. enzyme killing; 3. extraction; and 4. drying. The method has the following beneficial effects: (1) no toxic solvent is involved in the extraction, and thus reliable and safe conditions are provided for production of health-care products; (2) a product with a higher concentration of glucosinolates can be extracted from fresh broccoli; and (3) extraction equipment is simple, and there is no need for large improvement on techniques in the prior art, and thus the method is easy to implement with small investment.
Description
Technical field:
The invention belongs to the extraction process technology field of natural products, relate to thioglucose glucoside extract of a kind of fresh broccoli and preparation method thereof.
Background technology:
Glucosinolate (Glucosinolates is called for short GLS) is a kind of sulfur-bearing secondary metabolite, and it extensively is present in 15 kinds of dicotyledons.Wherein the glucosinolate content of Cruciferae (Cruciferous) plant is very abundant, and active anticancer is also large especially, is noted widely.Up to the present, had been found that more than 120 kind of glucosinolate.Although Brassica plants institute all exists glucosinolate in a organized way, some plant variety contains glucosinolates different in 15, only contains a few glucosinolate in most plants, and content is not too high.Although the broccoli total sulfur is not the highest for glucoside, its active large glucosinolate content is very high.The glucosinolate contained be take Glucoraphanin (Glucoraphanin) and 3-methylsulfinyl acrylic glucosinolate (Glucoiberin) as main; its catabolite isothiocyanate; mainly with Sulforaphane, be commonly called as (sulforaphen) and Iberin; Erucin is main, and what wherein content was the highest is sulforaphen.Sulforaphen can improve body immunity.Sulforaphen is a kind of multi-functional inducer, can induce body to produce II type detoxication enzyme-glutathione transferase and quinone reductase, and this enzyme can produce removing toxic substances to many carcinogenic substances, thereby plays protective effect on cancer risk.In broccoli, glucosinolate eats after can being degraded into isothiocyanate, also can directly eat.But sulforaphen is very unstable, therefore there is no so far the consumable products of sulforaphen.And Glucoraphanin stability is relatively good, it under microbial action, changes into sulforaphen in people's intestines, and is absorbed by the body, thereby plays function.The U.S. and Taiwan have been developed and take enhancing immunity and the cancer-resisting health food that Glucoraphanin is the major function composition.At present a lot of enterprises all carry out broccoli concentrated powder production, but the product of its production is extremely low containing Glucoraphanin glucosinolate concentration.Thereby be vital so explore the Glucoraphanin glucosinolate that a kind of effective extraction process obtains the broccoli of more amount.
Brassicaceous vegetable used in everyday is all cooking.On high pressure, steam, microwave and four kinds of method for cooking of low pressure, on the broccoli glucosinolate content, impact is studied F.Vallejo etc., find that microwave boiling meeting makes glucosinolate total content loss 74%, the steam boiling is minimum on the glucosinolate content impact.The report crucifers such as S.A.McNaughton were after boiling, and the content of glucosinolate has reduced 18.0%-59.2%, and average loss rate has reached 36%.Broccoliflorets is through the poach of 9-15min, and the loss range of thioglucose after culinary art is 17%-64%.And, through the Broccoliflorets of Microwave Treatment, the final loss of its glucosinolate is 27%-48%.After culinary art, the content of the isothiocyanate in crucifer is very low.First minute of starting of culinary art has the greatest impact to glucosinolate content, and in this minute, glucosinolate content has reduced 35%, and 5 minutes glucosinolate contents subsequently reduce 10%-15%.Therefore adopt and extract the utilization ratio that concentration technique can improve glucosinolate in broccoli.Can utilize leaf and the stem of original not edible broccoli to extract glucosinolate simultaneously.
Glucosinolate can dissolve in most of organic solvents, the commonly used ethanol that comprises, and n-butanols etc. simultaneously, also can reach very high solubility in water.According to the literature, the poor solubility of glucosinolate in organic solvent and water is apart from also little.Broccoli concentrated powder, generally adopt water extraction to get at present.Although glucosinolate is dissolved in water, can use in theory water extraction to get.But in fact, because in broccoli, myrosin is arranged, in leaching process, glucosinolate decomposes in a large number.Its catabolite is unstable again, therefore finally can't obtain the function product needed.Even the employing heating is gone out, after enzyme, water extracts, and the yield of glucosinolate is also very low.Also useful alcoholic extraction on producing at present, but technical not passing a test, same glucosinolate yield is very low.We collect 8 broccoli concentrated powders that other enterprise produces, and its Glucoraphanin glucosinolate content is all below 0.02%.Our research finds that the myrosin vigor in broccoli is very strong, can be in 5-10 minute, most of glucosinolate degraded.Therefore, the key that glucosinolate extracts will, when going out enzyme, can not make the glucosinolate degraded.
Summary of the invention:
The purpose of this invention is to provide thioglucose glucoside extract of a kind of fresh broccoli and preparation method thereof, its leaching process, containing poisonous solvent, does not provide reliable security for making health product; Can from fresh broccoli, extract the glucosinolate of high level; Extraction equipment is simple, does not need current technology is carried out to large improvement, and small investment is easily implemented.
In order to solve the existing problem of background technology, the present invention is by the following technical solutions: its preparation method is: 1, raw material is processed; 2, the enzyme that goes out is processed: bright broccoli (flower, stalk or tender leaf) is cut into small pieces (1-2 millimeter)----press M
Sample/ V
AlcoholAdd 95% alcohol at=1: 1, processes 20 minutes for 70 ℃; 3, extraction process: sample after the enzyme that goes out----cold filtration, collection alcohol filtrate----solid is pressed M
Sample/ V
WaterAdd water at=1: 1---processing 20 minutes for 70 ℃---, and-cold filtration ,-slag is pressed M to collection filter liquor---solid making beating---
Sample/ V
WaterAdd water at=1: 1---70 ℃ process 20 minutes----cold filtration,---slag water again repeats to extract 2 times---collects and merges aqueous extract that---Vacuum Concentration adds alcohol filtrate to original volume 1/3----, and---Vacuum Concentration is to paste, and---a small amount of ethanol of Jia (with 95% ethanol raw material weight 10% quite originally) dissolves 10 minutes---liquid vacuum is concentrated into paste----crude extracts to collect filter liquor; 4, the dry processing: crude extract----use concentrate weight 4-7 water-soluble solution doubly, spray-drying (or freeze drying).
The present invention has following beneficial effect: (1) leaching process, containing poisonous solvent, does not provide reliable security for making health product; (2) can from fresh broccoli, extract the glucosinolate of high level; (3) extraction equipment is simple, does not need current technology is carried out to large improvement, and small investment is easily implemented.
The specific embodiment:
This specific embodiment is by the following technical solutions: its preparation method is: the enzyme that 1, goes out is processed: bright broccoli (flower, stalk or tender leaf) is cut into small pieces (1-2 millimeter)----press M
Sample/
V alcoholAdd 95% alcohol at=1: 1, processes 20 minutes for 70 ℃; 2, extraction process: sample after the enzyme that goes out----cold filtration, collection alcohol filtrate----solid is pressed M
Sample/ V
WaterAdd water at=1: 1---processing 20 minutes for 70 ℃---, and-cold filtration ,-slag is pressed M to collection filter liquor---solid making beating---
Sample/ V
WaterAdd water at=1: 1---70 ℃ process 20 minutes----cold filtration,---slag water again repeats to extract 2 times---collects and merges aqueous extract that---Vacuum Concentration adds alcohol filtrate to original volume 1/3----, and---Vacuum Concentration is to paste, and---a small amount of ethanol of Jia (with 95% ethanol raw material weight 10% quite originally) dissolves 10 minutes---liquid vacuum is concentrated into paste----crude extracts to collect filter liquor; 3, the dry processing: crude extract----use concentrate weight 4-7 water-soluble solution doubly, spray-drying (or freeze drying); (5) draw product.
Example 1, the concentrated powder preparation of broccoli vegetables
(1) raw material is processed
1000 kilograms of broccoli, reject rotten cauliflower.Select, handle with care while pruning, every basket of (or basket) unsuitable overfill, prevent from weighing wounded or crushing.Silt is removed in cleaning.Water for cleaning need keep clean, and uses circulating water to clean raw material.
(2) enzyme that goes out is processed:
Shredding machine is cut into the thickness of 1-2 millimeter.The cauliflower of chopping enters the 4000L extractor, adds 1000 liter of 95% ethanol (liter), and sealing is opened steam and is warming up to 70 ℃ of insulations 20 minutes.
(3) extraction process:
With pump, feed liquid is input into to filter from extractor, Separation of Solid and Liquid, extract enters extractor No. 2.Extractor adds 1000 liters, water, and sealing is opened steam and is warming up to 70 ℃ of insulations 20 minutes.Separation of Solid and Liquid, extract enters tank No. 3.Solid is sent beater to by conveyer belt, with the broken cauliflower cell of beater.The cauliflower of having pulled an oar enters extractor.Extractor adds 1000 liters, water, and sealing is opened steam and is warming up to 70 ℃ of insulations 20 minutes.Separation of Solid and Liquid, extract enters tank No. 3.Same extracting in water 2 times.Merging repeatedly aqueous extract is input into vacuum concentration equipment and is concentrated.55 ℃ of Vacuum Concentrations.While being concentrated into original volume 1/3, the input alcohol enzyme liquid that goes out.45 ℃ of Vacuum Concentrations.Concentrate and recovered alcohol.Concentrate requires moisture to control 70% left and right.The concentrated end, check concentrate PH, if pH is too low, concentrate enters blend tank, adjusts pH=6.6.Add 100 liter of 95% ethanol and dissolve 10 minutes, obtain liquid, then Vacuum Concentration is waited until crude extract to paste.
(4) the dry processing:
Adopt spray-drying, require feed temperature≤105 ℃, outlet material temperature≤65 ℃.Dried material is cooled to room temperature in aseptic, dehumidifying workshop.At once with high-barrier moisture package encapsulation.
(5) product
Glucosinolate content accounts for the 2.4%-2.8% of product weight.100 kilograms of fresh feeds can obtain 2.9 kilograms of products.
Claims (1)
1. thioglucose glucoside extract of a fresh broccoli and preparation method thereof, is characterized in that its preparation method is: 1, raw material processing; 2, the enzyme that goes out is processed: bright broccoli stalk, the tender leaf 1-2 millimeter that is cut into small pieces----press M
Sample/ V
AlcoholAdd 95% alcohol at=1: 1, processes 20 minutes for 70 ℃; 3, extraction process: sample after the enzyme that goes out----cold filtration, collection alcohol filtrate----solid is pressed M
Sample/ V
WaterAdd water at=1: 1---processing 20 minutes for 70 ℃---, and-cold filtration ,-slag is pressed M to collection filter liquor---solid making beating---
Sample/ V
WaterAdd water at=1: 1---70 ℃ process 20 minutes----cold filtration,---slag water again repeats to extract 2 times---collects and merges aqueous extract that---Vacuum Concentration adds alcohol filtrate to original volume 1/3----, and---Vacuum Concentration is to paste, and---a small amount of ethanol of Jia (with 95% ethanol raw material weight 10% quite originally) dissolves 10 minutes---liquid vacuum is concentrated into paste----crude extracts to collect filter liquor; 4, the dry processing: crude extract----use concentrate weight 4-7 water-soluble solution, spray-drying or freeze drying doubly.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103740527A (en) * | 2013-12-27 | 2014-04-23 | 彭聪 | Brewing method of broccoli wine |
| CN105017343A (en) * | 2015-07-13 | 2015-11-04 | 长江师范学院 | Extraction method of tumorous stem mustard glucosinolate, method for degrading tumorous stem mustard glucosinolate into isothiocyanate, and functional food |
| CN110122738A (en) * | 2019-06-12 | 2019-08-16 | 合肥工业大学 | A kind of high sulforaphen content broccoli and preparation method and application |
| CN110638011A (en) * | 2019-11-05 | 2020-01-03 | 严钦武 | Pickling method of leaf mustard |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10308298A1 (en) * | 2003-02-26 | 2004-09-09 | Kullmer, Thomas, Priv. Doz. Dr. med. | Production of a plant preparation useful for treating cancer comprises extracting glucosinolates from plant material and enzymatically hydrolyzing the glucosinolates to isothiocyanates |
| US20080131578A1 (en) * | 2006-10-27 | 2008-06-05 | Caudill Seed and Warehouse Company, Inc. | Food or drink products, supplements or additives produced from high glucoraphanin-containing broccoli variety 'hopkins' |
| US20080311276A1 (en) * | 2007-06-12 | 2008-12-18 | Kraft Foods Holdings, Inc. | Production of Glucosinolates from Agricultural By-Products & Waste |
| CN101548760A (en) * | 2009-04-22 | 2009-10-07 | 宁波海逸生物科技有限公司 | Technique for preparing glucoraphanin-riched broccoli concentrated powder |
| CN102295667A (en) * | 2011-06-28 | 2011-12-28 | 浙江省农业科学院 | Method for extracting glucoraphanin compound from broccoli and cauliflower |
-
2012
- 2012-05-24 CN CN2012101632122A patent/CN103416733A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE10308298A1 (en) * | 2003-02-26 | 2004-09-09 | Kullmer, Thomas, Priv. Doz. Dr. med. | Production of a plant preparation useful for treating cancer comprises extracting glucosinolates from plant material and enzymatically hydrolyzing the glucosinolates to isothiocyanates |
| US20080131578A1 (en) * | 2006-10-27 | 2008-06-05 | Caudill Seed and Warehouse Company, Inc. | Food or drink products, supplements or additives produced from high glucoraphanin-containing broccoli variety 'hopkins' |
| US20080311276A1 (en) * | 2007-06-12 | 2008-12-18 | Kraft Foods Holdings, Inc. | Production of Glucosinolates from Agricultural By-Products & Waste |
| CN101548760A (en) * | 2009-04-22 | 2009-10-07 | 宁波海逸生物科技有限公司 | Technique for preparing glucoraphanin-riched broccoli concentrated powder |
| CN102295667A (en) * | 2011-06-28 | 2011-12-28 | 浙江省农业科学院 | Method for extracting glucoraphanin compound from broccoli and cauliflower |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103740527A (en) * | 2013-12-27 | 2014-04-23 | 彭聪 | Brewing method of broccoli wine |
| CN105017343A (en) * | 2015-07-13 | 2015-11-04 | 长江师范学院 | Extraction method of tumorous stem mustard glucosinolate, method for degrading tumorous stem mustard glucosinolate into isothiocyanate, and functional food |
| CN105017343B (en) * | 2015-07-13 | 2018-01-09 | 长江师范学院 | A kind of extracting method of tumorous stem mustard glucosinolate, the method and functional food that it is isothiocyanate of degrading |
| CN110122738A (en) * | 2019-06-12 | 2019-08-16 | 合肥工业大学 | A kind of high sulforaphen content broccoli and preparation method and application |
| CN110638011A (en) * | 2019-11-05 | 2020-01-03 | 严钦武 | Pickling method of leaf mustard |
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Application publication date: 20131204 |