CN1079871A - The extracting method of low ester pectin from sunflower - Google Patents
The extracting method of low ester pectin from sunflower Download PDFInfo
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- CN1079871A CN1079871A CN93106836A CN93106836A CN1079871A CN 1079871 A CN1079871 A CN 1079871A CN 93106836 A CN93106836 A CN 93106836A CN 93106836 A CN93106836 A CN 93106836A CN 1079871 A CN1079871 A CN 1079871A
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Abstract
The extracting method of low ester pectin from sunflower is a raw material with sunflower plate and stalk, and overall process comprises raw material pulverizing, decolorization of hot water containing soda, inorganic acid decalcification, pectin hot water extracting and 5 key steps of pectin alcohol precipitating.Whole indexs of the pectin product that obtains all meet U.S. FCC standard (food sanitation standard), and obviously are better than prior art.Adopt the inventive method to extract the recovery rate height of low-ester pectin, reach (is benchmark with the raw material dry weight) more than 9%, than prior art high approximately 50%.
Description
The present invention relates to extracting pectin, relate to the method for from the floral disc of sunflower and bar, extracting low-ester pectin or rather.
Pectin is widely used in fields such as food, medicine and cosmetics.In these fields, pectin is often used as gelling agent, thickener, stabilizing agent and emulsifying agent etc.
Up to now, the pectin great majority all are to extract in the waste residue by the skin of citrus and apple processing.In these raw materials, the major part of pectin all is that the form with free high-ester pectin exists, and this pectin is soluble in water, therefore extracts easily, and technology and equipment needed thereby are all fairly simple.But high-ester pectin is crossed sweet and peracid on mouthfeel, can not be fit to a lot of people's taste when therefore using in food industry.There is the people high-ester pectin to be changed into low-ester pectin (semi-synthetic low-ester pectin) in recent years by amidation.Cross the shortcoming of sweet and peracid and improved mouthfeel though the food that uses this class low-ester pectin to make has overcome, but because amidation brought some harmful substances into, so it does not just resemble the natural low-ester pectin (for example low ester pectin from sunflower) welcome.In addition, the production cost of this semi-synthetic low-ester pectin is also quite high.
Contain relatively large low-ester pectin in the sunflower, but it mainly is to exist with water-fast calcium salt (protoplasm pectin) form, therefore is difficult to extract.As far back as the seventies, people such as Canadian M.J.Y.Lin just extract low ester pectin from sunflower [M.J.Y.Lin et al.Extration of pectins from sunflower heads from the floral disc of sunflower and straw, J.Can. Inst. Food Sci.Technol., Vol.9, No.2 p70(1976)].Its process characteristic is to make chelating agent with calgon, makes the pectin calcium salt that is present in the sunflower plant change into water soluble pectin, thereby pectin is extracted.Because in the purification step of this technology, residual hexametaphosphate is difficult for being cleaned by alcohol, causes ash content in the pectin product up to 14%, has surpassed the numerical value (＜10%) of international standard regulation, and the color of this product is dark excessively, so this technology does not realize suitability for industrialized production.
1985, Shanghai Institute of Food has proposed a about extract the application (CN85106947A) of the method for low-ester pectin from sunflower, the main feature of this method is to use the hydrochloric acid decalcification at normal temperatures and pressures, makes the pectin calcium salt be transformed into pectin soluble in water.Because the accessory substance calcium chloride of decalcification easily by flush away, has therefore overcome the too high shortcoming of product ash content in the alcohol washing step.Its technical process is as follows:
1, raw material pulverizing: sunflower plate and bar are pulverized into about 60 purpose powder;
2, decolouring: add water and alkali in the raw material after pulverizing, the alkali solubility pigment in the raw material is dissolved out;
3, decalcification: add water and hydrochloric acid in the filter residue after decolouring, make calcium in the pectin calcium salt be transformed into calcium chloride and be dissolved out and therefore make water-fast protoplasm pectin to be transformed into pectin in soluble in water and the alkaline solution;
4, pectin extracts: add the water that is equivalent to 20 times of raw material weights approximately in the filter residue after decalcification, with alkali the pH value is transferred to 3.5-5 then, make pectolysis in water;
5, flocculation: utilize pectin to be insoluble to character in the acid stronger solution, in the pectin aqueous solution that extracts, add the concentrated hydrochloric acid that is equivalent to raw material weight 30-40%, make pectin be condensed into bulk, carry out Separation of Solid and Liquid then;
6, purify: utilize pectin to be insoluble to alcohol, its impurity (for example calcium chloride and fat-soluble pigment) then is dissolved in the character of alcohol, fully washs with alcohol;
7, oven dry: vacuum drying under about 60 ℃ condition;
8, pulverize and pack.
Though above technology has solved the too much problem of ash content, because overall process all is to carry out under the condition of normal temperature, so decalcification and pectin extract all incomplete.According to our test to this flow process, its recovery rate generally has only 4-6%(weight, press the raw material dry weight basis, down together), and because the flocculation step of this flow process adopts hydrochloric acid to make flocculant, the pectin grumeleuse of Xing Chenging is not easy to smash like this, and therefore the inside of blob of viscose can not get abundant washing when purifying, some impurity and fat-soluble pigment are still stayed the inside of gel piece, so the color of product is darker.Because above-mentioned shortcoming, cause this technology also to fail to realize industrialization.
The purpose of this invention is to provide a kind of above-mentioned shortcoming that do not exist, can be for the method for suitability for industrialized production, and this method should be able to reach low-ester pectin recovery rate height, decolouring fully and the quality of low-ester pectin reach the target of international edible and standards of pharmacopoeia comprehensively.
For achieving the above object, we have done following a series of research work.
1, decolouring step
We carry out Decolorant Test with hot water, room temperature buck and thermokalite water respectively.In these Decolorant Test, raw material is all＜the 2.25mm(60 order) sunflower plate and powder 100 gram of bar, the consumption of water is all 1500 grams (be equivalent to raw material weight 15 times), bleaching time is all 30 minutes (stirring).Result of the test is as follows:
(1) hot water decolouring:
Use ordinary tap water, 80 ℃ of water temperatures are filtered water and raw material stirring after 30 minutes, the filtrate thickness, and its pH value is 3.4, the color of filter residue is quite dark.As seen the effect of hot water decolouring is bad, and its reason mainly is that the natural colouring matter of sunflower is insoluble in the acidic aqueous solution.
(2) room temperature alkaline bleaching:
Material quantity is identical with hot water Decolorant Test (1) with water consumption, but water temperature is room temperature (about 25 ℃), adds 3 gram soda ash in addition, stir after 30 minutes and filter, filtrate is than thickness, and its pH value is about 8, the color of filter residue is still darker, and is still more obvious through the color of 2 washing rear filtrates.The effect of this explanation room temperature alkaline bleaching is still undesirable.
(3) decolorization of hot water containing soda:
Except water temperature is 70 ℃, other conditions are identical with room temperature alkaline bleaching test (2), filter the rear filtrate thickness, and its pH value is about 7.PH value of filtrate is transferred to 4 when following, and the precipitation capacity of the natural colouring matter obviously precipitation capacity than two experiments in front is many, and particularly the color of filter residue is much more of light color than the filter residue of preceding two experiments.After twice washing, the color of filtrate is very shallow.
From the data of above three experiments as can be seen, the decolorizing effect of thermokalite water is best.Pass through a large amount of tests afterwards again, further proved above-mentioned conclusion.And, lot of experiment results shows, the temperature of destainer and pH value all are crucial conditions, as long as the temperature of destainer is more than 50 ℃, the final pH value can obtain obviously to be better than the effect of prior art more than 6, but temperature should not be above 90 ℃, the final pH value should not surpass 8.5, otherwise pectin is had adverse effect.That is to say that the preference temperature during decolouring is 50 °-90 ℃, be preferably 60 °-80 ℃, suitable final pH value is 6-8.5, is preferably 6.5-7.5.As for the kind of alkali, do not have strict restriction, but it generally is an inorganic base, for example it can be Na
2CO
3, K
2CO
3, NaOH, KOH etc., wherein be preferably Na
2CO
3The use amount of alkali does not have strict restriction yet, and this will depend on the kind of alkali, the consumption of water and the source of raw material, and the consumption of general alkali is with the 2-5%(weight of raw material) be advisable, can add 3%(weight earlier usually) Na
2CO
3If the pH value is reduced to below 6 gradually in decolorization, then should replenish an amount of alkali so that pH remains on 6-8.5, is preferably 6.5-7.5.
2, decalcification step
Decalcification is not critical step in technological process of the present invention, and result of the test shows that the decalcification step can be used inorganic acids such as hydrochloric acid, sulfuric acid, also can use acetic acid, but preferably use hydrochloric acid.The concentration of acid is answered 0.1N at least, and to guarantee that calcium can fully dissolve, generally the concentration with acid is that 0.1N to 3N is advisable.Certainly, acidity higher again (for example 5N) also is fine.In addition, we find, if the temperature during with decalcification suitably improves, can obtain better effect, but should not carry temperature too high under strong acid condition, otherwise can play destruction to pectin, and the degree of gelation of product is reduced.Generally ℃ be advisable, be preferably 35 °-40 ℃ with room temperature to 45.Decalcification time should be greater than 20 minutes, and is preferable with 20-30 minute.
3, pectin extraction step
It is one of critical step that pectin extracts, and it directly influences the recovery rate of pectin.We extract pectin according to the technology of CN85106947A, promptly at room temperature extract with sodium carbonate liquor, and the pH value of extract is about 4.5, and the result shows that the highest of the recovery rate of pectin reaches 6%(weight, presses the raw material dry weight basis).Find through overtesting,, be preferably 75-80 ℃, recovery rate can be brought up to 9%(weight, press the raw material dry weight basis as long as temperature is brought up to 70 °-85 ℃) about.We also find in addition, and the pH value of solution has considerable influence to the color of recovery rate and product during extraction.If the pH value is low excessively, then pectin is difficult for stripping, causes recovery rate low excessively.If the pH value is too high, can make the pigment stripping that remains in the raw material again.Result of the test shows, the pH value is at 2.2-4.0, is preferably the high extraction (about 9%) that can both keep pectin in the scope of 2.6-3.6, can make the color of the liquid pectin that obtains the most shallow again, and the color and luster of the pectin finished product that is separated out by this liquid pectin is also fine.In addition, the water consumption in the extraction step must guarantee pectin fully is dissolved out, if but water consumption is excessive, and then the concentration of liquid pectin is low excessively, and the precipitating step of pectin is had certain influence.So water consumption generally should be 7-12 times of raw material dry weight, be preferably 8-10 doubly.Extraction time does not have strict restriction, but generally should be more than 20 minutes.The alkali that is used to regulate the pH value in the pectin extraction step does not have any restriction, and it can be any or multiple in the listed alkali of above-mentioned decolouring step, uses sodium carbonate but be preferably.
4, pectin precipitating step
The pectin precipitating also is one of committed step of the present invention.In prior art, utilize pectin to be insoluble to the character of strong acid solution, add hydrochloric acid in the liquid pectin and make the pectin precipitating, but as mentioned above, the pectin that separates out like this can form a kind of gel piece, this gel piece is difficult for smashing when the washing purifying, the inside of gel piece can not get abundant washing, causes some impurity and fat-soluble pigment to still have a sizable part to stay the inside of pectin piece, influences product quality.
Find through a large amount of tests, utilize pectin to be insoluble to character in the alcohol, make the pectin precipitating with alcohol, pectin is come out with the grain form precipitating, because the moisture that this pectin crystal grain is carried secretly seldom, time the impurity of pectin intragranular and fat-soluble pigment fully are dissolved out so after filtration, give a baby a bath on the third day after its birth with alcohol again, have also improved the content of galacturonic acid simultaneously.Place the pectin grain through the alcohol washing vacuum drying chamber dry under 60 ℃, again through pulverizing the pectin finished product that promptly becomes powdery.The waste alcohol of using in washing step can return in the precipitating step usefulness as precipitating pectin.
Through a large amount of tests, we provide a low-ester pectin extracting method that obviously is better than prior art, and this method comprises following several key step:
1, dry sunflower plate and bar are crushed to below the 0.25mm;
2, decolorization of hot water containing soda, bleaching temperature are 50 °-90 ℃, are preferably 60 °-80 ℃; It is 6-8.5 that the addition of alkali should make the final pH value, is preferably 6.5-7.5;
3, inorganic acid decalcification, the concentration of acid should be 0.1N at least, is preferably 0.1 to 3N, and the decalcification temperature is generally room temperature to 45 ℃, is preferably 35 °-40 ℃.
4, pectin extracts, and as extract, the extract temperature is generally 70 °-85 ℃, is preferably 75 °-80 ℃ with hot water; With alkali the final pH value of extract is adjusted to 2.2-4.0, is preferably 2.6-3.6; The water consumption of extract is 7-12 a times of raw material dry weight, is preferably 8-10 doubly.
5, pectin precipitating: add alcohol in liquid pectin, make pectin solution: the ratio of alcohol is 1: 0.8 to 1: 2.0, is preferably 1: 1 to 1: 1.5; Alcohol adds the back stirring promptly had the lenticular particle of a large amount of pectin to separate out in 30 minutes.Filter and fully wash, then the pectin grain vacuum drying is also pulverized, promptly obtain the pectin finished product with alcohol.
Therefore, low-ester pectin extracting method of the present invention comprises altogether: raw material pulverizing, decolouring, decalcification, pectin extraction and pectin precipitating be totally 5 steps.But, the invention is characterized in that decolouring, pectin extract and three steps of pectin precipitating.And for these three steps, its essential feature is: the decolouring step is a decolorization of hot water containing soda, and water temperature is 50 °-90 ℃, and the addition of alkali equals 6-8.5 with the final pH value of the aqueous solution and is as the criterion; The pectin extraction step is a hot water extracting, and water temperature is 70 °-85 ℃; With alkali the pH value of extract is adjusted to 2.2-4.0; The consumption of water equals 7-12 times of raw material dry weight; Pectin precipitating step is the alcohol precipitating, and pectin extracting soln is 1: 0.8 to 1: 2.0 with the ratio of alcohol.
As long as in pectous extracting method, take above-mentioned essential feature, just can make technology of the present invention compared with prior art obtain substantial marked improvement.Other above-mentioned features belong to further qualification, preferable or additional feature, add other features on the basis of above-mentioned essential feature, can make method of the present invention obtain better effect.
Advantage, the especially recovery rate that method of the present invention can be decoloured at pectin product, pectin recovery rate and pectin purity several respects obtain significantly to be better than prior art and more remarkable as this two aspect of galacturonic acid content of one of pectin purity leading indicator.The pectin recovery rate of the inventive method generally all reaches 9%(weight, presses the raw material dry weight basis), higher by 50% than prior art.Galacturonic acid content in the pectin that extracts with method of the present invention has reached 87.5%(weight), 66% exceeded 20% than what prior art (CN85106947A) reached approximately.Surpassed U.S. FCC standard (food sanitation standard) desired 〉=70%, even surpassed 82.3% of International Pharmacopoeia defined.
In order to explain the present invention better, enumerate two preferred embodiments below:
Embodiment 1
In acidproof leaching tanks, add sunflower powder (below the 0.25mm) 5000g, Na
2CO
3150g, light water 75L stirred 30 minutes under 70 ℃ temperature, here because acidic materials and natural colouring matter and Na in the sunflower
2CO
3Effect and pH is reduced to about 7 gradually from the strong basicity scope is because this pH value is in 6.5 to 7.5 the preferred range, so adjust pH more not.Remove the decolouring aqueous solution with filter press technique.With filter residue with 70 ℃ hot wash 2 times, press filtration again.The gained filter residue is put into above-mentioned acidproof leaching tanks, add water 50L, concentrated hydrochloric acid 2L, stir 30 minutes down with dissolving calcium wherein at 40 ℃, filter, wash with water 2 times, press filtration again will be put back in the leaching tanks through the filter residue of deliming, adds water 50L, and uses Na
2CO
3The pH value is regulated and maintained about 3.0, under 80 ℃ condition, stirred 30 minutes press filtration.The pectous filtrate of obtain is put into said vesse, add isopyknic alcohol (being used to wash the waste alcohol of pectin crystal grain in front in the experiment), stirred 30 minutes.At this moment pectin is separated out from solution with grains, then press filtration.Again the pectin crystal grain that leaches is put into another container, the fresh alcohol that is adjusted to about 3.0 with the pH value washs three times, each 5L.Filter out pectin crystal grain at last, under the sun, dry, obtain dry pectin 475G (recovery rate is a 9.5%(weight)).Product is sent to state food quality supervision and inspection center analyzes, it the results are shown in the table 1., the parameter of prior art result that CN85106947A obtains and U.S. FCC prescribed by standard is also listed in the table 1 in the lump simultaneously for for the purpose of contrasting.
The branch result of table 1, product of the present invention and prior art products and U.S. FCC standard
| Interventions Requested | Unit | Product of the present invention analyse the result | The analysis result of prior art products | The standard gauge definite value |
| Degree of gelation | Degree | 137 | 130 | 100 |
| Esterification degree | % | 27.3 | 30 | ≤50 |
| The amidatioon degree | % | 2.9 | ||
| Total galacturonic acid | % | 87.5 | 66 | ≤70 |
| Loss on drying | % | 9.7 | 10 | ≤12 |
| Total ash | % | 8.2 | 1.5 | ≤10 |
| Acid insoluble ash | % | 0.7 | 0.2 | ≤1 |
| Arsenic (As) | mg/kg | ＜3 | 0.07 | ≤3 |
| Heavy metal (in Pb) | mg/kg | ＜40 | 0.44 | ≤40 |
From the result of table 1 as can be seen, the quality index of product that this embodiment obtains all meets U.S. FCC standard, and majority parameters surpasses the index of prior art, and is wherein more remarkable with the content of total galacturonic acid.Should illustrate that the content of ashes of this embodiment product is than the prior art height, its reason is because the final products of this embodiment are to dry under in the open the condition and the cause of being sneaked into by dust.We have done second batch of experiment (embodiment 2) again after having purchased vacuum drying chamber for this reason.
Embodiment 2
Except final products adopted the vacuum drying chamber oven dry rather than dry under the condition in the open, other institutes were all identical with embodiment 1 with condition in steps.We have done analysis to the total ash of product, and recording its total ash is 0.53%, well below U.S. FCC prescribed by standard≤10%, also be lower than 1.5% of prior art largely.Other indexs except that ash content are identical with embodiment 1 basically.
More than listed embodiments of the invention, but these embodiment can not be as limitation of the invention.Those skilled in the art can make various changes to the present invention under the condition that does not deviate from design of the present invention and claim institute limited range, but all these classes changes still belong to scope of the present invention.Be also pointed out that in addition, though embodiments of the invention are only tested with dish and the bar of sunflower, but those skilled in the art are readily appreciated that, every plant that contains low-ester pectin all is suitable for adopting method of the present invention to extract wherein low-ester pectin, in the case, as long as its essential features in the application's claim institute restricted portion, must be considered to belong to scope of the present invention.
Claims (8)
1, the extracting method of low ester pectin from sunflower, this method comprise to be extracted the dish of sunflower and bar pulverizing, alkaline bleaching, inorganic acid decalcification, pectin and 5 key steps of pectin precipitating, it is characterized in that:
Said alkaline bleaching step is a decolorization of hot water containing soda, and used water temperature is 50-90 ℃, and the addition of alkali equals 6-8.5 with the final pH value of the aqueous solution and is as the criterion,
Said pectin extraction step is a hot water extracting, the 7-12 that the consumption of water equals the raw material dry weight doubly, water temperature is 70-85 ℃, with alkali the final pH value of extract is transferred to 2.2-4.0,
Said pectin precipitating step is the alcohol precipitating, and pectin extracting soln is 1: 0.8 to 1: 2.0 with the ratio of alcohol.
2, the extracting method of low ester pectin from sunflower as claimed in claim 1 is characterized in that, used water temperature is 60-80 ℃ in the alkaline bleaching step.
3, the extracting method of low ester pectin from sunflower as claimed in claim 1 is characterized in that, the alkali addition in the alkaline bleaching step equals 6.5-7.5 with the final pH value of the aqueous solution and is as the criterion.
4, as the extracting method of the low ester pectin from sunflower of claim 1 or 3, it is characterized in that used alkali is sodium carbonate in the alkaline bleaching step.
5, the extracting method of low ester pectin from sunflower as claimed in claim 1 is characterized in that, used water temperature is 75-80 ℃ in the pectin extraction step.
6, sunflower extracting pectin as claimed in claim 1 is characterized in that, the alkali that is used to regulate extracting liquid pH value in the pectin extraction step is sodium carbonate.
7, the extracting method of low ester pectin from sunflower as claimed in claim 1 is characterized in that, the water consumption in the pectin extraction step equals 8-10 times of raw material dry weight.
8, the extracting method of low ester pectin from sunflower as claimed in claim 1 is characterized in that, the pectin extracting soln in pectin precipitating step and the volume ratio of alcohol are 1: 1 to 1: 1.5.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93106836A CN1029290C (en) | 1993-06-10 | 1993-06-10 | Method of extracting low ester pectin from sunflower |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN93106836A CN1029290C (en) | 1993-06-10 | 1993-06-10 | Method of extracting low ester pectin from sunflower |
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| Publication Number | Publication Date |
|---|---|
| CN1079871A true CN1079871A (en) | 1993-12-29 |
| CN1029290C CN1029290C (en) | 1995-07-12 |
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|---|---|---|---|
| CN93106836A Expired - Fee Related CN1029290C (en) | 1993-06-10 | 1993-06-10 | Method of extracting low ester pectin from sunflower |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045449C (en) * | 1996-07-12 | 1999-10-06 | 张文沂 | Separation purifying method for sunflower low ester pectin |
| CN1067688C (en) * | 1994-11-18 | 2001-06-27 | 广西民族学院 | Process and apparatus for producing pectine by pre-acidolysis and continuous high-acidity extraction |
| CN103535837A (en) * | 2003-08-19 | 2014-01-29 | 杜邦营养生物科学有限公司 | Process for preparing a food product using depolymerised pectin as stabiliser |
| CN104341538B (en) * | 2013-08-01 | 2016-10-26 | 东北师范大学 | A kind of method for separating and preparing of high HG content Helianthi pectin |
| CN107474157A (en) * | 2017-08-28 | 2017-12-15 | 广西钟山县富强雅瑶华香农业有限公司 | A kind of extracting method of sunflower pectin |
| CN109762076A (en) * | 2019-01-28 | 2019-05-17 | 江南大学 | A method of extracting pectin and protein simultaneously from sunflower plate |
-
1993
- 1993-06-10 CN CN93106836A patent/CN1029290C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1067688C (en) * | 1994-11-18 | 2001-06-27 | 广西民族学院 | Process and apparatus for producing pectine by pre-acidolysis and continuous high-acidity extraction |
| CN1045449C (en) * | 1996-07-12 | 1999-10-06 | 张文沂 | Separation purifying method for sunflower low ester pectin |
| CN103535837A (en) * | 2003-08-19 | 2014-01-29 | 杜邦营养生物科学有限公司 | Process for preparing a food product using depolymerised pectin as stabiliser |
| CN104341538B (en) * | 2013-08-01 | 2016-10-26 | 东北师范大学 | A kind of method for separating and preparing of high HG content Helianthi pectin |
| CN107474157A (en) * | 2017-08-28 | 2017-12-15 | 广西钟山县富强雅瑶华香农业有限公司 | A kind of extracting method of sunflower pectin |
| CN109762076A (en) * | 2019-01-28 | 2019-05-17 | 江南大学 | A method of extracting pectin and protein simultaneously from sunflower plate |
| CN109762076B (en) * | 2019-01-28 | 2020-04-17 | 江南大学 | Method for simultaneously extracting pectin and protein from sunflower discs |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1029290C (en) | 1995-07-12 |
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