CN1045449C - Separation purifying method for sunflower low ester pectin - Google Patents
Separation purifying method for sunflower low ester pectin Download PDFInfo
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- CN1045449C CN1045449C CN96107137A CN96107137A CN1045449C CN 1045449 C CN1045449 C CN 1045449C CN 96107137 A CN96107137 A CN 96107137A CN 96107137 A CN96107137 A CN 96107137A CN 1045449 C CN1045449 C CN 1045449C
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Abstract
The present invention provides a separation purifying method for low ester pectin of sunflowers, which comprises the following steps: (1), saturation water solution of calcium chloride is added to pectin extracting liquid or solution, the weight of the saturation water solution of calcium chloride is equal to 3 to 5% of the total weight of solution, and calcium pectate of settling out is filtered and collected; (2), the calcium pectate is wore to form paste, decalcification is carried out through hydrochloric acid processing, and the pectate calcium is changed into pectin crystal grains. The method can also optionally comprises the following steps: (3), 2 to 10 times of water is added to the precipitation of the pectin crystal grains, a pH is adjusted to be. 5 to 3.5 by alkali, and stirring is carried out until the pectin is completely dissolved; (4), spray drying is carried out, and the products of loose pectin grains are manufactured. The separation purifying method for low ester pectin of sunflowers can obtain high-purity pectin products without alcohol, and has the advantages of simple production process and low cost.
Description
The present invention relates to the separation purification method of pectin, or rather, relate to the separation purification method of low ester pectin from sunflower.
The Chinese patent ZL93106836.3 of prior art discloses a kind of extracting method of low ester pectin from sunflower, this method comprises the separation and the purification procedures of low ester pectin from sunflower, this patent specification is stated as pectin precipitating step with the separation and the purification procedures merging of pectin, promptly " 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 use the alcohol thorough washing, then the pectin grain vacuum drying is also pulverized, promptly obtain the pectin finished product " (seeing that this patent disclosure Instructions Page 10 2-6 is capable).The advantage of the method for this separation and purifying is that pectin is separated out with the compact grained form, is easy to washing, impurity fully can be removed, thereby can be obtained the pectin product that the very high and quality index of purity all meets U.S. FCC III standard.Yet, learn according to production practice, according to the method for this patent, produce one ton of pure pectin and need consume 3-6 ton alcohol, thereby cause having improved greatly the cost of pectin, overslaugh the suitability for industrialized production of pectin.
The objective of the invention is will be at the shortcoming of prior art, provides a kind of alcohol consumption few or do not use alcohol, with low cost, can guarantee the separation purification method of the low ester pectin from sunflower of pectin product quality simultaneously.
The inventor is in order to solve the too much problem of alcohol consumption, many methods have been tested, comprising physics and mechanical means such as ultrafiltration method of enrichment and high speed centrifugation partition methods, but all do not have successfully, at last fractionation is being carried out finding after the deep research, in pectin extracting soln or pectolysis liquid, add the calcium chloride saturated solution, pectin (being the mixture of galacturonic acid and pectinic acid) is separated out with the grumeleuse form of calcium pectinate, thereby can remove the water-soluble impurity of the overwhelming majority, again this calcium pectinate grumeleuse is worn into pasty state, with hydrochloric acid the pH value of this mashed prod is transferred to 0.5-1.2, after reaction in 0.5 hour, calcium is removed fully, thereby make calcium pectinate become pectin again and improved purity.And because pectin is insoluble to acidic solution, and be the fine powder grains, so water just can be easy to its washes clean, thereby impurity is fully eliminated by the pectin that forms behind calcium pectinate mashed prod and the hydrochloric acid reaction.Yet the dissolution rate of the pectin of Huo Deing is slower like this, uses inconvenient on industrial production.So, be preferably in after the hydrochloric acid decalcification, the close grain shape pectin that is obtained is dissolved in Na
2CO
3, NaOH or NH
4OH is adjusted in the aqueous solution of pH2.5-3.5, thereby obtain a kind of pectin solution, then this pectin solution is adjusted to pure water and contains pectin 3-8 weight %, carry out drying with spray-drying process, the pectin powder of Huo Deing is loose particulate state like this, be easy to dissolving, be well suited for industrial production and use.Because these results of study, thereby finished the present invention.
Thereby, the invention provides the separation purification method of following every described low ester pectin from sunflower, it specifically is constructed as follows:
1, a kind of separation purification method of low ester pectin from sunflower is characterized in that, it comprises the following step:
(1) with pure water the extracting solution or the lysate of low ester pectin from sunflower is adjusted to the pectin that contains 0.8-2 weight %, toward wherein adding with respect to the pectin solution gross weight is the saturated calcium chloride water of 3-5 weight %, stirring reaction 5-30 minute, treat precipitation fully, filtering separation is also collected the calcium pectinate precipitation that separates out;
(2) pure water of 0.5-2 times of weight of adding in the calcium pectinate precipitation that is obtained, with grinding machine it is worn into the pasty state slurries, preferably be milled to particle diameter below 0.177mm (80 order), with hydrochloric acid with these slurries, the pH value be adjusted to 0.5-1.2, stirring reaction 15 minutes to 1 hour, preferred 20 minutes to 40 minutes, filter collecting precipitation, preferably with the pure water washing for several times to can't check calcium ion with ordinary method till, filter at last and collect pectin crystal grain precipitation product.
2, as above-mentioned first described method, it is characterized in that, in said step (2) afterwards, also comprise follow-up step (3) and (4), that is:
(3) in step (2) the pectin crystal grain that obtains precipitation, add 2-10 doubly, the pure water of preferred 4-7 times of weight, and then use Na
2CO
3, K
2CO
3, NaOH, KOH and NH
4Among the OH any one or more preferably used NH
4OH is adjusted to the pH value between the 2.5-3.5, is preferably between the 2.8-3.4, is stirred to the dissolving fully of pectin precipitation;
(4) with pure water obtaining pectin solution is adjusted to and contains pectin 3-8 weight %, the concentration of preferred 4-6 weight % is carried out spraying drying then.
Compare with the pectin separation purification method of prior art, the advantage of the separation purification method of low ester pectin from sunflower of the present invention is to use alcohol can obtain highly purified pectin product, and production technique is simple, and is with low cost.
Enumerate embodiment below and further explain the present invention.
Embodiment 1 is extracted and separation and purification pectin by Sunflower Receptacle
At first basically, the embodiment 1 according to prior art ZL93106836.3 prepares the low ester pectin from sunflower extracting solution, that is:
In acidproof leaching vat, add Sunflower Receptacle powder (below the 0.25mm) 5000g, Na
2CO
3150g, tap water 75l stirred 30 minutes under 60 ℃ temperature, at this moment because acidic substance and natural pigment and Na in the Sunflower Receptacle
2CO
3The effect and pH is reduced to about 7 gradually.Remove the decolouring aqueous solution with filter press technique.With filter residue with 60 ℃ hot wash 2 times, press filtration again.The gained filter residue is put into above-mentioned acidproof leaching vat, 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 vat through the filter residue of deliming, adds distilled water 50l and uses Na
2CO
3The pH value is regulated and maintained about 3.0, under 80 ℃ condition, stirred 30 minutes, press filtration, obtain filtrate 48l, the wherein about 11g/l of the content of pectin altogether.The pectin extracting soln that the obtained raw material as the inventive method embodiment is used.
Below, proceed experiment according to method of the present invention.
Adding distilled water 200l stirs in above-mentioned pectin extracting soln, then toward wherein adding the saturated calcium chloride water of 10kg, stirring reaction 20 minutes, the calcium pectinate precipitation that filtering separation and collection separate out, the about 1100g of acquisition calcium pectinate wet feed.
Add 1100g distilled water in the calcium pectinate precipitation, with a colloidal mill calcium pectinate is worn into the pasty state slurries, granularity is below 0.149mm (100 order).With hydrochloric acid the pH value of these slurries is adjusted to 1.0, stirring reaction 30 minutes, then for several times with distilled water wash, can't check calcium oxalate precipitation with oxalic acid solution to the filtrate till.Pectin crystal grain precipitation is collected in last press filtration.Obtain the about 950g of pectin crystal grain wet feed.
The dissolution rate of this pectin crystal grain in water is slower, for the pectin that obtains to be dissolved in the water rapidly, then carries out the spray-drying process step of pectin.
In above-mentioned pectin crystal grain wet feed, add distilled water 5l, this moment may since the pH value that still has a small amount of remaining hydrochloric acid to make this solution below 2, pectin is difficult to dissolve.NH with 0.2M
4OH solution is adjusted to 3.0 with the pH value, stirs after 30 minutes, and pectin dissolves fully.
In this pectin solution, add 5l distilled water again, carry out spraying drying after stirring, obtained the loose pectin powder 480g (extraction yield is 9.6 weight %) of particle.Product is sent to state food quality supervision and inspection center analyzes, it the results are shown in the table 1.Simultaneously, there is the index of patent result that ZL93106836.3 obtains and U.S. FCC III prescribed by standard also to list in the table 1 in the lump earlier the applicant for for the purpose of contrasting.
From the result of table 1 as can be seen, the quality index of product that this embodiment obtains all meets U.S. FCC III standard and also is better than this standard significantly and has patent product quality indicator that ZL93106836.3 obtains very approaching earlier with the applicant, and wherein most indexs also are better than or equal the index of this prior art.And method of the present invention can obtain high-quality product without alcohol, thereby greatly reduces cost, and has reduced the production unit volume, has simplified production technique, and is very favourable to industrial production.
Table 1 the present invention with patent ZL93106836.3 is arranged earlier
Analytical results and U.S. FCC III standard
| Interventions Requested | Unit | Product of the present invention | Patented product is arranged earlier | FCC III standard gauge definite value |
| Degree of gelation | Degree | 122 | 137 | ≥100 |
| Gamma value | ％ | 24.1 | 27.3 | ≤50 |
| The amidation degree | ％ | 0.2 | 2.9 | ≤40 |
| Total galacturonic acid | ％ | 97.6 | 87.5 | ≥70 |
| Weight loss on drying | ％ | 11.5 | 9.7 | ≤12 |
| Total percent of ash | ％ | 3.3 | 8.2 | ≤10 |
| Acid insoluble ash | ％ | 0.8 | 0.7 | ≤1 |
| Arsenic (AS) | mg/kg | ＜3 | ＜3 | ≤3 |
| Heavy metal is (with P bMeter) | mg/kg | ＜40 | ＜40 | ≤40 |
Embodiment 2 is by crude pectin separation and purification pectin
Getting a kind of galacturonic acid content is the pectin 500g of 86 weight %, with 80 ℃ distilled water 10000ml with pectin furnishing scattered paste shape, the saturated calcium chloride solution that adds 500ml, stirring reaction 20 minutes, blocky calcium pectinate precipitation is coagulated in acquisition, filtering separation is also collected calcium pectinate (about 1150g wet feed), toward wherein adding 1150ml distilled water blended rubber body mill it is worn into pasty state (granularity is below 0.149mm (100 order)) again.With hydrochloric acid the pH value is adjusted to 1.0, stirring reaction 30 minutes filters, and the calcium ion flush away is promptly obtained the pectin precipitation of purifying with distilled water.Again toward wherein adding distilled water 8000ml and it being stirred into suspension, with ammoniacal liquor its pH value is adjusted to 3.0, stir and it is dissolved fully, carry out spraying drying then, obtain the pectin powder of 443g, the index of its every quality index and embodiment 1 product that obtains is approaching, and the content of its total galacturonic acid is 93 weight %.
Claims (9)
1, a kind of separation purification method of low ester pectin from sunflower is characterized in that, it comprises the following step:
(1) pectin that the extracting solution or the lysate of low ester pectin from sunflower is adjusted to 0.8-2 weight % with pure water, toward wherein adding with respect to the pectin solution gross weight is the saturated calcium oxide aqueous solution of 3-5 weight %, stirring reaction 5-30 minute, treat precipitation fully, filtering separation is also collected the calcium pectinate precipitation that separates out;
(2) add the pure water of 0.5-2 times of weight in the calcium pectinate that obtained precipitation, with grinding machine it is worn into the pasty state slurries, with hydrochloric acid the pH value of these slurries is adjusted to 0.5-1.2, stirring reaction 15 minutes to 1 hour filters and collects pectin crystal grain and precipitate product.
2, the method for claim 1 is characterized in that, in said step (2) afterwards, also comprises follow-up step (3) and (4), that is:
(3) to step (2) add the pure water of 2-10 times of weight in the pectin crystal grain that the obtains precipitation, and then use Na
2CO
3, K
2CO
3, NaOH, KOH and NH
4Among the OH any one or more is adjusted to the pH value between the 2.5-3.5, is stirred to the dissolving fully of pectin precipitation;
(4) with pure water obtaining pectin solution is adjusted to the concentration that contains pectin 3-8 weight %, carries out spraying drying then.
3, method as claimed in claim 1 or 2 is characterized in that, with grinding machine the calcium pectinate precipitation is milled to below the 0.177mm (80 order) in step (2), and then carries out follow-up step.
4, method as claimed in claim 1 or 2 is characterized in that, in step (2) after the pH value of levigated slurries being adjusted to 0.5-1.2 with hydrochloric acid, stirring reaction 20 to 40 minutes, and then carry out follow-up step.
5, method as claimed in claim 1 or 2 is characterized in that, filters in step (2) after the collecting precipitation, extremely can't check calcium ion with the pure water repetitive scrubbing with ordinary method till, and then carry out follow-up step.
6, method as claimed in claim 2 is characterized in that, in step (3), to step (2) add the pure water of 4-7 times of weight in the pectin that the obtains precipitation, and then regulate pH value and other subsequent step.
7, method as claimed in claim 2 is characterized in that, in step (3), uses NH
4OH is adjusted to the pH value between the 2.5-3.5, and then carries out follow-up step.
8, as claim 2 or 7 described methods, it is characterized in that, the pH value is adjusted between the 2.8-3.4, and then carry out follow-up step in step (3).
9, as claim 2 or 7 described methods, it is characterized in that, in step (4), pectin solution is adjusted to the concentration that contains pectin 4-6 weight %, carry out spraying drying then.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96107137A CN1045449C (en) | 1996-07-12 | 1996-07-12 | Separation purifying method for sunflower low ester pectin |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96107137A CN1045449C (en) | 1996-07-12 | 1996-07-12 | Separation purifying method for sunflower low ester pectin |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1139674A CN1139674A (en) | 1997-01-08 |
| CN1045449C true CN1045449C (en) | 1999-10-06 |
Family
ID=5119546
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN96107137A Expired - Fee Related CN1045449C (en) | 1996-07-12 | 1996-07-12 | Separation purifying method for sunflower low ester pectin |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1062870C (en) * | 1997-12-16 | 2001-03-07 | 张文沂 | Method for purifying sun-flower seed low-ester pectine |
| CN103130913B (en) * | 2013-02-17 | 2016-08-03 | 暨南大学 | A kind of calcium pectinate and production method thereof and application |
| CN103864956B (en) * | 2014-03-18 | 2016-06-01 | 河北科技大学 | A kind of method extracting pectin from eggplant fruit |
| CN105384847B (en) * | 2015-10-14 | 2018-08-21 | 烟台安德利果胶股份有限公司 | A kind of instant pectin and preparation method thereof |
| CN105777936B (en) * | 2016-05-19 | 2018-06-22 | 江南大学 | A kind of low-ester pectin and preparation method thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60160893A (en) * | 1984-01-30 | 1985-08-22 | Mitsui Toatsu Chem Inc | Method to prepare improved purified fructan solution |
| CN87100163A (en) * | 1987-01-08 | 1988-07-20 | 江西工业大学 | Extract the method for sunflower low ester edible pectin with oxalic acid extraction-molysite deposition technology |
| CN1055466A (en) * | 1990-04-07 | 1991-10-23 | 中国科学院科理高技术公司成都分公司 | A kind of slaine method is obtained through refining the method for pectin |
| CN1070649A (en) * | 1992-09-15 | 1993-04-07 | 张家口地区果胶厂 | A kind of production method of extracting low-ester pectin from sunflower disc |
| CN1079871A (en) * | 1993-06-10 | 1993-12-29 | 张文沂 | The extracting method of low ester pectin from sunflower |
-
1996
- 1996-07-12 CN CN96107137A patent/CN1045449C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60160893A (en) * | 1984-01-30 | 1985-08-22 | Mitsui Toatsu Chem Inc | Method to prepare improved purified fructan solution |
| CN87100163A (en) * | 1987-01-08 | 1988-07-20 | 江西工业大学 | Extract the method for sunflower low ester edible pectin with oxalic acid extraction-molysite deposition technology |
| CN1055466A (en) * | 1990-04-07 | 1991-10-23 | 中国科学院科理高技术公司成都分公司 | A kind of slaine method is obtained through refining the method for pectin |
| CN1070649A (en) * | 1992-09-15 | 1993-04-07 | 张家口地区果胶厂 | A kind of production method of extracting low-ester pectin from sunflower disc |
| CN1079871A (en) * | 1993-06-10 | 1993-12-29 | 张文沂 | The extracting method of low ester pectin from sunflower |
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|---|---|
| CN1139674A (en) | 1997-01-08 |
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