CN105295434A - Method for combined extraction of haematochrome and pectin from pitaya peel - Google Patents
Method for combined extraction of haematochrome and pectin from pitaya peel Download PDFInfo
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- CN105295434A CN105295434A CN201510788412.0A CN201510788412A CN105295434A CN 105295434 A CN105295434 A CN 105295434A CN 201510788412 A CN201510788412 A CN 201510788412A CN 105295434 A CN105295434 A CN 105295434A
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Abstract
The invention discloses a method for combined extraction of haematochrome and pectin from pitaya peel. The method comprises the following specific steps: firstly chopping pitaya peel, blanching, drying, crushing, extracting by adding ethanol, filtering, and respectively collecting a filtrate and filter residue; carrying out extraction purification on the filtrate respectively by using a polyethylene glycol/ammonium sulfate aqueous two-phase system and trichloromethane so as to obtain a viscous pasty pitaya haematochrome; washing the filter residue with water to remove alcohol and carrying out heat insulation and acidolysis, processing by adding cation exchange resin and filtering, concentrating a filtrate, precipitating with ethanol, centrifuging, drying and crushing so as to obtain flaxen pectin powder. The method of the invention has advantages of simple equipment and low cost. In addition, high-purity haematochrome and high-ester pectin can be simultaneously extracted from pitaya peel. Thus, resource wasting caused by single extraction is avoided, and comprehensive utilization rate of pitaya can be remarkably raised.
Description
Technical field
The invention belongs to agricultural byproducts comprehensive utilization deep process technology field, be specifically related to a kind of method of combined extracting haematochrome and pectin from Hylocereus undatus pericarp.
Background technology
Hylocereus undatus has another name called celestial mamoncillo, Hylocereus undatus etc., is a kind of tropical fruit of high nutritive value, has the plurality of health care functions such as aid digestion, hypotensive, hypoglycemic, anti-oxidant, deeply likes by human consumer.Within 2013, China's Hylocereus undatus cultivated area reaches more than 100,000 mu, also has the trend constantly expanded at present.
Hylocereus undatus pericarp accounts for really heavy 1/4th, and it is rich in the native chemical such as haematochrome and pectin composition.But in food-processing and daily edible process, Hylocereus undatus pericarp is often directly abandoned by as waste material, causes the huge wasting of resources.Haematochrome in Hylocereus undatus pericarp is mainly Betacyanins and glycoside thereof, and it has well anti-oxidant, scavenging free radicals, raising immunizing power and the physiological function such as anticancer, can be used as natural food colour with health role or foodstuff additive; And pectin is the main component of soluble dietary fibre in human body seven major nutrient, and it also has good gelationization and emulsifying effect, is widely used in food, medicine and cosmetic industry.
At present more existing utilize Hylocereus undatus pericarp to extract the Study on Process of haematochrome and pectin for raw material.As patent CN1631987A discloses a kind of method extracting water-soluble red colouring matter from dragon fruit pulp, pericarp; Patent CN103497534A discloses one and utilizes supercritical CO
2the method of fluid extraction Hylocereus undatus pericarp pigment; Patent CN104212196A discloses the preparation method of haematochrome in a kind of Hylocereus undatus pericarp; Yuan Yafang etc. (" separation of red meat Hylocereus undatus pericarp pigment, purifying and HPLC-MS analyze ", University Of Agriculture and Forestry In Fujian's journal (natural science edition), 2013,42 (6): 589-592) separation of red meat Hylocereus undatus pericarp pigment, purifying research is reported; King marks (" extraction of Hylocereus undatus pericarp pigment and the research of anti-oxidant activity thereof ", foodstuffs industry science and technology, 2013 (43) 5:234-238) such as poems and reports the extraction of Hylocereus undatus pericarp pigment and the research of anti-oxidant activity thereof; Wang Xue etc. (" in pitaya peel the extraction of pectin and structural research thereof ", Food Additives Used in China, 2015,3:102-106) report extraction and the structural research thereof of pectin in pitaya peel; Chen Jingjing etc. (" optimizing research of red meat Hylocereus undatus pericarp pectous extracting method condition ", southern china fruit tree, 2014,43 (3): 96-98) report the optimizing research of red meat Hylocereus undatus pericarp pectous extracting method condition.These patents and document are all confined to the separation and Extraction of single component in Hylocereus undatus pericarp, raw material cannot be fully used, and in the extraction process of these single components, some only obtains the thick product of haematochrome, pectin, containing impurity such as a large amount of carbohydrates in these thick products, its quality does not reach industrial requirements; Some technology utilization supercritical CO
2fluid or high performance liquid chromatograph carry out separation and purification to haematochrome, although purity reaches requirement, there is apparatus expensive, the high deficiency of production cost; The employing macroporous adsorbent resin also had carries out absorption and purification, though a large amount of magazins' layout can be removed, absorption and the wash-out cycle of resin are long, add the complicacy of operation.
Summary of the invention
The object of the invention is for the deficiencies in the prior art, a kind of method of combined extracting haematochrome and pectin from Hylocereus undatus pericarp is provided, its equipment used is simple, easy to operate, extraction cost is low, product purity is high, can significantly improve the comprehensive utilization ratio of Hylocereus undatus pericarp resource.
For achieving the above object, the present invention adopts following technical scheme:
A method for combined extracting haematochrome and pectin from Hylocereus undatus pericarp, specifically comprises the following steps:
1) by fresh Hylocereus undatus pericarp chopping, boiling water boiling 5 ~ 8min, makes polygalacturonase inactivation, clear water rinsing post-drying, pulverizing;
2) by step poly-1) gained powder adds its volume 5 ~ 10 times, mass concentration is the ethanol of 70%, lixiviate 1 ~ 2h under room temperature, filters, and collects filtrate and filter residue respectively;
3) by poly-for step 2) gained filtrate vacuum concentration at 50-55 DEG C, to after dry, carries out abstraction purification with polyoxyethylene glycol/ammonium sulfate double-aqueous phase system; Upper strata dark red solution is the polyglycol solution containing haematochrome, and lower floor's light red solution is the ammoniumsulphate soln containing impurity such as carbohydrates;
4) step poly-3 is got) upper solution, add isopyknic chloroform extraction, haematochrome enters the aqueous phase solution on upper strata, and polyoxyethylene glycol enters the organic phase solution of lower floor, and Hylocereus undatus haematochrome is separated with polyoxyethylene glycol, collects upper strata aqueous phase solution;
5) by step poly-4) gained aqueous phase solution vacuum concentration at 50 ~ 55 DEG C, obtain the Hylocereus undatus haematochrome of thickness paste;
6) by step poly-2) gained filter residue tap water rinse, removing residual ethanol, then add the oxalic acid of filter residue volume 5 ~ 10 times of deionized waters and filter residue weight 1 ~ 3%, be 3.0 ~ 3.6 by sodium hydrate regulator solution pH value, be then heated to 60 ~ 80 DEG C, slowly stir 60min, filter, collect filtrate;
7) by poly-for step 6) gained filtrate adds ion exchange resin, and slowly stir 30 ~ 60min under room temperature, filter, collect filtrate;
8) by poly-for step 7) gained filter vacuum is concentrated into 1/4 ~ 1/5 of original volume, then adds the dehydrated alcohol of 1-2 times of volume, and through centrifugal, precipitation, dry, pulverize, obtain flaxen pectin powder.
Step poly-3) it is middle that polyoxyethylene glycol/polyglycol solution and ammoniumsulphate soln specifically join in filtrate by ammonium sulfate double-aqueous phase system abstraction purification, and after magnetic agitation 20 ~ 30min, regulator solution pH value is 5.0 ~ 5.5, and left at room temperature 6 ~ 12h makes its layering;
In described polyoxyethylene glycol/ammonium sulfate double-aqueous phase system, the mass concentration of polyoxyethylene glycol is 15 ~ 25%, and the mass concentration of ammonium sulfate is 10 ~ 15%; The molecular weight optional 2000,4000 and 6000 of polyoxyethylene glycol used, preferably 6000.
Ion exchange resin described in step 7) is storng-acid cation exchange resin, and its consumption is 1 ~ 2% of filter residue weight.
Step 2) and step 8) in ethanol used through reclaim after can be recycled.
compared with prior art, the present invention has following remarkable advantage:
(1) present invention achieves the combined extracting of Hylocereus undatus pericarp haematochrome, pectin two kinds of materials, and yield is suitable with a kind of material of existing single extraction with purity, but avoid the wasting of resources that single extraction brings, substantially increase the comprehensive utilization ratio of fire fruit dragon.
(2) when carrying out extraction purification to Hylocereus undatus pericarp haematochrome, the present invention first utilizes the ethanolic soln of low concentration to carry out lixiviate, obtain haematochrome crude extract, and then utilize polyoxyethylene glycol/ammonium sulfate double-aqueous phase system to be opened by the magazins' layout such as the haematochrome in crude extract and carbohydrate.Because polyoxyethylene glycol/ammonium sulfate aqueous two phase extraction technique can be carried out in a mild condition, thus farthest ensure that the stability of haematochrome, and its separation efficiency is high, the time is short, without the need to large-scale and complicated device, easy and simple to handle.
(3) owing to being rich in Ca in Hylocereus undatus pericarp
2+, Mg
2+plasma, has sealing process to pectin, can affect protopectin-and transform to water soluble pectin, therefore its extraction yield of acidity extraction pectin of routine is low, gained pectin is of poor quality.The mineral acid (hydrochloric acid, sulfuric acid, phosphoric acid etc.) that the present invention adopts oxalic acid to substitute and uses in conventional acid solution carries out acidolysis, utilizes oxalate denominationby to have very strong metal-chelating effect, can well by pericarp membrane wall with Ca
2+, Mg
2+the water-insoluble pectin extraction that chelating is formed out, adds the positively charged ion that ion exchange resin absorption is remaining simultaneously, can improve extraction yield and the quality of pectin in pectin solution.
Accompanying drawing explanation
Fig. 1 is the UV-Vis spectra figure of the Hylocereus undatus pericarp haematochrome solution of preparation of the present invention.
Fig. 2 is the UV-Vis spectra figure of the Hylocereus undatus pericarp haematochrome solution after single extraction purification.
Embodiment
More being convenient to make content of the present invention understand, below in conjunction with embodiment, technical solutions according to the invention are described further, but the present invention being not limited only to this.
combined extracting haematochrome and pectin in embodiment Hylocereus undatus pericarp
A method for combined extracting haematochrome and pectin from Hylocereus undatus pericarp, specifically comprises the following steps:
1) fresh Hylocereus undatus pericarp 400g being removed green scale is cut into the fritter that size is 3-4mm, boiling water boiling 5min, makes polygalacturonase inactivation, press dry, dry 12h, be then cooled to room temperature, be ground into powder with cooking machine in 60 DEG C of baking ovens after clear water rinsing for several times; Gained powder adds its volume 5 times, mass concentration is the ethanol of 70%, lixiviate 2h under room temperature, filters, and collects filtrate and filter residue respectively;
2) by poly-for step 1) gained filtrate at 50 DEG C vacuum concentration to after dry, add PEG6000 and ammoniumsulphate soln, the mass concentration of polyoxyethylene glycol in gained polyoxyethylene glycol/ammonium sulfate double-aqueous phase system is made to be 15%, the mass concentration of ammonium sulfate is 10%, then after magnetic agitation 30min, regulator solution pH value is 5.0, left at room temperature 6h, make its layering, upper strata dark red solution is the polyglycol solution containing haematochrome, and lower floor's light red solution is the ammoniumsulphate soln containing impurity such as carbohydrates; Get the poly-upper solution of step, add after isopyknic trichloromethane mixes, the centrifugal 10min of 3000rpm, make haematochrome enter the aqueous phase solution on upper strata, polyoxyethylene glycol enters the organic phase solution of lower floor, collects upper strata aqueous phase solution; Step is gathered gained aqueous phase solution vacuum concentration at 50 DEG C, obtain the Hylocereus undatus water-soluble natural haematochrome 5.68g of thickness paste, productive rate is 1.42%;
3) by step poly-1) gained filter residue tap water rinse, removing residual ethanol, add the oxalic acid of filter residue volume 5 times of deionized waters and filter residue weight 3% again, be 3.0 by sodium hydrate regulator solution pH value, then 60 DEG C are heated to, filter after the centrifugal 10min of slow stirring 60min, 3000rpm, collect filtrate; Step is gathered the 721 type storng-acid cation exchange resins that gained filtrate adds filter residue weight 1%, under room temperature, slowly stir 60min, filter, collect filtrate; Gained filter vacuum is concentrated into 1/4 of original volume, then add the dehydrated alcohol of 2 times of volumes, the centrifugal 10min of 6000rpm after room temperature placement 2h, obtains pectin precipitation, then pectin is deposited in 65 DEG C of vacuum driers and dries, take out levigate, obtain flaxen pectin powder 1.93g, through converting, its yield is 4.82g/kg(fresh weight), through FCC titration measuring, the gamma value of gained pectin is 64.6, is high ester pectin.
Get gained Hylocereus undatus haematochrome 1.0g, be dissolved in 100mL pure water, in its absorbancy of wavelength 400 ~ 660nm scope interscan, result as shown in Figure 1.Gained Hylocereus undatus haematochrome has obvious absorption peak in visible region, and its maximum absorption wavelength is 538nm, illustrates that its main component is beet glycoside pigment.The absorbance measuring haematochrome solution under 538nm is 0.830, according to look valency calculation formula, converses the look valency of Hylocereus undatus haematochrome
538nm=83.0.
the single extraction of haematochrome in comparative example 1 Hylocereus undatus pericarp
1) fresh Hylocereus undatus pericarp 400g being removed green scale is cut into the fritter that size is 3-4mm, boiling water boiling 5min, makes polygalacturonase inactivation, press dry, dry 12h, be then cooled to room temperature, be ground into powder with cooking machine in 60 DEG C of baking ovens after clear water rinsing for several times; Gained powder adds its volume 5 times, mass concentration is the ethanol of 70%, lixiviate 2h under room temperature, filters, and collects filtrate;
2) gained filtrate is adsorbed by D101 macroporous resin, obtain the macroporous resin being adsorbed with Hylocereus undatus haematochrome, then wash-out is carried out to macroporous resin, collect elutriant, with Rotary Evaporators vacuum concentration under temperature 50-55 DEG C of condition, obtain the Hylocereus undatus water-soluble natural haematochrome 6.42g of thickness paste, haematochrome productive rate is 1.60%.
Get fire imperial arnotto pigment 1.0g, is dissolved in 100mL pure water, and in its absorbancy of wavelength 400 ~ 660nm scope interscan, result as shown in Figure 2.Gained Hylocereus undatus haematochrome has two obvious absorption peaks at visible region 480nm and 538nm, these two wavelength are respectively the maximum absorption wavelength of betaxanthin and beet red glycosides, illustrate that Hylocereus undatus haematochrome crude extract is after macroporous resin purification, still has part betaxanthin to exist.The absorbance recording haematochrome solution at 538nm is 0.698, according to look valency calculation formula, converses the look valency of Hylocereus undatus haematochrome
538nm=69.8.
the single extraction of pectin in comparative example 2 Hylocereus undatus pericarp
1) fresh Hylocereus undatus pericarp 400g being removed green scale is cut into the fritter that size is 3-4mm, boiling water boiling 5min, makes polygalacturonase inactivation, press dry, dry 12h, be then cooled to room temperature, be ground into powder with cooking machine in 60 DEG C of baking ovens after clear water rinsing for several times; Gained powder adds the deionized water of its 5 times of volumes, with salt acid for adjusting pH to 1.5 ~ 1.6, stirs acidolysis 60min at 80 DEG C, filters after the centrifugal 10min of 3000rpm, collects filtrate; Gained filtrate rotary evaporation is concentrated into 1/4 of original volume, then adds the dehydrated alcohol of 2 times of volumes, and the centrifugal 10min of 6000rpm after room temperature placement 2h, obtains pectin precipitation; Be deposited in by gained pectin in 65 DEG C of vacuum driers and dry, take out levigate, obtain pectin powder 1.58g, after conversion, its yield is 3.96g/kg(fresh weight), through FCC titration measuring, the gamma value of gained pectin is 31.4, belongs to low-ester pectin.
More visible by embodiment and comparative example 1, the haematochrome yield of combined extraction technology is 1.42%, a little less than the haematochrome extraction yield (1.60%) of single extraction, but its look valency is then significantly higher than the haematochrome of single extraction, illustrate that the haematochrome purity that combined extracting of the present invention obtains is high, quality good.
More visible by embodiment and comparative example 2, pectin extraction rate and the pectin ester degree of combined extraction technology are all significantly higher than single extraction method, illustrate that adopting oxalic acid to substitute hydrochloric acid carries out acidolysis, coupled ion exchange process, can improve extraction yield and the quality of pectin greatly simultaneously.
The foregoing is only preferred embodiment of the present invention, all equalizations done according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (3)
1. the method for combined extracting haematochrome and pectin from Hylocereus undatus pericarp, is characterized in that: comprise the following steps:
1) by fresh Hylocereus undatus pericarp chopping, after boiling water boiling 5 ~ 8min, clear water rinsing, oven dry, pulverizing;
2) by step poly-1) gained powder adds its volume 5 ~ 10 times, mass concentration is the ethanol of 70%, lixiviate 1 ~ 2h under room temperature, filters, and collects filtrate and filter residue respectively;
3) by poly-for step 2) gained filtrate vacuum concentration at 50-55 DEG C, to after dry, carries out abstraction purification with polyoxyethylene glycol/ammonium sulfate double-aqueous phase system;
4) step poly-3 is got) upper solution, after adding isopyknic chloroform extraction, collect upper strata aqueous phase solution;
5) by step poly-4) gained aqueous phase solution vacuum concentration at 50 ~ 55 DEG C, obtain the Hylocereus undatus haematochrome of thickness paste;
6) by step poly-2) gained filter residue tap water rinse, then add the oxalic acid of filter residue volume 5 ~ 10 times of deionized waters and filter residue weight 1 ~ 3%, be 3.0 ~ 3.6 by sodium hydrate regulator solution pH value, then 60 ~ 80 DEG C are heated to, slow stirring 60min, filters, and collects filtrate;
7) by poly-for step 6) gained filtrate adds ion exchange resin, and slowly stir 30 ~ 60min under room temperature, filter, collect filtrate;
8) by poly-for step 7) gained filter vacuum is concentrated into 1/4 ~ 1/5 of original volume, then adds the dehydrated alcohol of 1-2 times of volume, and through centrifugal, precipitation, dry, pulverize, obtain flaxen pectin powder.
2. the method for combined extracting haematochrome and pectin from Hylocereus undatus pericarp according to claim 1, it is characterized in that: step poly-3) it is middle that polyoxyethylene glycol/polyglycol solution and ammoniumsulphate soln specifically join in filtrate by ammonium sulfate double-aqueous phase system abstraction purification, after magnetic agitation 20 ~ 30min, regulator solution pH value is 5.0 ~ 5.5, left at room temperature 6 ~ 12h, makes its layering;
In described polyoxyethylene glycol/ammonium sulfate double-aqueous phase system, the mass concentration of polyoxyethylene glycol is 15 ~ 25%, and the mass concentration of ammonium sulfate is 10 ~ 15%.
3. the method for combined extracting haematochrome and pectin from Hylocereus undatus pericarp according to claim 1, it is characterized in that: ion exchange resin described in step 7) is storng-acid cation exchange resin, its consumption is 1 ~ 2% of filter residue weight.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110881603A (en) * | 2019-12-24 | 2020-03-17 | 福建农林大学 | Pitaya peel-glucomannan composite microsphere body-shaping solid beverage and preparation method thereof |
| CN110881594A (en) * | 2019-12-23 | 2020-03-17 | 广西壮族自治区农业科学院 | Preparation method of dragon fruit juice |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110881594A (en) * | 2019-12-23 | 2020-03-17 | 广西壮族自治区农业科学院 | Preparation method of dragon fruit juice |
| CN110881603A (en) * | 2019-12-24 | 2020-03-17 | 福建农林大学 | Pitaya peel-glucomannan composite microsphere body-shaping solid beverage and preparation method thereof |
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