CN101245112B - Polyoses extracted from pistacia chinensis meal and extracting method thereof - Google Patents

Polyoses extracted from pistacia chinensis meal and extracting method thereof Download PDF

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CN101245112B
CN101245112B CN2008100471165A CN200810047116A CN101245112B CN 101245112 B CN101245112 B CN 101245112B CN 2008100471165 A CN2008100471165 A CN 2008100471165A CN 200810047116 A CN200810047116 A CN 200810047116A CN 101245112 B CN101245112 B CN 101245112B
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acid
solution
sodium
polysaccharide
potassium
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CN101245112A (en
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王承明
胡纱纱
陈娟娟
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YUNNAN NEW OCEAN AQUATIC PRODUCT SCIENCE AND TECHNOLOGY GROUP CO., LTD.
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Huazhong Agricultural University
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Abstract

The invention discloses a polysaccharide which is extracted from Chinese pistache and the extraction method; the polysaccharide is extracted by the following steps: the Chinese pistache raw material is added in the strong acidic solution, which is taken as extracting solution and has a concentration of 0.01 to 7mol/L, or the weak acid with the weight percentage concentration of 0.01 percent to 100 percent or the alkaline solution with the concentration of 0.05 to 8.0mol/L or the water according to the material liquid ratio of 1: 1 to 1:200g/ml and is taken out after 1 minute to 8 hours of extraction, the solution after removing the sediment is obtained by centrifugal separation or filtration, then the sufficient amount of solvent is added for full precipitation of the polysaccharide, finally the solution is removed by centrifugalization or filtration, anhydrous ethanol, propyl alcohol or propyl alcohol are used for washing for a plurality of times, and the crude polysaccharide is obtained by freeze drying. The extraction method takes the commonly used acidic solution and alkaline solution or water as the extracting liquid, the extraction conditions are simple and convenient, and the extraction method further takes the ultrasonic or microwave extraction as auxiliary means; the extraction method has higher polysaccharide yield, can greatly improve the additional values of processing and utilizing of the Chinese pistache and has great popularization and application prospects on the industrial aspect.

Description

A kind of polysaccharide that from pistacia chinensis meal, extracts and extracting method thereof
Technical field
The present invention relates to a kind of polysaccharide that from pistacia chinensis meal, extracts and extracting method thereof, belong to biochemical field.
Background technology
Chinese pistache, another name medicine wood, loblolly trees etc. belong to Anacardiaceae pistache plant.Originate in China, it is very wide to distribute, and in China North China, all there is distribution on ground such as East China, Central-South, southwestern, south China, northwest, also there is natural distributed on ground such as the Philippines in South East Asia.The nearest Chinese pistache seed oil that studies show that can extract biofuel, and is significant to solving present energy dilemma, but the development and use of the grouts after its oil expression are rarely had report.And the current useful macromolecular substance of natural radioactivity that has been used as of many vegetable polysaccharidess is studied widely and is utilized, existing result of study shows, that polysaccharide has is anti-oxidant, antitumor, reducing blood-fat, improve a series of functionally activies such as body's immunity, if can find and extract the comprehensive utilization value that polysaccharide in the Chinese pistache will improve the processing and utilization of Chinese pistache seed greatly.
Summary of the invention
The object of the present invention is to provide a kind of polysaccharide that extracts from pistacia chinensis meal and extracting method thereof, this method is simply effective, and cost is low, and higher with the yield of this method extraction polysaccharide.
Realize that the object of the invention technical scheme is a kind of method of extracting polysaccharide from pistacia chinensis meal, the concrete steps that adopted are as follows:
(1) gets the pistacia chinensis meal raw material, by 1: 1-1: it is basic solution or the water that the strongly acidic solution of 0.01-7mol/L or weak acid that mass percent concentration is 0.01%-100% or concentration are 0.05-8.0mol/L that the solid-liquid ratio of 200g/ml adds concentration as extracting solution, be to take out after lixiviate 1min-8 hour under the 0-800r/m condition at 10-100 ℃ with stirring velocity then, through the centrifugation precipitation or after filtering, obtain removing the solution of post precipitation;
(2) in the solution of gained removal post precipitation, add the C that capacity can make polysaccharide precipitation 1-C 10Pure and mild C 1-C 10One or more admixture solvents in the ketone fully precipitate polysaccharide;
(3) precipitated liquid is carried out centrifugal or filtration treatment, remove solution wherein, with throw out for several times, be drying to obtain the Chinese pistache Crude polysaccharides with dehydrated alcohol, propyl alcohol or acetone repetitive scrubbing.
Preceding in step (1), earlier the raw material seed dregs of rice are carried out pre-treatment and remove impurity, the raw material grouts are carried out pre-treatment adopt following steps successively: pulverize, sieve, sherwood oil refluxes, and dries.
On the basis of technique scheme, in step (1), pistacia chinensis meal added extracting solution after in the process of lixiviate, make under the effect of microwave of its ultrasonic wave that is in 0-10000W power or 0-80000W power.
And wherein the strongly acidic solution as extracting solution comprises hydrochloric acid, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, primary ammonium phosphate or their mixed solution, when extracting solution is strong acid, with pistacia chinensis meal by 1: the concentration that the solid-liquid ratio of 1-1: 200g/ml adds as extracting solution is the strongly acidic solution of 0.01-7.0mol/L, is to take out after lixiviate 1min-8 hour under the 0-800r/m condition 10-100 ℃ and stirring velocity.
And wherein the weak acid as extracting solution comprises carboxylic acid, carboxylic acid anhydride, hydrogen peroxide or these sour mixed solutions, when extracting solution is weak acid, with pretreated pistacia chinensis meal, by 1: 1-1: the concentration that the solid-liquid ratio of 200g/ml adds as extracting solution is the weak acid of 0.01%-100%, is to take out after lixiviate 1min-8 hour under the 0-800r/m condition at 10-100 ℃ with stirring velocity then.
And wherein the basic solution as extracting solution comprises potassium hydroxide, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, S-WAT, sodium phytate or these alkali mixed solutions, when extracting solution is basic solution, with the pre-treatment dregs of rice, by 1: 1-1: the concentration that the solid-liquid ratio of 200g/ml adds as extracting solution is the alkali of 0.05-8.0mol/L, is to take out after lixiviate 1min-8 hour under the 0-800r/m condition at 10-100 ℃ with stirring velocity.
Wherein used centrifugal condition is 2000-15000r/m, 1-40 ℃.
Adopt existing sulfuric acid-phynol method that the material that extracts with technical scheme provided by the invention is carried out qualitative analysis, this material is a glucide as can be known, and sugar can be divided into monose and polysaccharide, adds in this extracting method in the pure sedimentary process monose to be removed, and what this explanation the present invention extracted is polysaccharide.With sulfuric acid-phynol method the polysaccharide that obtains is carried out assay, the concentration of extracting solution, extraction temperature, extraction time and these conditions of solid-liquid ratio are the most remarkable to the polysaccharide yield influence in this technical scheme as can be known.
The present invention adopts the solution extraction method as shown from the above technical solution, and as extracting solution, extraction conditions is simple and convenient, can improve the added value of the processing and utilization of Chinese pistache greatly with commonly used acid, alkali or water, industrial good popularization and application prospect is arranged.
Embodiment
The present invention at first carries out pre-treatment with the raw material pistacia chinensis meal, promptly pulverize successively, sieve, sherwood oil refluxes to remove granule foreign, remaining grease, dry standby, the raw material pistacia chinensis meal is carried out pre-treatment can make extraction effect better, tackle the raw material pistacia chinensis meal generally speaking and carry out pre-treatment; Then by 1: 1-1: the concentration that the solid-liquid ratio of 200g/ml adds as extracting solution is strongly acidic solution or the weak acid of 0.01%-100% or basic solution or the water that concentration is 0.05-8.0mol/L of 0.01-7.0mol/L, behind 10-100 ℃ and stirring velocity 0-800r/m lixiviate 1min-8h, take out then, after filtration or the centrifugation post precipitation, obtain removing the solution of post precipitation; In the solution of gained removal post precipitation, add the C that capacity can make polysaccharide precipitation 1-C 10Pure and mild C 1-C 10One or more admixture solvents in the ketone are (as common used ethanol, propyl alcohol or acetone etc., the concentration of solvent and consumption only need make the mass percentage content of solvent in the solution that adds behind the solvent reach more than 80%, can allow polysaccharide precipitation get final product), polysaccharide is fully precipitated; At last precipitated liquid is carried out centrifugal or filtration treatment, remove solution wherein, with dehydrated alcohol and acetone repetitive scrubbing several, lyophilize promptly obtains Crude polysaccharides.
Below the invention will be further described by specific embodiment.
Embodiment 1
It is the hydrochloric acid of 0.4mol/L that the pretreated pistacia chinensis meal of 1g is added 20ml concentration, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, in primary ammonium phosphate or its mixed solution, put into 90 ℃ of water-bath lixiviates, take out behind the lixiviate 2h, behind suction filtration, obtain filtrate; With alkali neutralization, in filtrate, sealing is placed to and precipitates fully to add 95% etoh solvent that can make polysaccharide precipitation (or propyl alcohol acetone etc.) by 1: 3 ratio again; At last with ethanol sedimentation liquid through 12000r/m, 4 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or propyl alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (example hydrochloric acid as extracting solution time yield be 6.24%) more than 3%.
Embodiment 2
It is the hydrochloric acid of 0.4mol/L that the pretreated pistacia chinensis meal of 1g is added 20ml concentration, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, in primary ammonium phosphate or its mixed solution, put into lixiviate under 80 ℃ of water-bath 80000W microwave conditions, take out behind the lixiviate 1min, behind suction filtration, obtain filtrate; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 2000r/m, 1 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or propyl alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (example hydrochloric acid as extracting solution time yield be 6.35%) more than 5%.
Embodiment 3
It is the hydrochloric acid of 7.0mol/L that the pretreated pistacia chinensis meal of 1g is added 20ml concentration, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, in primary ammonium phosphate or its mixed solution, put into lixiviate under 10 ℃ of water-bath 800r/m stirring velocitys, take out behind the lixiviate 60min, behind suction filtration, obtain filtrate; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 12000r/m, 4 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or propyl alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (example hydrochloric acid as extracting solution time yield be 5.16%) more than 3%.
Embodiment 4
It is the hydrochloric acid of 4mol/L that the pretreated pistacia chinensis meal of 1g is added 200ml concentration, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, in primary ammonium phosphate or its mixed solution, put into 80 ℃ of water-bath lixiviates, take out behind the lixiviate 8h, behind suction filtration, obtain filtrate; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 15000r/m, 40 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or propyl alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (example hydrochloric acid as extracting solution time yield be 8.04%) more than 5%.
Embodiment 5
It is the hydrochloric acid of 7.0mol/L that the pretreated pistacia chinensis meal of 1g is added 1ml concentration, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, in primary ammonium phosphate or its mixed solution, put into the lixiviate of 100 ℃ of water-bath 10000W ultrasonic wave, take out behind the lixiviate 30min, through 15000r/m, 40 ℃, behind the centrifugal 15min, pour out supernatant liquor; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 12000r/m, 40 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or propyl alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (example hydrochloric acid as extracting solution time yield be 7.85%) more than 5%.
Embodiment 6
It is the potassium hydroxide of 1.0mol/L that the pretreated pistacia chinensis meal of 1g is added 200ml concentration, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, S-WAT, sodium phytate or its mixed solution, extracting solution is a potassium hydroxide, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, in S-WAT or the sodium phytate, put into 10 ℃ of water-bath lixiviates, take out behind the lixiviate 8h, through 10000r/m, 4 ℃, behind the centrifugal 5min, pour out supernatant liquor; With acid neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 10000r/m, 1 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as sodium hydroxide as extracting solution time yield be 7.42%) more than 4%.
Embodiment 7
It is the potassium hydroxide of 8.0mol/L that the pretreated pistacia chinensis meal of 1g is added 10ml concentration, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, S-WAT, sodium phytate or its mixed solution, extracting solution is a potassium hydroxide, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, in S-WAT or the sodium phytate, put into the lixiviate of 100 ℃ of water-bath 10000W ultrasonic wave, take out behind the lixiviate 30min, through 10000r/m, 4 ℃, behind the centrifugal 5min, pour out supernatant liquor; With acid neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 10000r/m, 4 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol and acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as sodium hydroxide as extracting solution time yield be 7.57.%) more than 5%.
Embodiment 8
It is the potassium hydroxide of 1.5mol/L that the pretreated pistacia chinensis meal of 1g is added 1ml concentration, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, S-WAT, sodium phytate or its mixed solution, extracting solution is a potassium hydroxide, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, in S-WAT or the sodium phytate, put into the lixiviate of 70 ℃ of water-bath 80000W microwaves, take out behind the lixiviate 1min, through 10000r/m, 40 ℃, behind the centrifugal 5min, pour out supernatant liquor; With acid neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 2000r/m, 4 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as sodium hydroxide as extracting solution time yield be 6.67%) more than 4%.
Embodiment 9
It is the potassium hydroxide of 0.05mol/L that the pretreated pistacia chinensis meal of 1g is added 6ml concentration, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, S-WAT, sodium phytate or its mixed solution, extracting solution is a potassium hydroxide, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, saleratus, yellow soda ash, in S-WAT or the sodium phytate, put into 70 ℃ of water-bath lixiviates, take out behind the lixiviate 3h, through 10000r/m, 4 ℃, behind the centrifugal 5min, pour out supernatant liquor; With acid neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 15000r/m, 4 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as sodium hydroxide as extracting solution time yield be 5.96%) more than 4%.
Embodiment 10
The pretreated pistacia chinensis meal of 1g is added in the 200ml water, put into 10 ℃ of water lixiviates, take out behind the lixiviate 8h,, 1 ℃, behind the centrifugal 15min, pour out supernatant liquor through 2000r/m; Add 95% ethanol in supernatant liquor by 1: 3 volume ratio again, sealing is placed to precipitation fully; At last with ethanol sedimentation liquid through 2000r/m, 1 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measure through sulfuric acid-phynol method that polysaccharide yield is 2.56% under this condition.
Embodiment 11
The pretreated pistacia chinensis meal of 1g is added in the 1ml water, put into the lixiviate of 100 ℃ of water 80000W microwaves, take out behind the lixiviate 1min, after pumping rate, obtain filtrate; Add 95% ethanol in supernatant liquor by 1: 3 volume ratio again, sealing is placed to precipitation fully; At last with ethanol sedimentation liquid through 15000r/m, 40 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measure through sulfuric acid-phynol method that polysaccharide yield is 3.02% under this condition.
Embodiment 12
The pretreated pistacia chinensis meal of 1g is added in the 40ml water, take out after putting into 90 ℃ of water-bath 10000W ultrasonic wave lixiviate 4h, behind suction filtration, obtain filtrate; Add 95% ethanol in supernatant liquor in 1: 3 ratio again, sealing is placed to precipitation fully; At last with ethanol sedimentation liquid through 10000r/m, 4 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measure through sulfuric acid-phynol method that polysaccharide yield is 3.46% under this condition.
Embodiment 13
It is in 3% carboxylic acid, carboxylic acid anhydride or the hydrogen peroxide that the pretreated pistacia chinensis meal of 1g is added 200ml concentration, puts into 10 ℃ of water-bath lixiviates, takes out behind the lixiviate 8h, through 10000r/m, 1 ℃, behind the centrifugal 5min, pours out supernatant liquor; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 10000r/m, 1 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as acetate as extracting solution time yield be 6.45%) more than 4%.
Embodiment 14
It is in 0.01% carboxylic acid, carboxylic acid anhydride or the hydrogen peroxide that the pretreated pistacia chinensis meal of 1g is added 10ml concentration, puts into the lixiviate of 100 ℃ of water-bath 10000W ultrasonic wave, takes out behind the lixiviate 30min, through 10000r/m, 4 ℃, behind the centrifugal 5min, pours out supernatant liquor; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 10000r/m, 4 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol and acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as sodium hydroxide as extracting solution time yield be 5.23.%) more than 4%.
Embodiment 15
It is in 100% carboxylic acid, carboxylic acid anhydride or the hydrogen peroxide that the pretreated pistacia chinensis meal of 1g is added 1ml concentration, puts into the lixiviate of 50 ℃ of water-bath 80000W microwaves, takes out behind the lixiviate 1min, through 10000r/m, 40 ℃, behind the centrifugal 5min, pours out supernatant liquor; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 2000r/m, 40 ℃, behind the centrifugal 10min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as acetate as extracting solution time yield be 6.76%) more than 4%.
Embodiment 16
It is in 5% carboxylic acid, carboxylic acid anhydride or the hydrogen peroxide that the pretreated pistacia chinensis meal of 1g is added 6ml concentration, puts into 70 ℃ of water-bath lixiviates, takes out behind the lixiviate 3h, through 10000r/m, 4 ℃, behind the centrifugal 5min, pours out supernatant liquor; With alkali neutralization, add 95% ethanol in supernatant liquor by 1: 3 ratio again, sealing is placed to fully and precipitates; At last with ethanol sedimentation liquid through 15000r/m, 4 ℃, behind the centrifugal 15min, outwell top ethanol, with dehydrated alcohol or acetone repetitive scrubbing for several times, lyophilize promptly obtains Crude polysaccharides.Measuring under this condition polysaccharide yield through sulfuric acid-phynol method is (as acetate as extracting solution time yield be 5.53%) more than 4%.

Claims (7)

1. polysaccharide that extracts from pistacia chinensis meal is characterized in that adopting following steps to extract and get:
(1) gets the pistacia chinensis meal raw material, by 1: 1-1: it is basic solution or the water that the strongly acidic solution of 0.01-7.0mol/L or weak acid that mass percent concentration is 0.01%-100% or concentration are 0.05-8.0mol/L that the solid-liquid ratio of 200g/ml adds concentration as extracting solution, be that lixiviate is taken out after 1 minute-8 hours under the 0-800r/m condition at 10-100 ℃ with stirring velocity then, through the centrifugation precipitation or after filtering, obtain removing the solution of post precipitation, wherein the strongly acidic solution as extracting solution comprises hydrochloric acid, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, primary ammonium phosphate or their mixed solution, weak acid as extracting solution is carboxylic acid, comprises potassium hydroxide as the basic solution of extracting solution, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, S-WAT, the mixed solution of sodium phytate or these alkali;
(2) in the solution of gained removal post precipitation, add the solvent that capacity can make polysaccharide precipitation, polysaccharide is fully precipitated;
(3) precipitated liquid is carried out centrifugal or filtration treatment, remove solution and get throw out, with throw out for several times, be drying to obtain the Chinese pistache Crude polysaccharides with dehydrated alcohol, propyl alcohol or acetone repetitive scrubbing.
2. according to the described polysaccharide that extracts from pistacia chinensis meal of claim 1, it is characterized in that: the solvent of used precipitation polysaccharide is C 1-C 10Pure and mild C 1-C 10One or more mixtures in the ketone.
3. the extracting method of the described polysaccharide that extracts from pistacia chinensis meal of claim 1 is characterized in that adopting following concrete steps:
(1) gets the pistacia chinensis meal raw material, by 1: 1-1: it is basic solution or the water that the strongly acidic solution of 0.01-7.0mol/L or weak acid that mass percent concentration is 0.01%-100% or concentration are 0.05-8.0mol/L that the solid-liquid ratio of 200g/ml adds concentration as extracting solution, be that lixiviate is taken out after 1 minute-8 hours under the 0-800r/m condition at 10-100 ℃ with stirring velocity then, after filtration or after centrifugal, obtain removing the solution of post precipitation, wherein the strongly acidic solution as extracting solution comprises hydrochloric acid, perchloric acid, chloric acid, hypochlorous acid, hydrofluoric acid, nitric acid, nitrous acid, phosphoric acid, Hydrogen bromide, bromic acid, Periodic acid, sulfuric acid, sulfonic acid, sulfurous acid, boric acid, phytic acid, trichoroacetic acid(TCA), trifluoroacetic acid, sodium pyrosulfate, sal enixum, sodium hydrogen phosphate, SODIUM PHOSPHATE, MONOBASIC, potassium hydrogen phosphate, potassium primary phosphate, ammonium chloride, ammonium nitrate, ammonium sulfate, monoammonium sulfate, primary ammonium phosphate or their mixed solution, weak acid as extracting solution is carboxylic acid, comprises potassium hydroxide as the basic solution of extracting solution, sodium hydroxide, amine, carboxylic acid sodium, carboxylic acid potassium, potassium sulfonate, sodium sulfonate, tetra-alkyl ammonium hydroxide, ammoniacal liquor, saleratus, salt of wormwood, potassium sulfite, POTASSIUM PHYTATE, sodium bicarbonate, yellow soda ash, S-WAT, the mixed solution of sodium phytate or these alkali;
(2) in the solution of gained removal post precipitation, add the solvent that capacity can make polysaccharide precipitation, polysaccharide is fully precipitated;
(3) precipitated liquid is carried out centrifugal or filtration treatment, remove solution and get throw out, with throw out for several times, be drying to obtain Crude polysaccharides with dehydrated alcohol, propyl alcohol or acetone repetitive scrubbing.
4. according to the extracting method of the described polysaccharide that from pistacia chinensis meal, extracts of claim 3, it is characterized in that: preceding in step (1), earlier the raw material pistacia chinensis meal is carried out pre-treatment and remove impurity, the raw material pistacia chinensis meal is carried out pre-treatment adopt following steps successively: pulverize, sieve, sherwood oil refluxes, and dries.
5. according to the extracting method of the described polysaccharide that from pistacia chinensis meal, extracts of claim 3, it is characterized in that: in step (1), the pistacia chinensis meal raw material added in the process of lixiviate behind the extracting solution, make under the effect of microwave of its ultrasonic wave that is in 0-10000W power or 0-80000W power.
6. according to the extracting method of the described polysaccharide that extracts from pistacia chinensis meal of claim 3, it is characterized in that: the solvent of precipitation polysaccharide is C 1-C 10Pure and mild C 1-C 10One or more mixtures in the ketone.
7. according to the extracting method of the described polysaccharide that extracts from pistacia chinensis meal of claim 3, it is characterized in that: used centrifugal condition is 2000-15000r/m, 1-40 ℃.
CN2008100471165A 2008-03-21 2008-03-21 Polyoses extracted from pistacia chinensis meal and extracting method thereof Expired - Fee Related CN101245112B (en)

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