CN1307076A - Method for extracting natural edible pigment safflor yellow - Google Patents

Method for extracting natural edible pigment safflor yellow Download PDF

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CN1307076A
CN1307076A CN 00101467 CN00101467A CN1307076A CN 1307076 A CN1307076 A CN 1307076A CN 00101467 CN00101467 CN 00101467 CN 00101467 A CN00101467 A CN 00101467A CN 1307076 A CN1307076 A CN 1307076A
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liquid
effluent liquid
safflower
water
pillar
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CN1101424C (en
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沈生荣
徐月荣
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Zhejiang University ZJU
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Zhejiang University ZJU
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Abstract

The extraction includes the steps of: leaching filtering column chromatography water washing, alcohol elution, concentration for reclaiming alcohol, concentration and drying, and regenerating column. The advantages of the present invention are simple production process, low production cost, high product stability, high effective component yield of over 20%, high dry powder color value, good product flowability for easy componuding, no environmental pollution, high material utilization and easy use in industry.

Description

The new method for extracting of natural food colour sailor yellow
The present invention relates to a kind of new method for extracting of natural food colour sailor yellow.
Safflower is the dried floral of feverfew safflower (Cacthamus tinctorius L.), be the traditional promoting blood flow and remove blood stasis drug of the traditional Chinese medical science, effect with promoting blood circulation to restore menstrual flow, stasis-dispelling and pain-killing, utilizing safflower or contain the prescription of safflower, treatment coronary heart disease, acute cerebral thrombosis---plug is sick, vascular conditions and hepatitis etc. obtain satisfied curative effect.In one's early years, once there was the people that safflower was carried out some pharmacological research, as to the contraction in uterus, blood pressure drops effect etc.Recent years, round cardiovascular disease, carried out more work, find that safflower has the platelet aggregation effect that increase coronary flow, inhibition adenosine diphosphate (ADP) (ADP) and collagen cause, improves the ability of small white mouse hypoxia tolerance etc.
(Safflor Yellow is the effective ingredient of extracting from safflower SY) to carthamin yellow, has multiple pharmacology effects such as the hat of expansion, step-down, antithrombotic, hypoxia tolerance, immunosuppression; Simultaneously as a kind of edible natural pigment, have good tinting strength, characteristics such as stability have excellent development and application prospect preferably.
Chemical Composition to safflower since the seventies has carried out extensive studies, has isolated 200 multiple components, wherein mainly contains flavonoid, lignanoids, polyyne class etc., and majority studies have shown that the effective constituent that mainly contains of safflower is present in its water-soluble part.Carthamin yellow is the water soluble mixt that contains multiple effective ingredient, is mainly the phenyl styryl ketone based compound, and exemplary configuration is as follows:
Figure A0010146700041
Molecular formula is C 21H 22O 11, molecular weight is: 450.40
The main present-color material of carthamin yellow is sailor yellow and oxide compound thereof, also can contain the carbohydrate, salt and the protein that exist in the raw material.
It is the ideal natural pigment that carthamin yellow is used for food colorant, than food synthetic pigment characteristics such as beautiful in colour, Nai Gaore, high pressure resistant, low temperature resistant, fast light, acidproof, anti-reduction and anti-microorganism is arranged.The LD of carthamin yellow mouse stomach administration 50Be 5.53/Kg, and think the LD of safe edible synthesized coloring matter lemon yellow (Tartrazine) mouse stomach administration at present 50Be 6.09/Kg, compare no significant difference, all can think safe and reliable, sub-acute toxicity test, the LD of mouse peritoneal injection 50Be 9.41/Kg, prolonged and repeatedly take low dose of carthamin yellow, can not cause accumulate poisoning.
Up to now, the production technique of relevant carthamin yellow etc. had many research reports, and representational technology has following several:
1, room temperature flooding redness, diatomite helps filter, add an amount of 1, the 2-propylene glycol, pressure reducing and steaming moisture content, concentrated solution adds acetone, yellow mercury oxide, vacuum is drained, yellow loose powder, solid yield is near 20%.
2,65 ℃ with 60% ethanol lixiviate safflower 8 hours, and vat liquor concentrating under reduced pressure, concentrated solution add 95% ethanol makes pure content reach 85%, and low temperature spends the night, the elimination precipitation, and supernatant concentration is drying to obtain.
3, decoct safflower 2 times with suitable quantity of water, boil half an hour after boiling at every turn, decocting liquid filters, merging filtrate, and concentrating under reduced pressure adds 3 times of amount 95% ethanol sedimentation impurity, and filtrate recycling ethanol is drying to obtain.
4, extract a few hours with 60% ethanol secondary room temperature, concentrate and reclaim ethanol, concentrated solution is crossed macroporous adsorbent resin, certain density ethanol liquid wash-out, and stripping liquid reclaims ethanol, concentrates vacuum-drying.
Comprehensive above operational path, the subject matter of existence is:
1. production technique is complicated, and is not easy to operate, time-consuming;
2. production cost height, product stability is bad;
3. the effective ingredient yield is low, and dry powder look valency is done not high;
4. product is mobile poor, is difficult to preparation.
The new method for extracting that the purpose of this invention is to provide a kind of natural food colour sailor yellow.
In order to achieve the above object, take following measures:
The extraction step of natural food colour sailor yellow is as follows:
1. lixiviate: usefulness safflower and water 1: 12~18 (weight: volume), room temperature lixiviate 4~8 hours, filtered through gauze removes slag, and filtrate was placed after 0.5~1.5 hour, and inclining supernatant liquid; Filter residue uses 1: 6 again~and 8 (the safflower dry weight: volume of water) the room temperature lixiviate is 1~3 hour, operates the same clear liquid, goes up pillar after merging twice clear liquid;
2. filter: the filter cloth aperture of adopting during filtration can not be too little, and 40~60 orders get final product, and is separated into suitablely with safflower and residue, and residue should be squeezed to dried;
3. upper prop: post specification: 75cm * φ 2.5cm is a column length and the ratio of interior warp is 30: 1;
Resin demand: 300ml;
Applied sample amount: 2500~3000ml, resin absorption reaches capacity and is best applied sample amount;
Last sample flow velocity: 20~25ml/min;
It is long-pending to abandon liquid: going up behind the sample at first, effluent liquid 800~1200ml discards all the other collections;
4. washing: after going up sample and finishing, water cleans pillar, and effluent liquid is collected, and can be used for safflower lixiviate or upper prop again, and washing is half of applied sample amount with volume, and is faint yellow only to effluent liquid;
5. alcohol takes off: it is 50~60% that alcohol takes off liquid concentration, and pure lift-off amasss 2000~2500ml, discards preceding 150~250ml effluent liquid, and elution speed is about 7~8ml/min, collects effluent liquid 1800~2300ml, needs 4~6 hours approximately;
6. concentrate and reclaim ethanol: 40~55 ℃ of following vacuum reclaim ethanol in the effluent liquid, get brown liquid;
7. concentrate and drying: 40~55 ℃ are continued vacuum concentration down to 1/8~1/12 of original volume, move into 50 ℃ of following vacuum-dryings in the vacuum drying oven;
8. finished product: finished product should be pale brown toner end, and easily the moisture absorption is brown, and forms bulk during the moisture absorption, and the product after the moisture absorption does not influence result of use, and yield should be greater than 20%, dry powder look valency P ( 1 cm 1 % ) ≥ 180
9. pillar regeneration: the pillar water after alcohol takes off washes to effluent liquid is slightly faint yellow or colourless and ends, and there is no pure smell, and then goes up sample and reuse.
Advantage of the present invention is:
1. production technique is simple and direct, easy to operate;
2. production cost is low, and product stability is good;
3. effective ingredient yield height (>20%), dry powder look valency height ( P 1 cm 1 % > 180 );
4. good product mobility, very easily preparation;
5. non-environmental-pollution and raw material availability height are promoted easily in batch production.
Elaborate below in conjunction with embodiment:
Embodiment 1
The extraction step of carthamin yellow is as follows:
1. lixiviate: with safflower and water 1: 12 (weight: volume), room temperature lixiviate 4 hours, filtered through gauze removes slag, the filtrate placement is after 0.5 hour, inclining supernatant liquid (removing throw out); Filter residue is used 1: 6 again, and (the safflower dry weight: volume of water) the room temperature lixiviate was operated the same clear liquid that gets more than 1 hour.Go up pillar after merging twice clear liquid, the residue after the secondary lixiviate can be used for other utilization.Crucial GPRS diffusion water amount and extraction time, otherwise influence yield.In addition, throw out should be accomplished most, otherwise influences the life-span of flow velocity and pillar, and prolongs flush time.
2. filter: the filter cloth aperture of adopting during filtration can not be too little, and 40~60 orders get final product, and is separated into suitablely with safflower and residue, and residue should be squeezed to dried.
3. upper prop: post specification: 75cm * φ 2.5cm is a column length and the ratio of internal diameter is 30: 1;
Resin demand: 300ml (resin uses preceding in strict accordance with the resin that dispatches from the factory pre-treatment standard operation) JAD-1 type (produce in the 3rd chemical plant, Jiangdu, Jiangsu, and particular design is one of key link of this patent);
Applied sample amount: 2500~3000ml, resin absorption reaches capacity and is best applied sample amount;
Last sample flow velocity: 20~25ml/min (natural drop, standard-sized sheet are put to flow automatically and be advisable);
It is long-pending to abandon liquid: going up behind the sample at first, effluent liquid 800ml discards (erosion of mixing is arranged), all the other collections.
4. washing: after going up sample and finishing, water cleans pillar, and effluent liquid is collected, and can be used for safflower lixiviate or upper prop again, and washing is half of applied sample amount with volume, to effluent liquid faint yellow only (can suitably discard a last part according to the effluent liquid color and luster).
5. alcohol takes off: it is 50% that alcohol takes off liquid concentration, and pure lift-off amasss 2000ml, 150ml effluent liquid before discarding, and elution speed is about 7ml/min, collects effluent liquid 1800ml, needs 4 hours approximately (being washed till effluent liquid is faint yellow ending).This segment process is wanted the strict determining alcohol of grasping.
6. concentrate and reclaim ethanol: 40 ℃ of following vacuum reclaim ethanol in the effluent liquid, get brown liquid.
7. concentrate and drying: 40 ℃ are continued vacuum concentration down to 1/8 of original volume, move into 40 ℃ of following vacuum-dryings in the vacuum drying oven.Attention: a: concentrating can not be excessive, otherwise mobile variation, unfavorable operation and influence quality product; B: concentrate with drying temperature and answer strictness to be lower than 60 ℃.
8. finished product: finished product should be pale brown toner end, and easily the moisture absorption is brown, and forms bulk during the moisture absorption.Product after the moisture absorption does not influence result of use, and yield should be greater than 20%, dry powder look valency P ( 1 cm 1 % ) ≥ 180
9. pillar regeneration: the pillar water after alcohol takes off washes to effluent liquid is slightly faint yellow or colourless and ends, and there is no pure smell, about 1000ml, and then go up sample and reuse.
Embodiment 2
The brightly yellowish extraction step of color red is as follows:
1. lixiviate: with safflower and water 1: 15 (weight: volume), room temperature lixiviate 6 hours, filtered through gauze removes slag, the filtrate placement is after 1 hour, inclining supernatant liquid; Filter residue uses room temperature lixiviate in 1: 7 more than 2 hours again, operates the same clear liquid, goes up pillar after merging twice clear liquid;
2. filter: the filter cloth aperture of adopting during filtration can not be too little, and 40~60 orders get final product, and is separated into suitablely with safflower and residue, and residue should be squeezed to dried;
3. upper prop: post specification: 75cm * φ 2.5cm is a column length and the ratio of internal diameter is 30: 1;
Resin demand: 300ml;
Applied sample amount: 2500~3000ml, resin absorption reaches capacity and is best applied sample amount;
Last sample flow velocity: 20~25ml/min;
It is long-pending to abandon liquid: going up behind the sample at first, effluent liquid 1000ml discards all the other collections;
4. washing: after going up sample and finishing, water cleans pillar, and effluent liquid is collected, and can be used for safflower lixiviate or upper prop again, and washing is half of applied sample amount with volume, and is faint yellow only to effluent liquid;
5. alcohol takes off: it is 55% that alcohol takes off liquid concentration, and pure lift-off amasss 2250ml, 200ml effluent liquid before discarding, and elution speed is about 7.5ml/min, collects effluent liquid 2000ml, needs 5 hours approximately (being washed till effluent liquid is faint yellow ending);
6. concentrate and reclaim ethanol: 50 ℃ of following vacuum reclaim ethanol in the effluent liquid, get brown liquid;
7. concentrate and drying: 50 ℃ are continued vacuum concentration down to 1/10 of original volume, move into 50 ℃ of following vacuum-dryings in the vacuum drying oven;
8. finished product: finished product should be pale brown toner end, and easily the moisture absorption is brown, and forms bulk during the moisture absorption.Product after the moisture absorption does not influence result of use, and yield should be greater than 20%, dry powder look valency P ( 1 cm 1 % ) ≥ 180
9. pillar regeneration: the pillar water after alcohol takes off washes to effluent liquid is slightly faint yellow or colourless and ends, and there is no pure smell, about 1000ml, and then go up sample and reuse.
Embodiment 3
The extraction step of carthamin yellow is as follows:
1. lixiviate: with safflower and water 1: 18 (weight: volume), room temperature lixiviate 8 hours, filtered through gauze removes slag, the filtrate placement is after 1.5 hours, inclining supernatant liquid (removing throw out); Filter residue is used 1: 8 again, and (the safflower dry weight: volume of water) the room temperature lixiviate is 1~3 hour, operates the same clear liquid that gets.Go up pillar after merging twice clear liquid, the residue after the secondary lixiviate can be used for other utilization.Crucial GPRS diffusion water amount and extraction time, otherwise influence yield.In addition, throw out should be accomplished most, otherwise influences the life-span of flow velocity and pillar, and prolongs flush time.
2. filter: the filter cloth aperture of adopting during filtration can not be too little, and 40~60 orders get final product, and is separated into suitablely with safflower and residue, and residue should be squeezed to dried.
3. upper prop: post specification: 75cm * φ 2.5cm is a column length and the ratio of internal diameter is 30: 1;
Resin demand: 300ml (resin uses preceding in strict accordance with the resin that dispatches from the factory pre-treatment standard operation) JAD-I type (produce in the 3rd chemical plant, Jiangdu, Jiangsu, and particular design is one of key link of this patent);
Applied sample amount: 2500~3000ml, resin absorption reaches capacity and is best applied sample amount;
Last sample flow velocity: 20~25ml/min (natural drop, standard-sized sheet are put to flow automatically and be advisable);
It is long-pending to abandon liquid: going up behind the sample at first, effluent liquid 1200ml discards (erosion of mixing is arranged), all the other collections.
4. washing: after going up sample and finishing, water cleans pillar, and effluent liquid is collected, and can be used for safflower lixiviate or upper prop again, and washing is half of applied sample amount with volume, to effluent liquid faint yellow only (can suitably discard a last part according to the effluent liquid color and luster).
5. alcohol takes off: it is 60% that alcohol takes off liquid concentration, and pure lift-off amasss 2500ml, 250ml effluent liquid before discarding, and elution speed is about 8ml/min, collects effluent liquid 2300ml, needs 6 hours approximately (being washed till effluent liquid is faint yellow ending).This segment process is wanted the strict determining alcohol of grasping.
6. concentrate and reclaim ethanol: 55 ℃ of following vacuum reclaim ethanol in the effluent liquid, and temperature should not surpass 60 ℃, gets brown liquid.
7. concentrate and drying: 55 ℃ are continued vacuum concentration down to 1/12 of original volume, move into 55 ℃ of following vacuum-dryings in the vacuum drying oven.Attention: a: concentrating can not be excessive, otherwise mobile variation, unfavorable operation and influence quality product; B: concentrate with drying temperature and answer strictness to be lower than 60 ℃.
8. finished product: finished product should be pale brown toner end, and easily the moisture absorption is brown, and forms bulk during the moisture absorption.Product after the moisture absorption does not influence result of use, and yield should be greater than 20%, dry powder look valency P ( 1 cm 1 % ) ≥ 180
9. pillar regeneration: the pillar water after alcohol takes off washes to effluent liquid is slightly faint yellow or colourless and ends, and there is no pure smell, about 1000ml, and then go up sample and reuse.
The carthamin yellow mass analysis:
(1) ignition residue (being ash content)
The 3g (accurately claiming to 0.0002g) that materialses places at the porcelain crucible of 700~800 ℃ of following constant weights, first low-temperature carbonization (300 ℃), and high temperature ashing again (about 500 ℃) moves into to cover and inspires confidence in the stove (high-temperature electric resistance furnace) 700~800 ℃ of following calcinations to constant weight.Product ash content≤14% under these processing condition.
(2) heavy metal (in lead)
1. the preparation of the test liquid 5g (claim accurate to 0.01g) that materialses is put in the kjeldahl flask, adds three of granulated glass spherees and nitric acid 10ml, slowly adds sulfuric acid 5ml then carefully.After question response relaxes, carefully be heated to when liquid begins to turn brown in the bottle, drip nitric acid to organism one by one and decompose fully, elevated temperature again, till the white cigarette of sulphur trioxide took place, this moment, solution should colourless or little band yellow-green colour.Brown as temperature rising back solution becomes, it is organic to add the broken ring of nitric acid again.Put coldly, carefully add water 10ml, boil, drive remaining nitric acid away, to bottle, the white cigarette of sulphur trioxide takes place.If desired, then can repeat several, become water white transparency until liquid and end to remove remaining nitric acid.Put coldly, carefully solution is diluted with less water, change in the 50ml volumetric flask, with not washing kjeldahl flask for several times, washing lotion is incorporated in the volumetric flask, and cooling adds water to scale, shakes up.
2. 10% potassium cyanide solution 20ml is got in the preparation of potassium cyanide-ammonia water mixture, places the 150ml beaker, adds ammoniacal liquor 75ml, is diluted with water to 100ml.
3. typical curve is plotted in 6 separating funnels, respectively add 1% salpeter solution 20ml, potassium cyanide-ammonia water mixture 4ml, extract once with 5mg/100ml dithizone-trichloromethane liquid respectively, discard the trichloromethane layer, with the residual dithizone of a small amount of trichloromethane flush away row, until the trichloromethane liquid layer is colourless, order adds plumbous reference liquid (1 μ l/ml) 0.0 then, 1.0,3.0,5.0,7.0,9.0ml in 6 separating funnels, use the one trichloromethane liquid 10ml extracting of 1mg/100ml dithizone respectively once, jolting 1min, tell the trichloromethane liquid layer and place the 2cm cuvette, surveying its absorbancy with spectrophotometer in 510nm wavelength place, is zero point with the reagent blank, the drawing standard curve.
4. measure formality and accurately draw said sample liquid 10ml, place the 125ml separating funnel, add 20% diammonium hydrogen citrate solution 15ml, 20% oxammonium hydrochloride solution 1ml and 0.1% thymolsulfonphthalein test solution (TS-247) 2-4 drips, adding ammoniacal liquor to solution again is blue-greenish colour, add 10% potassium cyanide solution 5ml, regulating with 10% hydrochloric acid soln becomes grass green (this moment, pH was about 9) again, with 5mg/100ml dithizone-trichloromethane liquid 2-3ml extracting for several times, and till to the last single extraction liquid still is green.Merge extract, wash with the jolting of 15ml water, tell the trichloromethane liquid layer in second separating funnel, washing water are used 5mf/100ml pair, and thin hydrazone-trichloromethane liquid 2-3ml extracting once, telling the trichloromethane liquid layer incorporates in second separating funnel, with 1% salpeter solution 20ml, each 10ml, sieve is got secondary, discard the trichloromethane liquid layer, merge nitric acid extraction liquid in another separating funnel, with a small amount of trichloromethane 3-5ml washing acid solution, to the trichloromethane liquid layer is colourless, to remove residual trichloromethane liquid, then rotate funnel and be sunken to back, bottom branch by it, add potassium cyanide-ammonia water mixture 4ml then, 1mg/100ml dithizone-trichloromethane liquid 10ml, jolting 1min, standing demix is cleaned funnel exit with absorbent cotton, telling trichloromethane liquid layer drying absorbent cotton filters, discard filtrate just, collect filtrate in the 2cm cuvette, survey its absorbancy in 510nm wavelength place with spectrophotometer, with measurement result and the contrast of plumbous typical curve, check in lead content, draw simultaneously with same reagent blank liquid 10ml and the sample of handling of sample and operate simultaneously, and in coupon results, deduct institute's sounding lead content in the blank.
In addition, also available atomic absorption spectrophotometer method test, concrete steps can be consulted relevant document.Product heavy metal content≤50ppm under this technology.
(3) arsenic:
1. arsenic reference liquid (1 μ l/ml is accurately drawn in the drafting of typical curve; Referring to TS-34) 0.0,0.5,1.0,2.0,3.0ml, place the hydrogen arsenide producer respectively, respectively adding water, to make its cumulative volume be 40ml, add 1: 1 sulphuric acid soln 10ml, 15% liquor kalii iodide 1ml, 40% stannous chloride solution 2ml, mixing adds arsenic-less metal zinc 3g, the airway of lead acetate cotton is housed rapidly beyond the Great Wall, and the ozzle of airway inserted fill in the graduated cylinder of 5ml silver salt solution, treat that gas takes place to shake the hydrogen arsenide producer behind the 20min, took out airway after 20 minutes, as the not enough 5ml of solution in the graduated cylinder, the application silver salt solution is supplied, and this liquid is moved in the 1cm cuvette, surveys its absorbancy with spectrophotometer in 540nm wavelength place.With the reagent blank is zero point, the drawing standard curve.
2. the test liquid 10ml in the above-mentioned lead test of the accurate absorption of determination step is in the hydrogen arsenide producer, control is equipped with described in the typical curve from " adding water to 40ml " then, survey its absorbancy with spectrophotometer in 540nm wavelength place equally, with measurement result and the contrast of arsenic typical curve, check in arsenic content, draw and the simultaneously treated reagent blank liquid of sample 10ml simultaneously, operate simultaneously with sample, and in the result, deduct arsenic content measured in the blank.Product arsenic content≤2ppm under these processing condition.
(4) sanitary index:
With 60 look valency carthamin yellows is material (containing 15% ethanol), presses the measuring method of sanitary index, and the product sanitary index that gets this technology is as follows:
1. total plate count :≤1000U/g
2. fungi count :≤100U/g
3. intestinal bacteria: do not detect
(5) look valency:
Accurately taking by weighing sample 0.10g (dry powder) or liquid is about 0.20~0.30g, moves in the 100ml volumetric flask, uses the distilled water constant volume.Getting this 5ml and move in the 100ml volumetric flask, use the distilled water constant volume, measure absorbance A with the 1cm cuvette under 403nm, is blank with distilled water, calculates look valency P as follows:
Figure A0010146700111
Not in 0.2~0.7 scope, should readjust sample size as absorbance A.The look valency of product under these processing condition: dry powder look valency P ( 1 cm 1 % ) ≥ 180 About.
(6) absorbancy ratio:
Under wavelength 360nm, 400nm, measure absorbance A respectively with above-mentioned color solution and calculate A 400/ A 360Value gets final product.Product absorbance ratio under these processing condition is about 1.30.
(7) pH value:
Recording above-mentioned colorimetric with pH meter is 4.0~6.0 with the pH value of sample liquid.
(8) solvability:
Accurately take by weighing the 0.15g sample, with dissolved in distilled water and be settled to 50ml, measure the transmittance of color solution greater than 85% at wavelength 650nm with the 1cm cuvette.
(9) yield:
By 60 look valencys, yield>20%.
(10) uv-vis spectra of product:
With above-mentioned colorimetric sample liquid, (scope 250~550nm) gets spectrum, all has absorption peak to occur about 403nm and 360nm in Beckman DU-640 type UV, visible light scanner scanning.
(11) moisture of dry powder (weight loss on drying):
105 ℃ of constant weight methods record smaller or equal to 3%.
(12) product performance:
230 ℃ of fusing points, photostabilization is good, and tone is stable in pH value 5~7 scopes; To thermally-stabilised.Dyeability to starch is good, and is relatively poor to proteinic dyeability, and iron ion can make its blackout, Ca 2+, Sn 2+, Mg 2+, Cu 2+, Al 3+Plasma does not almost have influence.(alkalescence or acid) soluble in water, hot water, Diluted Alcohol, rare propylene glycol are dissolved in dehydrated alcohol hardly, are insoluble to ether, sherwood oil, grease and acetone etc.
The raw material detection method
Take by weighing the dry safflower of 10g, add water 150ml, room temperature lixiviate 3 hours is filtered, it is centrifugal that (10000rpm 10min) removes slag, and gets supernatant liquor 1ml, be diluted with water to 100ml, under 403nm, record the absorbance A of safflower vat liquor, calculate look valency P as follows with the 1cm cuvette: The P value that raw material records by this method should be more than or equal to 7.5.

Claims (2)

1. the new method for extracting of a natural food colour sailor yellow is characterized in that its extraction step is as follows:
1. lixiviate: usefulness safflower and water 1: 12~18 (weight: volume), room temperature lixiviate 4~8 hours, filtered through gauze removes slag, and filtrate was placed after 0.5~1.5 hour, and inclining supernatant liquid; Filter residue uses 1: 6 again~8 (the safflower dry weight: volume of water) room temperature lixiviate more than 1~3 hour, operate the same clear liquid, go up pillar after merging twice clear liquid;
2. filter: the filter cloth aperture of adopting during filtration can not be too little, and 40~60 orders get final product, and is separated into suitablely with safflower and residue, and residue should be squeezed to dried;
3. upper prop: post specification: 75cm * φ 2.5cm is a column length and the ratio of internal diameter is 30: 1;
Resin demand: 300ml;
Applied sample amount: 2500~3000ml, resin absorption reaches capacity and is best applied sample amount;
Last sample flow velocity: 20~25ml/min;
It is long-pending to abandon liquid: going up behind the sample at first, effluent liquid 800~1200ml discards all the other collections;
4. washing: after going up sample and finishing, water cleans pillar, and effluent liquid is collected, and can be used for safflower lixiviate or upper prop again, and washing is half of applied sample amount with volume, and is faint yellow only to effluent liquid;
5. alcohol takes off: it is 50~60% that alcohol takes off liquid concentration, and pure lift-off amasss 2000~2500ml, discards preceding 150~250ml effluent liquid, and elution speed is about 7~8ml/min, collects effluent liquid 1800~2300ml, needs 4~6 hours approximately;
6. concentrate and reclaim ethanol: 40~55 ℃ of following vacuum reclaim ethanol in the effluent liquid, get brown liquid;
7. concentrate and drying: 40~55 ℃ are continued vacuum concentration down to 1/8~1/12 of original volume, move into 40~55 ℃ of following vacuum-dryings in the vacuum drying oven;
8. finished product: finished product should be pale brown toner end, and easily the moisture absorption is brown, and forms bulk during the moisture absorption, and the product after the moisture absorption does not influence result of use, and yield should be greater than 20%, dry powder look valency P ( 1 cm 1 % ) ≥ 180
9. pillar regeneration: the pillar water after alcohol takes off washes to effluent liquid is slightly faint yellow or colourless and ends, and there is no pure smell, and then goes up sample and reuse.
2. the new method for extracting of a kind of natural food colour sailor yellow according to claim 1 is characterized in that its extraction step is as follows:
1. lixiviate: with safflower and water 1: 15 (weight: volume), room temperature lixiviate 6 hours, filtered through gauze removes slag, the filtrate placement is after 1 hour, inclining supernatant liquid; Filter residue use 1: 7 again (the safflower dry weight: volume of water) room temperature lixiviate more than 2 hours, operate the same clear liquid, go up pillar after merging twice clear liquid;
2. filter: the filter cloth aperture of adopting during filtration can not be too little, and 40~60 orders get final product, and is separated into suitablely with safflower and residue, and residue should be squeezed to dried;
3. upper prop: post specification: 75cm * φ 2.5cm is a column length and the ratio of internal diameter is 30: 1;
Resin demand: 300ml;
Applied sample amount: 2500~3000ml, resin absorption reaches capacity and is best applied sample amount;
Last sample flow velocity: 20~25ml/min;
It is long-pending to abandon liquid: going up behind the sample at first, effluent liquid 1000ml discards all the other collections;
4. washing: after going up sample and finishing, water cleans pillar, and effluent liquid is collected, and can be used for safflower lixiviate or upper prop again, and washing is half of applied sample amount with volume, and is faint yellow only to effluent liquid;
5. alcohol takes off: it is 55% that alcohol takes off liquid concentration, and pure lift-off amasss 2250ml, 200ml effluent liquid before discarding, and elution speed is about 7.5ml/min, collects effluent liquid 2000ml, needs 5 hours approximately (being washed till effluent liquid is faint yellow ending);
6. concentrate and reclaim ethanol: 50 ℃ of following vacuum reclaim ethanol in the effluent liquid, get brown liquid;
7. concentrate and drying: 50 ℃ are continued vacuum concentration down to 1/10 of original volume, move into 50 ℃ of following vacuum-dryings in the vacuum drying oven;
8. finished product: finished product should be pale brown toner end, and easily the moisture absorption is brown, and forms bulk during the moisture absorption.Product after the moisture absorption does not influence result of use, and yield should be greater than 20%, dry powder look valency P ( 1 cm 1 % ) ≥ 180
9. pillar regeneration: the pillar water after alcohol takes off washes to effluent liquid is slightly faint yellow or colourless and ends, and there is no pure smell, and then goes up sample and reuse.
CN00101467A 2000-01-21 2000-01-21 Method for extracting natural edible pigment safflor yellow Expired - Fee Related CN1101424C (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1935176B (en) * 2005-09-23 2010-07-14 北京星昊医药股份有限公司 Method for preparing red flower extract containing total red flower uranidin
CN102031013A (en) * 2010-11-12 2011-04-27 合肥工业大学 Method for extracting brown pigment from lotus receptacle
CN101774989B (en) * 2009-02-04 2011-07-27 王来忠 Method for extracting refined yellow pigment from red flowers
CN102660139A (en) * 2012-05-18 2012-09-12 江西国亿生物科技有限公司 Preparation of high-quality arthamin yellow

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3410610B2 (en) * 1996-03-04 2003-05-26 東洋インキ製造株式会社 Separation method of safflower yellow pigment and sugar from safflower extract

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1935176B (en) * 2005-09-23 2010-07-14 北京星昊医药股份有限公司 Method for preparing red flower extract containing total red flower uranidin
CN101774989B (en) * 2009-02-04 2011-07-27 王来忠 Method for extracting refined yellow pigment from red flowers
CN102031013A (en) * 2010-11-12 2011-04-27 合肥工业大学 Method for extracting brown pigment from lotus receptacle
CN102660139A (en) * 2012-05-18 2012-09-12 江西国亿生物科技有限公司 Preparation of high-quality arthamin yellow
CN102660139B (en) * 2012-05-18 2013-09-11 江西国亿生物科技有限公司 Preparation of high-quality arthamin yellow

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