CN1528193A - Method for black rice haematochrome from black rice bran - Google Patents

Method for black rice haematochrome from black rice bran Download PDF

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Publication number
CN1528193A
CN1528193A CNA2003101048565A CN200310104856A CN1528193A CN 1528193 A CN1528193 A CN 1528193A CN A2003101048565 A CNA2003101048565 A CN A2003101048565A CN 200310104856 A CN200310104856 A CN 200310104856A CN 1528193 A CN1528193 A CN 1528193A
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alcohol
black rice
temperature
lixiviate
hours
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Chinese (zh)
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朱蓓薇
董秀萍
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Dalian Polytechnic University
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Dalian Institute of Light Industry
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Priority to CNA2003101048565A priority Critical patent/CN1528193A/en
Publication of CN1528193A publication Critical patent/CN1528193A/en
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  • Coloring Foods And Improving Nutritive Qualities (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The present invention relates to a method for extracting black rice red colour matter from black rice bran. Said method includes the following steps: using black rice bran as raw material, mixing it with edible alcohol accoridng to a certain proportion, pickling at a certain temp., perfectly making zymohydrolysis extraction, and making the mixed extract pass through kieselguhr filter to make treatment, then vacuum concentrating and recovering alcohol, the concentrate is coarse colour matter liquor, making the coarse colour matter liquor pass through NKA macroporous adsorption resin to make purification, successively using water and alcohol to make elution, collecting alcohol eluent, vacuum concentrating and recovering alcohol to obtain high-purity colour matter liquor, concentrating said colour matter liquor, spray-drying and collecting under the sterile condition so as to obtain the invented finished product.

Description

The preparation method of natural edible pigment in the black rice chaff
Technical field the present invention relates to a kind of preparation method of food coloring product.
Background technology it is found that along with the deep development of medical science toxicology and biological study the metabolite of synthetic food color in human body that once allows to use has carcinogenesis, therefore uses to be restricted.Natural colouring matter is because safe, painted natural and self nutrition and pharmacological action replaces the application of synthetic food color just gradually.In recent years, the research of extracting natural edible pigment from black rice was more, but the extraction process imperfection, the look valency is not high, and quality is unsatisfactory.
It is raw material with the black rice chaff that summary of the invention the object of the invention is to provide a kind of, through extracting and purifying obtains the preparation method of high luminance relay valency, high-quality natural edible pigment.
The present invention mainly is achieved through the following technical solutions: comprise raw material processing, lixiviate, filtration, absorption, wash-out, concentrate, step such as spray-drying, specific as follows:
One, raw material lixiviate
1, a lixiviate
(the weight kilogram: the volume liter) carry out lixiviate in aseptic jar, alcohol concentration was 0~95%, and extraction temperature is 15~70 ℃, and extraction time is 1~14 hour, and the pH value is 2~6 by 1: 3~1: 9 with black rice chaff and alcohol.
2, secondary lixiviate
(the weight kilogram: the volume liter) carry out lixiviate in aseptic jar, alcohol concentration was 0~95%, and extraction temperature is 30~80 ℃, and extraction time is 2~10 hours, and the pH value is 2~6 by 1: 3~1: 9 with black rice chaff residue and alcohol after the lixiviate.
3, three lixiviates
The ferment of black rice chaff residue adding 0.02~0.1% after the secondary lixiviate is carried out glycolysis, and temperature is 30~60 ℃, and the time is 0.5~2 hour.And then with alcohol (the weight kilogram: the volume liter) carry out lixiviate, alcohol concentration was 0~95%, and extraction temperature is 30~80 ℃, and extraction time is 2~10 hours, and the pH value is 2~6 by 1: 3~1: 9.
The allotment of above-mentioned leaching liquor pH value: 1. can adopt Vc and different Vc-Na compound;
Or 2. adopt citric acid, natrium citricum and V cCompound;
Or 3. adopt hydrochloric acid and citric acid compound
Two, filter
1, coarse filtration: extract is put hold-up tank room temperature cooling precipitation 7~12 hours into.
2, smart filter: said extracted liquid passes through diatomaceous earth filter.
3, vacuum concentrates: recovered alcohol is soft to the extract.
Three, purifying
1, absorption: above-mentioned concentrate cleans repeatedly with distilled water by NKA macroporous absorbent resin adsorpting pigment again, removes impurity, abandons liquid.
2, wash-out: be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 40~90% edible alcohol wash-outs, collect and flow out liquid.
Four, drying
1, concentrate: above-mentioned filtrate is carried out vacuum, and to be concentrated into concentration be 15~18%.
2, spray-drying: with adding ferment by 0.1 ‰~0.7 ‰ in the pigment concentrate, make the starch degradation that contains in the concentrate, under 60~85 ℃ of temperature, be incubated 1.5~3 hours, carry out spray-drying then.Dry concrete operations condition is as follows: the concentrate temperature is 55~80 ℃; 125~135 ℃ of EATs, 105~115 ℃ of tower temperature
The present invention has following advantage compared to existing technology:
1. product of the present invention be with countries in the world extensively the accessory substance rice bran of the black rice of plantation be raw material, sufficient raw, cheap;
2. adopt compound extraction, promptly carry out twice acid lixiviate, an enzyme process lixiviate obviously improves the recovery rate of pigment on the one hand, and the pigment residual volume is few in the residue; The digestion agent consumption is few on the other hand, and cost is low, the comprehensive utilization ratio height;
3. adopt Vc and different Vc-Na compound (or citric acid, natrium citricum and Vc is compound; Or hydrochloric acid and citric acid is compound), regulate the leaching liquor pH value, the acid leaching liquor character of gained gentleness, and extraction efficiency is very high;
4. the NKA macroporous absorbent resin is applied to actual production, the natural edible pigment that obtains, look valency E " 100 1% 1cm, product purity is higher than the national standard of existing haematochrome far away.Not only beautiful in colour, and certain medicinal efficacy is arranged, be a kind of natural food colour resource that medical value is arranged;
5. product is a kind of nontoxic, harmless, tasteless natural colouring matter, and its tone can change with the difference of pH value, and acidity is red, and neutrality is baby pink, and alkalescence is that reddish violet is to bluish violet;
6. extracting method is comparatively easy, and technological process is short, and equipment needed thereby is few, and specification requirement is low, and work efficiency height and consuming little energy are free from environmental pollution in the production process;
7. this product purpose is wide, both can be used for the toning of beverage, cold drink and drinks, also can be used for the additive of foodstuffs such as cold cuts class, jam, cakes such as candy class, ham sausage and toiletries, and cost is low, the economic benefit height.The small investment instant effect, big, medium-sized and small enterprises all can go into operation.
The specific embodiment
Example 1
100 kilograms of black rice chaffs and 300 liters of alcohol are carried out lixiviate in aseptic jar, alcohol concentration is 95%, and extraction temperature is 15 ℃, and extraction time is 1 hour, and adding Vc and different Vc-Na adjust pH is 6.Black rice chaff residue and alcohol after the lixiviate are carried out lixiviate for 300 liters in aseptic jar, alcohol concentration is 95%, and extraction temperature is 30 ℃, and extraction time is 2 hours, and adding Vc and different Vc-Na adjusting pH value is 6.The ferment that black rice chaff residue after the secondary lixiviate is added 20 grams carries out glycolysis, and temperature is 30 ℃, and the time is 2 hours.Carry out lixiviate with 300 liters of alcohol in aseptic jar then, alcohol concentration is 95%, and extraction temperature is 30 ℃, and extraction time is 2 hours, and adding Vc and different Vc-Na adjusting pH value is 6.Put No. three extracts into hold-up tank room temperature cooling precipitation 12 hours as coarse filtration, the coarse filtration liquid that obtains is by the smart filter of diatomaceous earth filter, and to concentrate recovered alcohol soft to the extract for vacuum then.Filtered fluid after concentrating repeatedly cleans with distilled water by NKA macroporous absorbent resin adsorpting pigment again, removes impurity.Be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 40% edible alcohol wash-out then, collect and flow out liquid, obtain the natural edible pigment solution behind the purifying.It is 50 liters that its vacuum is concentrated into volume, adds ferment 5 grams, and insulation is 1.5 hours under 85 ℃ of temperature, carries out spray-drying then.Dry concrete operations condition is as follows: the concentrate temperature is 55 ℃; 125 ℃ of EATs, 105 ℃ of tower temperature promptly obtain the high-purity natural edible pigment.
Example 2
100 kilograms of black rice chaffs and water are carried out lixiviate for 900 liters in aseptic jar, extraction temperature is 70 ℃, and extraction time is 14 hours, and adding citric acid, natrium citricum and Vc adjust pH is 2.Black rice chaff residue and water after the lixiviate are carried out lixiviate for 900 liters in aseptic jar, extraction temperature is 80 ℃, and extraction time is 10 hours, and adding citric acid, natrium citricum and Vc adjusting pH value is 2.The ferment that black rice chaff residue after the secondary lixiviate is added 100 grams carries out glycolysis, and temperature is 60 ℃, and the time is 0.5 hour.Carry out lixiviate with 900 premium on currency in aseptic jar then, extraction temperature is 80 ℃, and extraction time is 10 hours, and adding citric acid, natrium citricum and Vc adjusting pH value is 2.Put No. three extracts into hold-up tank room temperature cooling precipitation 7 hours as coarse filtration, the coarse filtration liquid that obtains is by the smart filter of diatomaceous earth filter, and to concentrate recovered alcohol soft to the extract for vacuum then.Filtered fluid after concentrating repeatedly cleans with distilled water by NKA macroporous absorbent resin adsorpting pigment again, removes impurity.Be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 90% edible alcohol wash-out then, collect and flow out liquid, obtain the natural edible pigment solution behind the purifying.It is 160 liters that its vacuum is concentrated into volume, and pigment concentrate is added ferment 112 grams, and insulation is 3 hours under 60 ℃ of temperature, carries out spray-drying then.Dry concrete operations condition is as follows: the concentrate temperature is 80 ℃; 135 ℃ of EATs, 115 ℃ of tower temperature promptly obtain the high-purity natural edible pigment.
Example 3
100 kilograms of black rice chaffs and alcohol are carried out lixiviate for 300 liters in aseptic jar, alcohol concentration is 95%, and extraction temperature is 15 ℃, and extraction time is 1 hour, and adding citric acid, natrium citricum and Vc adjust pH is 6.Black rice chaff residue and alcohol after the lixiviate are carried out lixiviate for 300 liters in aseptic jar, alcohol concentration is 95%, and extraction temperature is 30 ℃, and extraction time is 2 hours, and adding hydrochloric acid and lemon acid for adjusting pH value is 6.The ferment that black rice chaff residue after the secondary lixiviate is added 20 grams carries out glycolysis, and temperature is 30 ℃, and the time is 1.5hr.Carry out lixiviate for 300 liters in aseptic jar with alcohol then, alcohol concentration is 95%, and extraction temperature is 30 ℃, and extraction time is 4 hours, and adding citric acid, natrium citricum and Vc adjusting pH value is 6.Put No. three extracts into hold-up tank room temperature cooling precipitation 12 hours as coarse filtration, the coarse filtration liquid that obtains is by the smart filter of diatomaceous earth filter, and to concentrate recovered alcohol soft to the extract for vacuum then.Filtered fluid after concentrating repeatedly cleans with distilled water by NKA macroporous absorbent resin adsorpting pigment again, removes impurity.Be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 40% edible alcohol wash-out then, collect and flow out liquid, obtain the natural edible pigment solution behind the purifying.It is 50 liters that its vacuum is concentrated into volume, adds ferment 5 grams, and insulation is 1.5 hours under 85 ℃ of temperature, carries out spray-drying then.Dry concrete operations condition is as follows: the concentrate temperature is 55 ℃; 125 ℃ of EATs, 105 ℃ of tower temperature promptly obtain the high-purity natural edible pigment.
Example 4
100 kilograms of black rice chaffs and water are carried out lixiviate for 900 liters in aseptic jar, extraction temperature is 70 ℃, and extraction time is 14 hours, and adding citric acid, natrium citricum and Vc adjust pH is 2.Black rice chaff residue and water after the lixiviate are carried out lixiviate for 900 liters in aseptic jar, extraction temperature is 80 ℃, and extraction time is 10 hours, and adding Vc and different Vc-Na adjusting pH value is 2.The ferment that black rice chaff residue after the secondary lixiviate is added 100 grams carries out glycolysis, and temperature is 60 ℃, and the time is 2 hours.Carry out lixiviate with 900 premium on currency in aseptic jar then, extraction temperature is 80 ℃, and extraction time is 10 hours, and adding hydrochloric acid and lemon acid for adjusting pH value is 2.Put No. three extracts into hold-up tank room temperature cooling precipitation 7 hours as coarse filtration, the coarse filtration liquid that obtains is by the smart filter of diatomaceous earth filter, and to concentrate recovered alcohol soft to the extract for vacuum then.Filtered fluid after concentrating repeatedly cleans with distilled water by NKA macroporous absorbent resin adsorpting pigment again, removes impurity.Be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 90% edible alcohol wash-out then, collect and flow out liquid, obtain the natural edible pigment solution behind the purifying.It is 160 liters that its vacuum is concentrated into volume, and pigment concentrate is added ferment 112 grams, and insulation is 3 hours under 60 ℃ of temperature, carries out spray-drying then.Dry concrete operations condition is as follows: the concentrate temperature is 80 ℃; 135 ℃ of EATs, 115 ℃ of tower temperature promptly obtain the high-purity natural edible pigment.
Example 5
100 kilograms of black rice chaffs and alcohol are carried out lixiviate for 300 liters in aseptic jar, alcohol concentration is 95%, and extraction temperature is 15 ℃, and extraction time is 1 hour, and adding hydrochloric acid and citric acid adjust pH is 6.Black rice chaff residue and alcohol after the lixiviate are carried out lixiviate for 300 liters in aseptic jar, alcohol concentration is 95%, and extraction temperature is 30 ℃, and extraction time is 2 hours, and adding Vc and different Vc-Na adjusting pH value is 6.The ferment that black rice chaff residue after the secondary lixiviate is added 20 grams carries out glycolysis, and temperature is 30 ℃, and the time is 2 hours.Carry out lixiviate with alcohol 300L in aseptic jar then, alcohol concentration is 95%, and extraction temperature is 30 ℃, and extraction time is 2 hours, and adding citric acid, natrium citricum and Vc adjusting pH value is 6.Put No. three extracts into hold-up tank room temperature cooling precipitation 12 hours as coarse filtration, the coarse filtration liquid that obtains is by the smart filter of diatomaceous earth filter, and to concentrate recovered alcohol soft to the extract for vacuum then.Filtered fluid after concentrating repeatedly cleans with distilled water by NKA macroporous absorbent resin adsorpting pigment again, removes impurity.Be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 40% edible alcohol wash-out then, collect and flow out liquid, obtain the natural edible pigment solution behind the purifying.It is 50 liters that its vacuum is concentrated into volume, adds ferment 5 grams, and insulation is 1.5 hours under 85 ℃ of temperature, carries out spray-drying then.Dry concrete operations condition is as follows: the concentrate temperature is 55 ℃; 125 ℃ of EATs, 105 ℃ of tower temperature promptly obtain the high-purity natural edible pigment.
Example 6
100 kilograms of black rice chaffs and water are carried out lixiviate for 900 liters in aseptic jar, extraction temperature is 70 ℃, and extraction time is 14 hours, and adding hydrochloric acid and citric acid adjust pH is 2.Black rice chaff residue and water after the lixiviate are carried out lixiviate for 900 liters in aseptic jar, extraction temperature is 80 ℃, and extraction time is 10 hours, and adding citric acid, natrium citricum and Vc adjusting pH value is 2.The ferment that black rice chaff residue after the secondary lixiviate is added 100 grams carries out glycolysis, and temperature is 60 ℃, and the time is 0.5 hour.Carry out lixiviate with 900 premium on currency in aseptic jar then, extraction temperature is 80 ℃, and extraction time is 10 hours, and adding Vc and different Vc-Na adjusting pH value is 2.Put No. three extracts into hold-up tank room temperature cooling precipitation 7 hours as coarse filtration, the coarse filtration liquid that obtains is by the smart filter of diatomaceous earth filter, and to concentrate recovered alcohol soft to the extract for vacuum then.Filtered fluid after concentrating repeatedly cleans with distilled water by NKA macroporous absorbent resin adsorpting pigment again, removes impurity.Be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 90% edible alcohol wash-out then, collect and flow out liquid, obtain the natural edible pigment solution behind the purifying.It is 160 liters that its vacuum is concentrated into volume, and pigment concentrate is added ferment 112 grams, and insulation is 3 hours under 60 ℃ of temperature, carries out spray-drying then.Dry concrete operations condition is as follows: the concentrate temperature is 80 ℃; 135 ℃ of EATs, 115 ℃ of tower temperature promptly obtain the high-purity natural edible pigment.

Claims (3)

1, the preparation method of natural edible pigment in a kind of black rice chaff is characterized in that:
1. raw material lixiviate: adding concentration in the black rice chaff is 0~95% alcohol, and its ratio is to add 3~9 liters of alcohol in 1 kilogram of black rice chaff, and lixiviate is 1~14 hour in aseptic jar, and its pH value is 2~6, and temperature is 15~70 ℃,
2. filter: with extract room temperature cooling-sedimentation 7~12 hours, get supernatant by diatomaceous earth filter, vacuum concentrates recovered alcohol, and is soft to the extract,
3. purifying: above-mentioned concentrate by NKA macroporous absorbent resin adsorpting pigment, is cleaned with distilled water and removes impurity, be adsorbed on natural edible pigment on the NKA macroporous absorbent resin with 40~90% edible alcohol wash-outs then, collect outflow liquid,
4. dry: above-mentioned outflow liquid is carried out vacuum, and to be concentrated into concentration be 15~18%, in pigment concentrate, add 0.1 ‰~0.7 ‰ ferment again, under 60~85 ℃ of temperature, be incubated 1.5~3 hours, carry out spray-drying then, its condition is that the concentrate temperature is 55~80 ℃, 125~130 ℃ of EATs, 105~115 ℃ of tower temperature.
2, the preparation method of natural edible pigment according to claim 1, it is characterized in that: adding concentration in the black rice chaff residue after a lixiviate is 0~95% alcohol, its ratio is to add 3~9 liters of alcohol in 1 kilogram of rice bran residue, lixiviate is 2~10 hours in aseptic jar, its pH value is 2~6, and temperature is 30~80 ℃.
3, the preparation method of natural edible pigment according to claim 1 and 2 is characterized in that: add 0.02~0.1% ferment in the black rice chaff residue after above-mentioned lixiviate and carry out glycolysis, temperature is 30~60 ℃, and the time is 0.5~2 hour.Adding concentration then is 0~95% alcohol, and its ratio is to add 3~9 liters of alcohol in 1 kilogram of black rice chaff residue, then pH value 2~6,30~80 ℃ of lixiviates of temperature 2~10 hours.
CNA2003101048565A 2003-10-14 2003-10-14 Method for black rice haematochrome from black rice bran Pending CN1528193A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102020868A (en) * 2010-05-21 2011-04-20 湖北紫鑫生物科技有限公司 Method for extracting purple sweet potato anthocyanin
CN102140259A (en) * 2010-12-22 2011-08-03 晨光生物科技集团股份有限公司 Stabilization processing method for haematochrome of red rice
CN102659871A (en) * 2012-05-08 2012-09-12 魏有良 Method for extracting and refining anthocyanin in black rice
CN101649127B (en) * 2009-09-18 2012-11-28 长春海涛天然色素有限公司 Preparation technology of red pigments of red rice
CN101747661B (en) * 2009-12-22 2012-12-05 晨光生物科技集团股份有限公司 Technology for improving ang-kak red pigment quality by utilizing enzyme preparation
CN106754082A (en) * 2017-02-15 2017-05-31 刘煜华 A kind of production method of black rice thick wine

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101649127B (en) * 2009-09-18 2012-11-28 长春海涛天然色素有限公司 Preparation technology of red pigments of red rice
CN101747661B (en) * 2009-12-22 2012-12-05 晨光生物科技集团股份有限公司 Technology for improving ang-kak red pigment quality by utilizing enzyme preparation
CN102020868A (en) * 2010-05-21 2011-04-20 湖北紫鑫生物科技有限公司 Method for extracting purple sweet potato anthocyanin
CN102140259A (en) * 2010-12-22 2011-08-03 晨光生物科技集团股份有限公司 Stabilization processing method for haematochrome of red rice
CN102659871A (en) * 2012-05-08 2012-09-12 魏有良 Method for extracting and refining anthocyanin in black rice
CN106754082A (en) * 2017-02-15 2017-05-31 刘煜华 A kind of production method of black rice thick wine

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