CN109401358A - A method of haematochrome is extracted from Jasmine flower residue - Google Patents

A method of haematochrome is extracted from Jasmine flower residue Download PDF

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Publication number
CN109401358A
CN109401358A CN201710704486.0A CN201710704486A CN109401358A CN 109401358 A CN109401358 A CN 109401358A CN 201710704486 A CN201710704486 A CN 201710704486A CN 109401358 A CN109401358 A CN 109401358A
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jasmine
jasmine flower
flower residue
residue
ethyl alcohol
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不公告发明人
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Feng Shunzhen
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Feng Shunzhen
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0096Purification; Precipitation; Filtration

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Coloring Foods And Improving Nutritive Qualities (AREA)

Abstract

The invention discloses a kind of methods for extracting haematochrome from Jasmine flower residue, by Jasmine flower residue cleaning, remove impurity, it is carried out 10-30 seconds in far infrared sterilizer, then high-temperature sterilization is carried out again, sterilising temp range is set as 120-130 DEG C, pressure is 0.2~0.3MPa, and sterilizing duration range is 30-40 minutes;Jasmine flower residue is placed in water and impregnate 1-24 hours, its water content is made to reach 30-50%;Jasmine flower residue after vacuum drying is crushed to 400 mesh or more in super-micro wall-broken grinder;Again into smashed Jasmine flower residue powder, the ethyl alcohol of Jasmine 1.1-1.5 times of residue powder weight of flower is added, the concentration of the ethyl alcohol is 40-50%'s, pass through ultrasonic continuous stream biomixer again, supersonic frequency 15-40KHz, power 1000-3000W, flow is 15Kg to suspension per hour, obtained broken Jasmine flower residue powder suspension.

Description

A method of haematochrome is extracted from Jasmine flower residue
Technical field
The invention belongs to health product technology fields, relate generally to a kind of method for extracting haematochrome from Jasmine flower residue.
Background technique
Edible pigment is also known as colorant, is the food additives by food color and for the purpose of improving food color, with The rapid development of food industry also increasingly increases the demand of edible pigment.Edible pigment can be divided into people because of its source difference Work synthetic dyestuff and natural pigment two major classes, with regard to edible pigment application evolution from the point of view of, in the middle of the 19th century before, be apply than More crude natural pigment is as edible pigment;After in the middle of the 19th century, since synthetic dyestuff is come out one after another, and with it with color Pool is bright-coloured, and stability is good, strong coloring force, is suitable for toning, and easy to dissolve, quality is uniform, odorless, tasteless and low in cost etc. one Number of advantages, thus be widely used in food, to increase style and kind and the appetite sense for improving people of food, but with The increase of the improvement of people's living standards and health care consciousness, the secondary colour that the food such as beverage, candy, cake and drinks are used More stringent requirements are proposed for element.Past, common secondary colour was known as azo group (- N=N-), it is a kind of chromophoric group, contained this The compound of kind group is all coloured substance, but many azo-compounds are carcinogenic substances, has different degrees of chronic toxicity With carcinogenic and teratogenesis.In recent years, it since synthetic dyestuff toxicity is increasingly that people is of interest, is gradually limited in external many developed countries System is even forbidden to use synthetic dyestuff, and the country also just slowly eliminates its use.Most natural pigments due to edible safety without Poison, natural in color, many kinds have the effects that physiological activity has certain nutrition and health care and anti-inflammatory concurrently, they retain Part natural component abundant is such as in plant: vitamin, amino acid, nucleotide, flavonoids and certain required members Element etc. is not only widely used in the products such as various cosmetics, food, beverage, to help the deviation for correcting color rate and emphasize to indicate Style possessed by different food products, and the industries such as medicine, health care product are also applicable in, therefore in the international market, natural colour Plain sales volume annual growth is maintained at 10% or so, so domestic go in for the study develops unit and the personnel of natural food colour It is increasing, develop and utilize the certainty that natural plant pigment replaces synthetic food color to have become history.With edible secondary colour Element is compared, and edible natural pigment has following advantages: 1, most natural pigments are nontoxic and without side-effects, highly-safe;2, Containing nutriment needed by human or itself be exactly vitamin or the object with vitamin property in many natural pigments Matter, such as riboflavin, beta carotene;3, the natural pigment having has certain pharmacological effect, has prophylactic treatment to certain diseases Effect, such as rutin sophorin natural edible flavochrome have and make one to maintain the normal resistivity of capillary and to prevent artery sclerosis function Can, medically always as the ancillary drug and nutritional supplement for treating disease of cardiovascular system;4, the coloring of natural pigment Tone compare naturally, closer to natural materials color.But at present it is not yet found that people is using Jasmine flower residue as raw material
Natural pigment has certain nutrition and pharmacological action, coloring certainly however is favored by people because it is safe and reliable. Natural red colouring matter is divided into fat-soluble natural red colouring matter and water-soluble natural haematochrome, and fat-soluble natural red colouring matter is due to molten in water Solution degree is poor, and dispersion is uneven, thus application is restricted.Water-soluble natural haematochrome is present in plant cell liquor, due to It is uniformly dispersed in water, colours nature, is highly-safe, there are also certain nutritive value or pharmacological actions for some, in modern food work It is just gradually taken seriously in industry development.
Currently, the extracting method to water-soluble natural haematochrome mainly uses extraction, i.e., by mature dry fruit After pericarp crushes, coarse powder is extracted with organic solvent, then leaching liquor is concentrated, dries to obtain haematochrome solid product, there are commonly Solvent has acetone, ethyl alcohol, ether, chloroform etc..The product yield that this technique obtains is not high, and product purity is poor, later period purification Difficulty, and solvent recovery is costly, the production cycle is long.
Summary of the invention
Aiming at the shortcomings in the prior art, the purpose of the present invention is to provide one kind extracts haematochrome from Jasmine flower residue Method.
To achieve the goals above, the technical solution adopted by the present invention is that:
A method of haematochrome being extracted from Jasmine flower residue, the described method comprises the following steps:
Jasmine flower residue cleaning is removed impurity, carries out 10-30 seconds in far infrared sterilizer, then by step (1) High-temperature sterilization is carried out again, sets sterilising temp range as 120-130 DEG C, pressure is 0.2~0.3MPa, and sterilizing duration range is 30-40 minutes;Jasmine flower residue is placed in water and impregnate 1-24 hours, its water content is made to reach 30-50%;Vacuum is dry Jasmine flower residue after dry is crushed to 400 mesh or more in super-micro wall-broken grinder;Again to smashed Jasmine flower residue powder In end, the ethyl alcohol of Jasmine 1.1-1.5 times of residue powder weight of flower is added, the concentration of the ethyl alcohol is 40-50%, then is passed through Ultrasonic continuous stream biomixer, supersonic frequency 15-40KHz, power 1000-3000W, flow is suspension per hour 15Kg, obtained broken Jasmine flower residue powder suspension;
Step (2) preparation Jasmine flower residue extracting solution simultaneously filters;
After the evaporation of step (3) filtrate, resulting residue is the haematochrome extracted from Jasmine flower residue.
Step (2) adds 95% ethyl alcohol of food grade in gained jasmine pollen suspension in step (1), makes ethyl alcohol total weight Jasmine is extracted again for Jasmine weight 15, pot for solvent extraction is closed and with stirring, and extraction temperature is 65-70 DEG C, when extraction Between be 6-8h, Jasmine extract is obtained by filtration by 300-400 mesh.
Above-mentioned Jasmine alcohol extract is concentrated using vacuum suction method in step (3), and the temperature of vacuum suction concentration is 50-60 DEG C, time 2-4h, the adsorbent of vacuum suction concentration is active carbon or non-polar macroporous resin, and weight is former Jasmine weight 1-2 times of amount, using the high volatile component extracted out when adsorbent Adsorption Concentration with gaseous state ethyl alcohol, after gaseous state ethyl alcohol is then adsorbed agent The cool trap in face recycles, and the group of vacuum concentration is divided into Jasmine medicinal extract;Use supercritical CO2Extractive technique is to being adsorbed with Jasmine The adsorbent of high volatile component extracts, and extraction kettle pressure is 30-40Mpa, temperature is 20-25 DEG C, and separating still pressure is 8- 10Mpa, temperature are 50-60 DEG C, flow 90-100L/hr, obtain sticky paste haematochrome.
In step (1), every 1 parts by weight Jasmine flower residue is additionally added 0.5-1 parts of honey element, and 0.5-1 parts of maltodextrin, 0.2-0.5 parts of hydrochloric acid solutions, so that the pH value of Jasmine flower residue powder suspension is 5-6.
Specific embodiment
Embodiment 1
A method of haematochrome being extracted from Jasmine flower residue, the described method comprises the following steps:
Jasmine flower residue cleaning is removed impurity, carries out 10 seconds in far infrared sterilizer, then again by step (1) High-temperature sterilization is carried out, sets sterilising temp range as 120 DEG C, pressure 0.2MPa, sterilizing duration range is 30 minutes;By jasmine It spends colored residue to be placed in water impregnate 1 hour, its water content is made to reach 30%;Jasmine flower residue after vacuum drying is super Micro- wall-broken grinder is crushed to 400 mesh or more;Again into smashed Jasmine flower residue powder, Jasmine flower residue powder is added The ethyl alcohol of 1.1 times of last weight, the concentration of the ethyl alcohol is 40%, then passes through ultrasonic continuous stream biomixer, supersonic frequency Rate 15KHz, power 1000W, flow is 15Kg to suspension per hour, and obtained broken Jasmine flower residue powder suspends Liquid;
Step (2) preparation Jasmine flower residue extracting solution simultaneously filters;
After the evaporation of step (3) filtrate, resulting residue is the haematochrome extracted from Jasmine flower residue.
Step (2) adds 95% ethyl alcohol of food grade in gained jasmine pollen suspension in step (1), makes ethyl alcohol total weight Jasmine is extracted again for Jasmine weight 15, pot for solvent extraction is closed and with stirring, and extraction temperature is 70 DEG C, and extraction time is Jasmine extract is obtained by filtration by 400 mesh in 8h.
Above-mentioned Jasmine alcohol extract is concentrated using vacuum suction method in step (3), and the temperature of vacuum suction concentration is 60 DEG C, when Between be 4h, the adsorbent of vacuum suction concentration is active carbon or non-polar macroporous resin, and weight is the 2 of former Jasmine weight Times, using the high volatile component extracted out when adsorbent Adsorption Concentration with gaseous state ethyl alcohol, it is subsequent cool that gaseous state ethyl alcohol is then adsorbed agent Trap recycling, the group of vacuum concentration are divided into Jasmine medicinal extract;Use supercritical CO2Extractive technique is volatilized to Jasmine height is adsorbed with The adsorbent of component extracts, and extracts that kettle pressure is 40Mpa, temperature is 25 DEG C, and separating still pressure is 10Mpa, temperature 60 DEG C, flow 100L/hr obtains sticky paste haematochrome.
In step (1), every 1 parts by weight Jasmine flower residue is additionally added 1 part of honey element, and 1 part of maltodextrin, 0.5 part of hydrochloric acid Solution, so that the pH value of Jasmine flower residue powder suspension is 6.
Embodiment 2
A method of haematochrome being extracted from Jasmine flower residue, the described method comprises the following steps:
Jasmine flower residue cleaning is removed impurity, carries out 30 seconds in far infrared sterilizer, then again by step (1) High-temperature sterilization is carried out, sets sterilising temp range as 130 DEG C, pressure 0.3MPa, sterilizing duration range is 40 minutes;By jasmine It spends colored residue to be placed in water impregnate 24 hours, its water content is made to reach 50%;Jasmine flower residue after vacuum drying exists Super-micro wall-broken grinder is crushed to 400 mesh or more;Again into smashed Jasmine flower residue powder, Jasmine flower residue is added The ethyl alcohol that 1.5 times of powder weight, the concentration of the ethyl alcohol are 50%, then pass through ultrasonic continuous stream biomixer, ultrasound Frequency 40KHz, power 3000W, flow is 15Kg to suspension per hour, and obtained broken Jasmine flower residue powder suspends Liquid;
Step (2) preparation Jasmine flower residue extracting solution simultaneously filters;
After the evaporation of step (3) filtrate, resulting residue is the haematochrome extracted from Jasmine flower residue.
Step (2) adds 95% ethyl alcohol of food grade in gained jasmine pollen suspension in step (1), makes ethyl alcohol total weight Jasmine is extracted again for Jasmine weight 15, pot for solvent extraction is closed and with stirring, and extraction temperature is 70 DEG C, and extraction time is Jasmine extract is obtained by filtration by 400 mesh in 8h.
Above-mentioned Jasmine alcohol extract is concentrated using vacuum suction method in step (3), and the temperature of vacuum suction concentration is 60 DEG C, when Between be 4h, the adsorbent of vacuum suction concentration is active carbon or non-polar macroporous resin, and weight is the 2 of former Jasmine weight Times, using the high volatile component extracted out when adsorbent Adsorption Concentration with gaseous state ethyl alcohol, it is subsequent cool that gaseous state ethyl alcohol is then adsorbed agent Trap recycling, the group of vacuum concentration are divided into Jasmine medicinal extract;Use supercritical CO2Extractive technique is volatilized to Jasmine height is adsorbed with The adsorbent of component extracts, and extracts that kettle pressure is 40Mpa, temperature is 25 DEG C, and separating still pressure is 10Mpa, temperature 60 DEG C, flow 100L/hr obtains sticky paste haematochrome.
In step (1), every 1 parts by weight Jasmine flower residue is additionally added 0.5 part of honey element, 0.5 part of maltodextrin, 0.2 part Hydrochloric acid solution, so that the pH value of Jasmine flower residue powder suspension is 5.
Finally, it should be noted that obviously, above-described embodiment is only intended to clearly illustrate the application example, and simultaneously The non-restriction to embodiment.For those of ordinary skill in the art, it can also do on the basis of the above description Other various forms of variations or variation out.There is no necessity and possibility to exhaust all the enbodiments.And thus drawn Shen go out obvious changes or variations still in the protection scope of the application type among.

Claims (4)

1. a kind of method for extracting haematochrome from Jasmine flower residue, which is characterized in that the described method comprises the following steps:
Jasmine flower residue cleaning is removed impurity, carries out 10-30 seconds in far infrared sterilizer by step (1), then again into Row high-temperature sterilization sets sterilising temp range as 120-130 DEG C, and pressure is 0.2~0.3MPa, and sterilizing duration range is 30-40 Minute;Jasmine flower residue is placed in water and impregnate 1-24 hours, its water content is made to reach 30-50%;After vacuum drying Jasmine flower residue in super-micro wall-broken grinder be crushed to 400 mesh or more;Again into smashed Jasmine flower residue powder, The ethyl alcohol of Jasmine 1.1-1.5 times of residue powder weight of flower is added, the concentration of the ethyl alcohol is 40-50%, then passes through ultrasound Wave continuous flow cell crusher, supersonic frequency 15-40KHz, power 1000-3000W, flow is 15Kg to suspension per hour, is obtained The broken Jasmine flower residue powder suspension arrived;
Step (2) preparation Jasmine flower residue extracting solution simultaneously filters;
After the evaporation of step (3) filtrate, resulting residue is the haematochrome extracted from Jasmine flower residue.
2. the method for extracting haematochrome from Jasmine flower residue according to claim 1, which is characterized in that step (2) is in step Suddenly add 95% ethyl alcohol of food grade in gained jasmine pollen suspension in (1), make 15 times of weight of ethyl alcohol total weight Jasmine it is right Jasmine is extracted, and pot for solvent extraction is closed and with stirring, and extraction temperature is 65-70 DEG C, extraction time 6-8h, by 300- Jasmine extract is obtained by filtration in 400 mesh.
3. the method for extracting haematochrome from Jasmine flower residue according to claim 1, which is characterized in that step (3) uses Above-mentioned Jasmine alcohol extract is concentrated in vacuum suction method, and the temperature of vacuum suction concentration is 50-60 DEG C, time 2-4h, and vacuum is inhaled The adsorbent of attached concentration is active carbon or non-polar macroporous resin, and weight is 1-2 times of former Jasmine weight, utilizes adsorbent The high volatile component extracted out when Adsorption Concentration with gaseous state ethyl alcohol, gaseous state ethyl alcohol are then adsorbed the subsequent cool trap recycling of agent, and vacuum is dense The group of contracting is divided into Jasmine medicinal extract;Use supercritical CO2Extractive technique is to the adsorbent for being adsorbed with the high volatile component of Jasmine It extracts, extracts that kettle pressure is 30-40Mpa, temperature is 20-25 DEG C, separating still pressure is 8-10Mpa, temperature 50-60 DEG C, flow 90-100L/hr obtains sticky paste haematochrome.
4. the method for extracting haematochrome from Jasmine flower residue according to claim 1, it is characterised in that: in step (1), often 1 parts by weight Jasmine flower residue is additionally added 0.5-1 parts of honey element, and 0.5-1 parts of maltodextrin, 0.2-0.5 parts of hydrochloric acid solutions, so that The pH value of Jasmine flower residue powder suspension is 5-6.
CN201710704486.0A 2017-08-16 2017-08-16 A method of haematochrome is extracted from Jasmine flower residue Pending CN109401358A (en)

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Cited By (1)

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Application publication date: 20190301