CN107674452B - Method for extracting Dan osmanthus yellow pigment - Google Patents

Method for extracting Dan osmanthus yellow pigment Download PDF

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CN107674452B
CN107674452B CN201711145487.2A CN201711145487A CN107674452B CN 107674452 B CN107674452 B CN 107674452B CN 201711145487 A CN201711145487 A CN 201711145487A CN 107674452 B CN107674452 B CN 107674452B
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yellow pigment
extraction
osmanthus
sweet osmanthus
ethyl alcohol
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CN107674452A (en
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舒孝顺
马文豪
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Changsha University of Science and Technology
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    • 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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Abstract

The invention discloses a method for extracting a red-sweet osmanthus yellow pigment, which adopts absolute ethyl alcohol and ultrasonic auxiliary process for extraction and specifically comprises the following steps: (1) vacuum drying, pulverizing and sieving fresh flos Osmanthi Fragrantis to obtain flos Osmanthi Fragrantis powder; (2) soaking the sweet osmanthus powder in absolute ethyl alcohol; (3) carrying out ultrasonic extraction on the soak solution obtained in the step (2) to obtain a red-sweet osmanthus yellow pigment extraction crude product; (4) and removing impurities and purifying the extracted crude product of the red-sweet osmanthus yellow pigment to obtain pure red-sweet osmanthus yellow pigment. The invention adopts the absolute ethyl alcohol and the ultrasonic auxiliary process to extract the yellow pigment of the osmanthus fragrans, can shorten the production time, reduce the energy and solvent consumption and the generation of waste, and can improve the yield and the purity of the extract at the same time; not only reduces the operation cost, but also avoids the damage of the yellow pigment component of the sweet osmanthus flower, which is heat sensitive (easy to degrade or destroy at high temperature).

Description

method for extracting Dan osmanthus yellow pigment
Technical Field
The invention belongs to the field of natural pigment extraction, and particularly relates to a method for extracting an osmanthus fragrans yellow pigment by adopting absolute ethyl alcohol and an ultrasonic-assisted process.
Background
Pigments can be classified into natural pigments and synthetic pigments according to their origin. As many researches indicate that some synthetic pigments have other harmful effects such as mutagenicity, carcinogenicity and the like besides general toxicity to human bodies, more and more people pay attention to the development and utilization of natural pigments in view of the harmfulness of the synthetic pigments to the human bodies. The natural pigment is safe and reliable, has natural color and luster, has both nutritional and pharmacological effects, is favored by people, especially along with the increasing self-protection consciousness of people in recent years, along with the increasing popularization and large-scale application of green food and natural cosmetics, the development and utilization of the natural pigment become hot spots in the food industry and the cosmetic industry all over the world, and the application of the safe, natural and nontoxic natural pigment to replace the synthetic pigment tends to be great.
osmanthus fragrans (Osmanthus fragrans), also known as Olea officinalis, is a flower of Melilotus officinalis of Oleaceae, and has mild character and spicy flavor. Osmanthus fragrans is widely distributed in Yunnan province, Sichuan province, Guangxi province, Guangdong province, Hubei province and other provinces. The flavochrome of the osmanthus fragrans is a glycoside, is a derivative of benzopyran, has the function of slowing the progression of arteriosclerosis of human bodies, can also prevent and treat various cardiovascular and cerebrovascular diseases, can also be used as a food photoprotectant and a free radical scavenger, and has the simplest application as a food processing colorant. Nowadays, natural pigments with nutrition, health care, safety and health are growing up, and synthetic pigments are gradually abandoned by people, so that the natural osmanthus yellow pigment has great development and utilization values and wide market prospects.
Although the existing osmanthus yellow pigment is researched, the extraction research is very little, the process is not very reasonable, the extraction solvent mostly adopts ethanol with lower concentration such as 80%, 85% and 95%, the extraction impurities are more, the subsequent separation and purification are difficult, the separation and purification cost is high, the extraction method also mainly adopts the traditional extraction method, reflux extraction method and microwave extraction method, and the defects and disadvantages that the period is long, the energy consumption is high, the production cost is high, the yellow pigment is easy to damage during high-temperature reflux or microwave high-temperature extraction and the like generally exist.
Disclosure of Invention
the invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and providing a method for extracting the osmanthus fragrans yellow pigment by adopting absolute ethyl alcohol and an ultrasonic auxiliary process.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
A method for extracting the yellow pigment of the sweet osmanthus flower adopts absolute ethyl alcohol and ultrasonic auxiliary technology for extraction, and comprises the following steps:
(1) Vacuum drying, pulverizing and sieving fresh flos Osmanthi Fragrantis to obtain flos Osmanthi Fragrantis powder;
(2) Soaking the sweet osmanthus powder in absolute ethyl alcohol; if absolute ethyl alcohol is not adopted, the polarity is too high by adopting a conventional aqueous ethyl alcohol solution, the osmanthus yellow pigment in the aqueous ethyl alcohol solution is easy to oxidize and hydrolyze, the solubility of the osmanthus yellow pigment in the aqueous ethyl alcohol solution is too low, and the pigment extraction rate is low;
(3) carrying out ultrasonic extraction on the soak solution obtained in the step (2) at normal temperature (30 ℃) to obtain a red-sweet osmanthus yellow pigment extraction crude product;
(4) And removing impurities and purifying the extracted crude product of the red-sweet osmanthus yellow pigment to obtain pure red-sweet osmanthus yellow pigment.
In the above method, preferably, in the step (3), the number of times of ultrasonic extraction is 1-5, and the time for each ultrasonic extraction is 10-50 min. If the extraction is directly carried out without ultrasonic extraction, the ethanol solvent is difficult to enter the cells of the osmanthus fragrans, the dissolution of the yellow pigment is slow, the extraction efficiency of the osmanthus fragrans yellow pigment is low, and the extraction time is long.
In the above method, preferably, in the step (3), the number of times of ultrasonic extraction is 3, and the time for each extraction is 10 min.
Preferably, in the step (2), the ratio of the sweet osmanthus flower powder to the absolute ethyl alcohol is 1 g: (6-14) mL. The extraction efficiency is not high when the dosage of the extraction solvent is small, the required extraction times need to be increased, the cost of the solvent is high, and the extraction time and the production period are prolonged; the consumption of the extraction solvent is large, the cost of the solvent is high, and the investment is overlarge due to the fact that larger extraction production equipment is needed due to overlarge extraction volume; through repeated research, the feed-liquid ratio of the osmanthus fragrans powder to the absolute ethyl alcohol is finally determined to be 1 g: (6-14) mL.
Preferably, in the step (2), the ratio of the sweet osmanthus flower powder to the absolute ethyl alcohol is 1 g: 12 mL.
in the above method, preferably, in the step (2), the time for soaking the sweet osmanthus flower powder in the absolute ethyl alcohol is 30 min. The applicant finds that when the soaking time is less than 30min, the solvent cannot fully permeate into the cells, the requirement on subsequent extraction time is prolonged, the subsequent extraction efficiency is influenced, and the extraction efficiency is low; if the soaking time is too long, the time is wasted, the extraction rate is not influenced, the whole production period is prolonged, and the production cost is increased; the applicant finds that the osmanthus fragrans flower powder can be soaked for 30 minutes, the anhydrous solvent can be just fully permeated into the osmanthus fragrans flower cells, and the leaching efficiency is high.
In the above method, preferably, in the step (1), the temperature of the vacuum drying is 40 ℃, and the time of the vacuum drying is 6 hours; crushing by adopting a high-speed universal crusher in the crushing process, wherein the mass of dried sweet osmanthus is controlled to be 20g each time of crushing; sieving refers to sieving with 100 mesh sieve.
in the above method, preferably, in the step (4), the specific process of impurity removal and purification includes:
Firstly, dissolving the red-sweet osmanthus yellow pigment crude product by using hot water with the weight 10 times that of the crude product to obtain a hot water solution of the crude product; extracting with ethyl acetate equal in volume to the crude hot water solution for 3 times, mixing extractive solutions, concentrating the extractive solution to obtain extract, and vacuum drying to obtain pure yellow pigment of flos Osmanthi Fragrantis.
the method adopts ultrasonic wave to assist in extracting the osmanthus yellow pigment, utilizes the strong vibration, high acceleration, strong cavitation effect and strong stirring action of the ultrasonic wave to shorten the time for the effective components of the osmanthus yellow pigment to enter a solvent, accelerates the extraction process, improves the extraction rate, can extract at 20-50 ℃ and even at low temperature, and can effectively avoid the damage of high temperature to the effective components of the osmanthus yellow pigment.
in the process of the invention, absolute ethyl alcohol is adopted as an extraction solvent, the polarity of the absolute ethyl alcohol is smaller than that of ethyl alcohol with the purity of 95 percent, the osmanthus yellow pigment is a fat-soluble pigment with small polarity, so that the solubility of the osmanthus yellow pigment is higher by adopting the absolute ethyl alcohol, the absolute ethyl alcohol does not contain water and hardly contains dissolved oxygen, the osmanthus yellow pigment is not oxidized and hydrolyzed in the absolute ethyl alcohol, the degradation damage is small, the extraction rate is naturally higher, meanwhile, normal-temperature ultrasonic extraction is also added in the extraction process, the short-time extraction is carried out at a lower temperature, the damage to the thermosensitive osmanthus yellow pigment is extremely small, the two processes are combined, so that the extraction rate of the osmanthus yellow pigment is high, the production time is shorter, the comprehensive production cost is lower, in addition, the extraction and purification processes are adopted, the production time and the cycle are further shortened, and the three processes are skillfully and organically combined, the extraction rate of the yellow pigment of the osmanthus fragrans is higher, the purity is higher, the production time and the production period are greatly shortened, the equipment investment is reduced, the comprehensive production cost is greatly reduced, the comprehensive benefit is greatly increased, and the method is more suitable for large-scale production. In addition, the method adopts the absolute ethyl alcohol as the extraction solvent, the absolute ethyl alcohol does not contain moisture and water-soluble oxygen, and compared with the hydrous ethyl alcohol with a certain concentration, the method does not cause hydrolysis and oxidation damage of the osmanthus yellow pigment in the extraction process, so that the osmanthus yellow pigment is not easy to degrade in the extraction process, and the extraction rate is better.
Compared with the prior art, the invention has the advantages that:
(1) the method adopts absolute ethyl alcohol to soak the osmanthus fragrans yellow pigment, and the absolute ethyl alcohol has high solubility on the osmanthus fragrans yellow pigment and low solubility on impurities, particularly low solubility on water-soluble impurities; meanwhile, an ultrasonic auxiliary process is adopted, the stability of the red-scented osmanthus yellow pigment is not easy to damage at a lower temperature, the extraction rate of the red-scented osmanthus yellow pigment is high, the impurities are few, the purity is high, the subsequent separation and purification are easy, the production period is short, and the production cost is low.
(2) The invention adopts the absolute ethyl alcohol and the ultrasonic auxiliary process to extract the yellow pigment of the osmanthus fragrans, can shorten the production time, reduce the energy and solvent consumption and the generation of waste, and can improve the yield and the purity of the extract at the same time; not only reduces the operation cost, but also avoids the damage of the yellow pigment component of the sweet osmanthus flower, which is heat sensitive (easy to degrade or destroy at high temperature).
(3) The purity of the red-rooted osmanthus flower yellow pigment obtained by the method is as high as more than 80%, and the yield of the red-rooted osmanthus flower yellow pigment is as high as more than 2.230%.
(4) The whole production process of the invention does not adopt any toxic solvent and toxic chemicals, does not discharge any waste water and waste gas, does not have any environmental pollution, and the residual sweet osmanthus residue after extraction can be used as animal feed or organic fertilizer, can be further comprehensively developed and utilized, and is a green and environment-friendly production process.
drawings
FIG. 1 shows the effect of different leaching agents on the extraction effect of the yellow pigment from osmanthus fragrans in example 1 of the present invention.
FIG. 2 shows the effect of different feed liquid ratios on the extraction effect of the yellow pigment from sweet osmanthus flower in example 2 of the present invention.
FIG. 3 shows the effect of different ultrasonic times on the extraction effect of the yellow pigment from osmanthus fragrans in embodiment 3 of the present invention.
FIG. 4 shows the effect of different ultrasonic extraction times on the extraction effect of the yellow pigment from osmanthus fragrans in embodiment 4 of the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1: influence of different leaching agents on extraction of the yellow pigment of osmanthus fragrans
Extracting the yellow pigment of the osmanthus by adopting different extracting agents, and specifically comprising the following steps:
Harvesting the sweet osmanthus flowers on sunny days (no water exists on the surfaces of the flowers), placing the harvested fresh sweet osmanthus flowers in a vacuum drying oven within 1 hour, carrying out vacuum drying for 6 hours at 40 ℃, crushing the dried sweet osmanthus flowers by using a high-speed universal crusher, crushing 20g of the crushed sweet osmanthus flowers each time, and finally sieving the powdery sweet osmanthus flowers by using a 100-mesh sieve to obtain sweet osmanthus flower powder (the sweet osmanthus flower powder is stored at low temperature under sealed vacuum to prevent the pigment from oxidative degradation, and is used for extracting the pigment in subsequent experiments).
Respectively weighing 3g of 5 parts of dried sweet osmanthus powder by using an analytical balance, respectively placing the weighed powder in 5 triangular flasks with 100mL, and then mixing the weighed powder with the powder-liquid ratio of 1 g: adding 10mL (pollen mass g/solvent volume mL) of methanol, absolute ethyl alcohol, acetone, ethyl acetate and petroleum ether, respectively, soaking at room temperature for 30min, and extracting with ultrasonic wave for 1 time for 40 min. After the leaching is finished, naturally cooling to room temperature, and filtering to obtain an extracting solution (namely a red osmanthus yellow pigment extraction crude product); then the volume is determined to be 250mL, the corresponding lixiviant is used as a blank control at room temperature, and the absorbance value of the yellow pigment extracting solution of the osmanthus fragrans in different lixiviants at the wavelength of 330nm is measured by an lcm cuvette on an ultraviolet-visible spectrophotometer, and the result is shown in Table 1 and figure 1.
TABLE 1 Effect of different lixiviants on absorbance
As can be seen from table 1 and fig. 1, the absorbance of the yellow pigment in the methanol and absolute ethanol leaching solution is the greatest, and the ethanol is the best leaching agent for the red-scented osmanthus yellow pigment because the methanol has high toxicity and the solvent price and the extraction cost are higher than those of the absolute ethanol, wherein when the absolute ethanol is used as the extraction solvent, the purity of the yellow pigment reaches 80.2%, and the yield is 2.233%.
Example 2: influence of feed liquid ratio on extraction of Dan Gui Osmanthus yellow pigment
The invention relates to a method for extracting a yellow pigment from osmanthus fragrans, which comprises the following specific steps:
Respectively weighing 3g of dried Dan osmanthus flower powder (see example 1 for pretreatment of Dan osmanthus flower powder) by using an analytical balance, placing the dried Dan osmanthus flower powder into 5 triangular flasks of 100mL, adding absolute ethyl alcohol according to the material-liquid ratio (mass g of Dan osmanthus flower powder/volume mL of solvent)) of 1:6, 1:8, 1:10, 1:12 and 1:14, soaking for 30 minutes at room temperature, and then extracting for 1 time by using ultrasonic waves for 40 minutes. Naturally cooling to room temperature after the leaching is finished, and filtering to obtain an extracting solution (namely a red osmanthus yellow pigment extraction crude product); then, the volume is determined to be 250mL by using absolute ethyl alcohol, the absolute ethyl alcohol is used as a blank control at room temperature, and the absorbance values of the yellow pigment extracting solution of the osmanthus fragrans at the wavelength of 330nm are measured by using a 1cm cuvette on an ultraviolet-visible spectrophotometer, wherein the results are shown in Table 2 and figure 2.
TABLE 2 Effect of different feed solution ratios on absorbance
As can be seen from Table 2 and FIG. 2, the absorbance is the largest when the ratio of the feed to the liquid is 1:6, the absorbance is the second when the ratio of the feed to the liquid is 1:10, but the absorbance is 1% larger than the ratio of the feed to the liquid when the ratio of the feed to the liquid is 1:10, the influence is very small, and the ratio of the feed to the liquid is 1:10 in consideration of mass production.
Dissolving the 5 parts of the red-rooted osmanthus yellow pigment crude product with hot water 10 times that of the crude product, extracting with ethyl acetate of the same volume as the hot water solution of the crude product for 3 times, mixing the extracting solutions, concentrating the extracting solution to an extractum state, and performing vacuum drying to obtain pure red-rooted osmanthus yellow pigment, wherein the purity of the yellow pigment obtained by an experiment with a material-to-liquid ratio of 1:10 reaches 80.0%, and the corresponding yield is 2.231%.
Example 3: influence of ultrasonic time on extraction of yellow pigment of osmanthus fragrans
The invention relates to a method for extracting a yellow pigment from osmanthus fragrans, which comprises the following specific steps:
Respectively weighing 3g of dried osmanthus fragrans powder by 5 parts by using an analytical balance (see example 1 for pretreatment of the osmanthus fragrans powder), placing the dried osmanthus fragrans powder into 5 triangular flasks of 100mL, adding absolute ethyl alcohol according to the optimal material-liquid ratio of 1:10, soaking for 30 minutes at room temperature, and performing ultrasonic extraction for 1 time for 10, 20, 30, 40 and 50 minutes respectively. Naturally cooling to room temperature after the leaching is finished, and filtering to obtain an extracting solution (namely a red osmanthus yellow pigment extraction crude product); then, the volume is determined to 250mL by using absolute ethyl alcohol, the absolute ethyl alcohol is used as a blank control at room temperature, and the absorbance of the yellow pigment extract of the osmanthus fragrans at the wavelength of 330nm under different extraction times is measured by using a 1cm cuvette and an ultraviolet-visible spectrophotometer, and the result is shown in Table 3 and figure 3.
TABLE 3 Effect of different ultrasound times on absorbance
as can be seen from table 3 and fig. 3, the absorbance values increased and then decreased with the ultrasound time, and the absorbance value was maximum at 20 minutes. Under the condition of a certain power, the temperature is also increased along with the increase of the ultrasonic extraction time, so that the yellow pigment is damaged and lost, and the phenomenon that the absorbance value is rapidly reduced occurs. Therefore, the ultrasonic extraction time should be optimally controlled to be 20 minutes, and the optimal extraction effect can be achieved.
Dissolving the 5 parts of the obtained red-brown osmanthus yellow pigment crude product with hot water which is 10 times that of the crude product, extracting with ethyl acetate which has the same volume as the hot water dissolving solution of the crude product, combining extracting solutions after 3 times of extraction, finally concentrating the extracting solution to an extractum state, and drying in vacuum to obtain pure red-brown osmanthus yellow pigment. Wherein, the ultrasonic time is 20 minutes: the purity of the yellow pigment reaches 80.1 percent, and the corresponding yield is 2.232 percent.
Example 4: influence of ultrasonic extraction times on extraction of yellow pigment of osmanthus fragrans
The invention relates to a method for extracting a yellow pigment from osmanthus fragrans, which comprises the following specific steps:
respectively weighing 3g of dried osmanthus fragrans powder by using an analytical balance, placing the weighed 5 parts of dried osmanthus fragrans powder into 5 triangular flasks with the volume of 100mL (see example 1 for pretreatment of the osmanthus fragrans powder), adding 95% ethanol into the triangular flasks according to the material-liquid ratio of 1:10, soaking for 30 minutes at room temperature, then performing ultrasonic extraction for 1 time, 2 times, 3 times, 4 times and 5 times respectively, wherein the extraction time is 20 minutes each time, naturally cooling to room temperature after the extraction is finished, and filtering to obtain an extracting solution (namely an osmanthus fragrans yellow pigment extracting crude product); then, the volume is determined to be 250mL by using absolute ethyl alcohol, the concentration of the absolute ethyl alcohol is used as a blank control at room temperature, and the absorbance value of the extraction solution of the yellow pigment of the osmanthus fragrans at the wavelength of 330nm is measured by using a 1cm cuvette on an ultraviolet-visible spectrophotometer for different ultrasonic extraction times, and the result is shown in table 4 and figure 4.
TABLE 4 Effect of ultrasound extraction times on absorbance
as can be seen from table 4 and fig. 4, the absorbance of the yellow pigment of osmanthus fragrans is maximized after 3 ultrasonic extractions, and the absorbance of the yellow pigment is increased only slightly after the number of extractions is increased, so that the number of extractions is selected as 3, which is the optimal number of extractions, considering other factors such as saving material, time, and labor.
Dissolving the 5 parts of the obtained red-brown osmanthus yellow pigment crude product in hot water which is 10 times that of the crude product, extracting with ethyl acetate which has the same volume as the hot water dissolving solution of the crude product for 3 times, mixing the extracting solutions, finally concentrating the extracting solution to an extractum state, and drying in vacuum to obtain pure red-brown osmanthus yellow pigment; the purity of yellow pigment obtained in 3 extraction experiments was 80.0%, corresponding to 2.231% yield.
according to the experimental results of the factors, the influence degree of each factor is analyzed, 3 levels are respectively selected according to 4 factors of the type of the leaching agent, the ratio of the material to the liquid, the extraction time and the extraction times, the designed orthogonal test is shown in the table 5, and the orthogonal test results are shown in the table 6.
TABLE 5 four-factor three-level table
Table 643 orthogonal experimental protocols and results
the experimental operation is carried out according to the experimental conditions listed in the orthogonal table, and the orthogonal experimental result is correspondingly analyzed, so that the larger the range is, the larger the influence on the extraction process is. The sequence of the influencing factors of the extraction process of the yellow pigment of the osmanthus fragrans is as follows: lixiviant type > ultrasonic extraction times > extraction time > material-liquid ratio. The orthogonal extraction result shows that the optimal extraction process for extracting the yellow pigment by ultrasonic waves comprises the following steps: extracting with anhydrous ethanol at a ratio of 1:12 for 3 times (10 min each time).
the optimal extraction process for extracting the yellow pigment by ultrasonic waves is verified by three repeated experiments, the experimental results are shown in table 7, the results are basically consistent with the results of orthogonal experiments, the results are relatively stable, repeated experiments can be carried out, the extraction effect is better, the average purity of the yellow pigment in 3 experiments reaches 80.0%, and the corresponding average yield is 2.230%.
Table 7 verification results
The above examples illustrate that: the method takes absolute ethyl alcohol as an extraction solvent, has high solubility to the yellow pigment of the osmanthus fragrans, is not easy to degrade and damage the yellow pigment of the osmanthus fragrans, has low solubility to impurities, and particularly has low solubility to water-soluble impurities; meanwhile, the ultrasonic process is adopted, the stability of the red-sweet osmanthus yellow pigment is not easy to damage at a lower temperature, the extraction rate of the red-sweet osmanthus yellow pigment is high, the impurities are few, the purity is high, the subsequent separation and purification are easy, the production period is short, and the production cost is low.

Claims (4)

1. The method for extracting the yellow pigment of the osmanthus fragrans is characterized by adopting absolute ethyl alcohol and an ultrasonic auxiliary process for extraction, and specifically comprises the following steps:
(1) vacuum drying, pulverizing and sieving fresh flos Osmanthi Fragrantis to obtain flos Osmanthi Fragrantis powder; the temperature of vacuum drying is 40 ℃, and the time of vacuum drying is 6 hours;
(2) Soaking the sweet osmanthus powder in absolute ethyl alcohol for 30 min; the feed-liquid ratio of the sweet osmanthus powder to the absolute ethyl alcohol is 1 g: (6-14) mL;
(3) Carrying out normal-temperature ultrasonic extraction on the soak solution obtained in the step (2) to obtain a red-sweet osmanthus yellow pigment extraction crude product; the ultrasonic extraction times are 3 times, and the time of each ultrasonic extraction is 10 min;
(4) And removing impurities and purifying the extracted crude product of the red-sweet osmanthus yellow pigment to obtain pure red-sweet osmanthus yellow pigment.
2. The method of claim 1, wherein in the step (2), the feed-liquid ratio of the osmanthus fragrans powder to the absolute ethyl alcohol is 1 g: 12 mL.
3. The method according to any one of claims 1 to 2, wherein in step (1),
Crushing by adopting a high-speed universal crusher in the crushing process, wherein the mass of dried sweet osmanthus is controlled to be 20g each time of crushing;
Sieving refers to sieving with 100 mesh sieve.
4. The method according to any one of claims 1-2, wherein in the step (4), the specific process of impurity removal and purification is as follows:
Firstly, dissolving the red-sweet osmanthus yellow pigment crude product by using hot water with the weight 10 times that of the crude product to obtain a hot water solution of the crude product; extracting with ethyl acetate equal in volume to the crude hot water solution for 3 times, mixing extractive solutions, concentrating the extractive solution to obtain extract, and vacuum drying to obtain pure yellow pigment of flos Osmanthi Fragrantis.
CN201711145487.2A 2017-11-17 2017-11-17 Method for extracting Dan osmanthus yellow pigment Expired - Fee Related CN107674452B (en)

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