CN117694424A - Sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances and preparation method thereof - Google Patents
Sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances and preparation method thereof Download PDFInfo
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- CN117694424A CN117694424A CN202410035073.8A CN202410035073A CN117694424A CN 117694424 A CN117694424 A CN 117694424A CN 202410035073 A CN202410035073 A CN 202410035073A CN 117694424 A CN117694424 A CN 117694424A
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- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention provides a method for preparing sea-buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances, and relates to the technical fields of extraction of the flavone and inositol substances in sea-buckthorn leaves and processing of the instant powder. The specific technical scheme includes that the dried sea buckthorn leaves are extracted with ethanol-water solution in an ultrasonic auxiliary mode, maltodextrin is added into the concentrated extract to serve as a drying aid, and finally freeze-dried instant powder is obtained through a vacuum freeze-drying process. The prepared sea buckthorn leaf freeze-dried instant powder overcomes the defect of poor appearance form of the commercial sea buckthorn tea, has higher extraction rate and retention rate of active ingredients such as flavone, inositol and the like, and can effectively maintain the fragrance and taste of sea buckthorn leaves. Has wide market prospect, further improves the economic value of the sea-buckthorn leaves, and can provide a certain guiding effect for the development of high added value products of the sea-buckthorn leaf industry.
Description
Technical Field
The invention relates to the technical field of instant powder processing, in particular to a preparation method of sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances.
Technical Field
The sea buckthorn has the most abundant natural sea buckthorn germplasm resources in the world, is the country with the largest artificial cultivation area, has significant important physiological activities of regulating blood fat, resisting inflammation, resisting oxidation, reducing blood sugar, resisting bacteria, resisting tumors and the like, and the main active ingredients are polysaccharide, flavonoid, polyphenol, inositol compounds and the like. Particularly, as a methyl ether derivative of inositol, quebrachitol in sea buckthorn leaves has been studied to show that the quebrachitol has good inhibitory activity on alpha-amylase, and can promote glucose consumption of relevant cells and regulate lipid metabolism in a proper dosage range. Is a natural active ingredient with great utilization value.
However, the content of quebrachitol in different parts of sea buckthorn is obvious, wherein the content of the sea buckthorn leaves is far higher than that of sea buckthorn pulp and seed meal. The sea buckthorn leaves have very rich species content of flavor precursor substances (amino acids, organic acids and the like) and high palatability. However, the sea buckthorn tea is sold in the market at present, and the surface of the leaf blade is provided with white star-shaped soft hair, so that more tea hair is produced during brewing, and the market popularization is influenced due to poor sensory quality.
The instant powder, instant tea and other products in the market are mostly obtained by extracting raw materials with water and directly drying. However, because of the large intermolecular attraction of many active ingredients such as flavonoids in sea buckthorn leaves, the solubility in water is extremely low, so the water extraction method cannot ensure the extraction of the active ingredients of the final product, and the extraction rate and the utilization rate are very low. While the active ingredients such as flavones are readily soluble in highly polar solvents such as ethanol. Ethanol has low toxicity as polar molecule and is widely used in food industry.
Because the glass transition temperature of the organic acid, polysaccharide and other small molecular weight substances contained in the sea buckthorn leaves is very low, the phenomenon of sticking to the wall in direct drying is serious, and the powder collecting rate can be greatly reduced, so that the processing loss rate is increased. Therefore, maltodextrin with high molecular weight and good solubility is selected as a drying aid to improve the glass transition temperature and the powder collecting rate, and reduce the viscosity and the hygroscopicity of the powder, so that the powder has good fluidity and solubility.
Hot air drying, microwave drying, spray drying, vacuum freeze drying and the like are common drying technologies in the field of food processing at present. However, the products obtained by these thermal processes such as hot air drying and spray drying have the following disadvantages: the color and luster are dull, the browning degree is deeper, and the retention rate of active ingredients is low. In addition, the product also produces a roasted and burnt smell, which is detrimental to the quality evaluation of the instant powder of seabuckthorn leaves. The freeze-dried powder product obtained by vacuum freeze-drying can effectively reduce the heat loss of low-boiling-point aroma components and retain the original green aroma of the sea buckthorn leaves to a great extent.
According to the dissolution characteristics of flavone and inositol substances in the sea-buckthorn leaves, the invention develops a processing technology of freeze-dried instant sea-buckthorn leaf powder by adopting ethanol-water solution extraction and vacuum freeze-drying. Not only can expand the extraction range of active substances in the sea buckthorn leaves and improve the extraction rate of the active substances, but also can effectively reduce the heat loss of the nutritional active ingredients and keep the original active substances to the greatest extent.
Disclosure of Invention
On the basis of the traditional instant powder processing technology, the invention optimizes related technological parameters, provides a preparation technology capable of effectively retaining flavone and inositol substances and preserving good mouthfeel and flavor, and improves the nutritional quality and sensory quality of the product. The method comprises the following steps: pulverizing, extracting with ethanol, concentrating under reduced pressure, dissolving in water, pre-freezing, and vacuum lyophilizing to obtain lyophilized instant powder rich in flavone and inositol.
In one embodiment, the crushing is specifically that the dried sea buckthorn leaves are crushed and then pass through a 10-30 mesh sieve for preservation in a dark place.
Preferably, the fresh sea buckthorn leaves are dried in the shade at room temperature. Compared with mechanical drying, natural drying in the shade can preserve the nutrient substances in the sea buckthorn leaves to a greater extent, and prevent the loss of fragrance.
In one embodiment, the ethanol extraction is specifically to weigh a certain amount of crushed seabuckthorn leaf powder, then add ethanol-water solution, stir and mix uniformly and soak for 10-20h at room temperature. Then under heating condition, ultrasound assisted extraction is performed.
Preferably, the volume fraction of the ethanol-water solution is 50-90%, and the ratio of extracted feed liquid is between 1:25 and 1:35 (g: mL). The heating temperature of ultrasonic assisted extraction is 40-50deg.C, and the extraction time is 40-50min.
In one embodiment, the concentrating under reduced pressure specifically comprises filtering the mixture, removing residue to obtain folium Hippophae extractive solution, and removing solvent with rotary evaporator to obtain pasty folium Hippophae extract.
Preferably, the water bath temperature of the rotary evaporator should be controlled at 40-50deg.C, and the pasty extract refers to pasty extract of Hippophae rhamnoides leaves without alcohol smell, which is obtained by completely removing solvent (purified water and ethanol).
In one embodiment, the water solution is prepared by adding purified water 5-6 times of the raw materials, mixing with the pasty extract of folium Hippophae, and then performing ultrasonic treatment for 20-30min. And finally, adding maltodextrin into the aqueous solution of the extract to obtain a mixed material liquid of the sea buckthorn leaf extract and the maltodextrin.
Preferably, maltodextrin is added in an amount of 10-20% of the mass of the aqueous extract solution, with the purpose of promoting sufficient dissolution of the wall-sticking extract.
In one embodiment, the prefreezing step comprises spreading mixed liquid of folium Hippophae extract and maltodextrin for 3-4mm, and prefreezing in a low temperature refrigerator at-20deg.C for 16-20 hr.
In one embodiment, the vacuum freeze drying is specifically that the materials are dried under vacuum and low temperature environment, and the sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances is obtained after full crushing.
Preferably, the temperature of the vacuum freeze drying is-45 to-50 ℃, the vacuum degree is 10Pa, and the freeze drying time is 16-24 hours.
In conclusion, the invention optimizes the related extraction and drying processes to prepare the sea buckthorn leaf freeze-dried instant powder product rich in flavone and inositol substances, and has the advantages of convenient carrying, good solubility, good taste and the like. Compared with the prior art, the invention has the advantages that:
1. based on the dissolution characteristics of bioactive substances such as flavone and inositol in sea buckthorn leaves, the invention selects the ethanol-water mixed solution as an extraction solvent, and is more beneficial to the dissolution of other active substances while extracting inositol substances such as quebrachitol and the like, thereby efficiently extracting other alcohol-soluble active ingredients.
2. Because the sea buckthorn leaves contain polysaccharide substances and the feed liquid to be dried has lower glass transition temperature, serious wall sticking phenomenon can occur in the drying process, maltodextrin is selected as a drying aid, so that the glass transition temperature and the powder collecting rate are improved, and the viscosity and the hygroscopicity of the powder are reduced, so that the sea buckthorn leaves have good fluidity and solubility.
3. The whole process flow has almost no high temperature. The stability set for both ultrasound-assisted extraction and rotary evaporation was below 50 ℃. The drying mode adopts vacuum freeze drying, thereby reducing the browning and caking of the product to the greatest extent. Effectively reduces the heat loss of the nutrition active ingredients and has high retention rate of the nutrition activity.
Drawings
FIG. 1 is a schematic flow chart of the method of the present invention.
FIG. 2 is a gas phase diagram of quebrachitol in the sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances prepared by the method of the invention.
Table 1 shows the solubility and flowability related index comparisons between the examples of the present invention and the control group.
Table 2 shows the active ingredients of the examples of the present invention and the control group compared with the sensory evaluation results.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Example 1
The embodiment discloses a preparation method of sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances, which comprises the following steps:
(1) Crushing: naturally drying fresh folium Hippophae at room temperature in shade, pulverizing, sieving with 30 mesh sieve, and storing in shade.
(2) Alcohol extraction: weighing a certain amount of dry sea buckthorn leaf powder, adding ethanol-water solution with volume fraction of 60% into the powder according to a feed-liquid ratio of 1:25 (g: mL), and stirring and mixing uniformly. After soaking for 12h, ultrasonic extraction is carried out for 50min under the heating condition of 45 ℃.
(3) Concentrating under reduced pressure: filtering the extract mixture, collecting supernatant, and rotary evaporating at 45deg.C in water bath to remove solvent (ethanol-water), wherein the extract is pasty and has no smell of ethanol.
(4) And (3) water-dissolving: adding purified water with the mass of 5 times of that of the raw materials into the pasty sea buckthorn leaf extract, carrying out ultrasonic treatment for 20min to promote the full dissolution of the extract, and then adding maltodextrin with the addition amount of 10% of that of the aqueous solution of the extract.
(5) Pre-freezing: the mixed liquid of the sea buckthorn leaf extract and maltodextrin is kept to be spread to be 3-4mm in thickness, and pre-frozen for 20 hours in a low-temperature refrigerator at the temperature of minus 20 ℃ so as to ensure that the liquid is completely frozen.
(6) Vacuum freeze drying: drying the pre-frozen material in vacuum and low temperature, and fully pulverizing to obtain the sea buckthorn leaf freeze-dried instant powder. The temperature of vacuum freeze drying is-45 ℃, the vacuum degree is 10Pa, and the freeze drying time is 24 hours.
Example 2
The embodiment discloses a preparation method of sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances, which comprises the following steps:
(1) Crushing: naturally drying fresh folium Hippophae at room temperature in shade, pulverizing, sieving with 30 mesh sieve, and storing in shade.
(2) Alcohol extraction: weighing a certain amount of dry sea buckthorn leaf powder, adding ethanol-water solution with the volume fraction of 70% into the powder according to the feed-liquid ratio of 1:30 (g: mL), and stirring and mixing uniformly. After soaking for 12 hours, ultrasonic extraction is carried out for 60 minutes under the heating condition of 50 ℃.
(3) Concentrating under reduced pressure: filtering the extract mixture, collecting supernatant, and rotary evaporating at 50deg.C in water bath to remove solvent (ethanol-water), wherein the extract is pasty and has no smell of ethanol.
(4) And (3) water-dissolving: adding purified water with the mass of 5 times of that of the raw materials into the pasty sea buckthorn leaf extract, carrying out ultrasonic treatment for 20min to promote the full dissolution of the extract, and then adding maltodextrin with the addition amount of 10% of that of the aqueous solution of the extract.
(5) Pre-freezing: the mixed liquid of the sea buckthorn leaf extract and maltodextrin is kept to be spread to be 3-4mm in thickness, and pre-frozen for 20 hours in a low-temperature refrigerator at the temperature of minus 20 ℃ so as to ensure that the liquid is completely frozen.
(6) Vacuum freeze drying: drying the pre-frozen material in vacuum and low temperature, and fully pulverizing to obtain the sea buckthorn leaf freeze-dried instant powder. The temperature of vacuum freeze drying is-45 ℃, the vacuum degree is 10Pa, and the freeze drying time is 24 hours.
Example 3
The embodiment discloses a preparation method of sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances, which comprises the following steps:
(1) Crushing: naturally drying fresh folium Hippophae at room temperature in shade, pulverizing, sieving with 30 mesh sieve, and storing in shade.
(2) Alcohol extraction: weighing a certain amount of dry sea buckthorn leaf powder, adding ethanol-water solution with volume fraction of 60% into the powder according to a feed-liquid ratio of 1:25 (g: mL), and stirring and mixing uniformly. After soaking for 12h, ultrasonic extraction is carried out for 50min under the heating condition of 45 ℃.
(3) Concentrating under reduced pressure: filtering the extract mixture, collecting supernatant, and rotary evaporating at 45deg.C in water bath to remove solvent (ethanol-water), wherein the extract is pasty and has no smell of ethanol.
(4) And (3) water-dissolving: adding purified water with the mass of 5 times of that of the raw materials into the pasty sea buckthorn leaf extract, carrying out ultrasonic treatment for 20min to promote the full dissolution of the extract, and then adding maltodextrin with the addition amount of 15% of that of the aqueous solution of the extract.
(5) Pre-freezing: the mixed liquid of the sea buckthorn leaf extract and maltodextrin is kept to be spread to be 3-4mm in thickness, and pre-frozen for 20 hours in a low-temperature refrigerator at the temperature of minus 20 ℃ so as to ensure that the liquid is completely frozen.
(6) Vacuum freeze drying: drying the pre-frozen material in vacuum and low temperature, and fully pulverizing to obtain the sea buckthorn leaf freeze-dried instant powder. The vacuum freeze drying temperature is-45 ℃, the vacuum degree is 10Pa, and the freeze drying time is 20h.
Control group 1
Control 1 was only added with gum arabic as a drying aid during the processing of the present invention when dissolved in water.
Control group 2
Control group 2 was only added with beta-cyclodextrin as a drying aid when in water-soluble during the process of the invention.
Control group 3
Control group 3 was dried by microwave during the process of the present invention
Control group 4
In the processing process of the invention, the control group 4 is dried by hot air.
Performance testing
Solubility: 1g of each of the instant powder of seabuckthorn leaf in examples 1 to 3 and comparative examples 1 and 2 was weighed and placed in a beaker, 100mL of distilled water at 50℃was added respectively, and the mixture was centrifuged after sufficient stirring. Taking the supernatant after centrifugation, drying in an oven until the weight is constant, and recording the quality. Experiments were repeated three times and the average was taken. The percentage of the ratio of the mass of the supernatant after drying to the sample weighing is the solubility.
Infiltration time: 1g of the instant powder of seabuckthorn leaf in examples 1-3 and comparative examples 1, 2 was weighed and placed in a beaker containing 50mL distilled water at 50 ℃. Once the powder is placed in the beaker, a timer is started and the time required for the powder to completely wet, i.e. the wetting time, is recorded.
TABLE 1
| Solubility (%) | Time of infiltration(s) | |
| Example 1 | 97.60 | 26.99 |
| Example 2 | 98.03 | 24.89 |
| Example 3 | 97.99 | 28.65 |
| Control group 1 | 65.96 | 83.23 |
| Control group 2 | 88.17 | 31.65 |
Sensory evaluation: referring to the national standard method, 2g of the samples of examples 1-3 and comparative examples 3, 4 were taken and placed in a clean petri dish, and the petri dish was placed on qualitative filter paper and observed for color and appearance under natural light.
Determination of total flavonoids: an appropriate amount of the instant powder of seabuckthorn leaf in examples 1-3 and comparative examples 3, 4 was weighed, dissolved in 60% ethanol, added with 0.3ml of 5% sodium nitrite solution, 0.3ml of 10% aluminum nitrate solution, finally added with 2ml of 4% sodium hydroxide solution, and the absorbance value was measured at 510 nm. And accurately quantifying by using a rutin standard curve.
TABLE 2
| Total flavone content (mg/kg) | White sparrow wood alcohol content (mg/kg) | Color and groupWeave pattern | |
| Example 1 | 47.94 | 65.89 | The color is yellow green, the texture is dispersed, and the caking is avoided |
| Example 2 | 45.36 | 89.65 | The color is yellow green, the texture is dispersed, and the caking is avoided |
| Example 3 | 43.73 | 67.34 | The color is yellow green, the texture is dispersed, and the caking is avoided |
| Control group 3 | 40.68 | 56.77 | The color is yellow brown but uneven, and has slight caking |
| Control group 4 | 41.66 | 52.52 | The color is yellow brown but uneven, and has slight caking |
As can be seen from Table 1, the solubility of inventive examples 1-3 > control 1-2, and the wetting time of examples 1-3 < control 1-2, demonstrate that the invention selects maltodextrin as a drying aid, and that the wetting time is shorter and the solubility is better. The color and the tissue morphology of the invention in the examples 1-3 are obviously better than those of the control group 3-4, which shows that the invention selects the drying mode of vacuum freeze drying, the retention rate of flavone and quebrachitol is higher, the oxidation browning degree is lower, and the sensory quality is better.
The present invention is not limited to the above-mentioned embodiments, but is intended to be limited to the following embodiments, and any modifications, equivalents and modifications can be made to the above-mentioned embodiments without departing from the scope of the invention.
Claims (7)
1. A preparation method of sea buckthorn leaf freeze-dried instant powder rich in flavone and inositol substances is characterized by comprising the following steps:
(1) Crushing: naturally drying fresh folium Hippophae at room temperature in shade, pulverizing, sieving, and storing in shade.
(2) Alcohol extraction: weighing a certain amount of crushed seabuckthorn leaf powder, adding ethanol-water solution, stirring and mixing uniformly, and soaking at room temperature. Then under heating condition, ultrasound assisted extraction is performed.
(3) Concentrating under reduced pressure: filtering the mixture, removing residue to obtain extractive solution of folium Hippophae, and removing solvent by rotary evaporator to obtain pasty extract without alcohol smell.
(4) And (3) water-dissolving: adding purified water, mixing with the pasty sea buckthorn leaf extract obtained in the step (3), and then performing ultrasonic treatment to promote the full dissolution of the wall-sticking extract. And finally, adding maltodextrin into the aqueous solution of the extract to obtain a mixed material liquid of the sea buckthorn leaf extract and the maltodextrin.
(5) Pre-freezing: tiling the sea buckthorn leaf extract and maltodextrin mixed liquid obtained in the step (4), and pre-freezing in a low-temperature refrigerator.
(6) Vacuum freeze drying: drying the pre-frozen material obtained in the step (5) in a vacuum and low-temperature environment.
2. The method for preparing the seabuckthorn leaf freeze-dried instant powder rich in flavone and inositol according to claim 1, wherein the ethanol extraction liquid ratio of the step (2) is between 1:25 and 1:35 (g: mL).
3. The method for preparing the seabuckthorn leaf freeze-dried instant powder rich in flavone and inositol according to claim 1, wherein the volume fraction of the ethanol-water solution in the step (2) is 50-90%.
4. The method for preparing the seabuckthorn leaf freeze-dried instant powder rich in flavone and inositol according to claim 1, wherein the heating temperature of ultrasonic-assisted extraction in the step (2) is 40-50 ℃ and the extraction time is 40-50min.
5. The method for preparing the seabuckthorn leaf freeze-dried instant powder rich in flavone and inositol substances according to claim 1, wherein the water bath temperature of the rotary evaporator in the step (3) is 40-50 ℃ during the reduced pressure concentration.
6. The method for preparing the seabuckthorn leaf freeze-dried instant powder rich in flavone and inositol substances according to claim 1, wherein the mass fraction of maltodextrin added in the step (4) during water dissolution is 10-20%.
7. The method for preparing the seabuckthorn leaf freeze-dried instant powder rich in flavone and inositol substances according to claim 1, wherein the conditions in the step (6) of vacuum freeze-drying are as follows: the temperature is-45 to-50 ℃, the vacuum degree is 0-10Pa, and the freeze-drying time is 16-24h.
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