CN117982553A - Method for processing cyclocarya paliurus leaves and method for producing cyclocarya paliurus leaf products - Google Patents

Abstract

The application relates to the technical field of Chinese medicinal material processing, in particular to a processing method of cyclocarya paliurus leaves and a production method of cyclocarya paliurus leaf products. The processing method comprises the following steps: placing cyclocarya paliurus leaves in a pressure-resistant bag, and vacuumizing and sealing; and placing the vacuum-sealed cyclocarya paliurus leaves in a condition that the temperature is not more than 40 ℃ and the pressure is 100-600 MPa, and performing pressure treatment for 5-15 min. Compared with the prior art, the application has the following beneficial effects: the cyclocarya paliurus leaves are processed by adopting a specific processing technology, so that the cyclocarya paliurus leaves have good extraction effect on temperature-sensitive active ingredients, and particularly have good extraction effect on cyclocarya paliurus polysaccharide, flavone, triterpene and saponin.

Description

Method for processing cyclocarya paliurus leaves and method for producing cyclocarya paliurus leaf products

Technical Field

The application relates to the technical field of Chinese medicinal material processing, in particular to a processing method of cyclocarya paliurus leaves and a production method of cyclocarya paliurus leaf products.

Background

Cyclocarya paliurus is a special treasure plant in China, and cyclocarya paliurus leaves are sweet in taste and have the effects of clearing heat, relieving swelling, relieving pain, reducing blood sugar and the like. The main active ingredients of cyclocarya paliurus leaves are polysaccharide, flavone, triterpene and saponin, and the chemical ingredients are not high-temperature resistant and can damage the molecular stability at the temperature of more than 50 ℃.

The current cyclocarya paliurus leaf processing technology comprises the following steps: li Yanpo, ying et al, describe the method described in "optimizing conditions and antioxidant Activity of cyclocarya paliurus polysaccharides extracted under ultra high pressure": the dried cyclocarya paliurus leaves are crushed and sieved by a 40-mesh sieve. Petroleum ether (boiling range 60-90 ℃) is added according to the ratio of 1:10 (g/mL), the mixture is refluxed for 1h for degreasing, and the filter residue is filtered and dried for subsequent tests. Adding absolute ethanol at a ratio of 1:3 (g/mL), heating and refluxing in 80deg.C water bath to remove micromolecular alcohol solution, filtering, and drying the obtained residue. And (3) filling the deoiled and dealcoholized cyclocarya paliurus powder into a polyethylene composite bag according to a certain feed liquid ratio, removing air seal, placing into an ultrahigh pressure device for ultrahigh pressure treatment, filtering after pressure relief, adding 3 times of absolute ethyl alcohol, centrifuging at 8 000r/min for 10min, taking supernatant, and measuring the polysaccharide content of cyclocarya paliurus. Wang Yunbing, bao Re, and the processing flow recorded in the section I of the cyclocarya paliurus tea bag processing technology is as follows: picking fresh Shetan green, deactivating enzyme, spreading to cool, rolling, primary drying, tea frying, secondary drying, crushing, screening, grading, packaging and the like. Dong Caijun methods for measuring cyclocarya paliurus flavone and methods for extracting and separating and researching biological activity of cyclocarya paliurus flavone are disclosed. The method recorded in the "extraction and application research of cyclocarya paliurus flavonoid compounds" published by the corollary of the present invention. However, the existing processing method of cyclocarya paliurus leaves has poor extraction effect on temperature-sensitive active ingredients.

Disclosure of Invention

Based on the above, one or more embodiments of the present application provide a processing method of cyclocarya paliurus leaves, which has a good effect of extracting temperature-sensitive active ingredients.

One or more embodiments of the present application provide a method of processing cyclocarya paliurus leaves, the method comprising:

placing cyclocarya paliurus leaves in a pressure-resistant bag, and vacuumizing and sealing; and

The vacuum-sealed cyclocarya paliurus leaves are subjected to pressure treatment for 5 to 15 minutes under the conditions that the temperature is not more than 40 ℃ and the pressure is 100 to 600 MPa.

In some embodiments of the application, the cyclocarya paliurus leaves are further subjected to a drying treatment before vacuum sealing;

Optionally, the temperature of the drying process does not exceed 50 ℃; further alternatively, the temperature of the drying treatment is 23-28 ℃; still further alternatively, the drying process includes: air-drying;

optionally, the moisture content of the dried cyclocarya paliurus leaves is not more than 12wt%.

In some embodiments of the application, the cyclocarya paliurus leaves are not crushed.

In some embodiments of the application, the conditions of the pressure treatment include:

The temperature is not more than 40 ℃;

the pressure is 100MPa to 500MPa, optionally 250MPa to 400MPa, further optionally 200MPa to 400MPa; and

The treatment time is 8min-12min.

In some embodiments of the application, before vacuum sealing, the cyclocarya paliurus leaves are not subjected to drying treatment, or the dried cyclocarya paliurus leaves are soaked with water after the drying treatment;

Optionally, the temperature of the drying process does not exceed 50 ℃; further alternatively, the temperature of the drying treatment is 23-28 ℃; still further alternatively, the drying process includes: air-drying;

Optionally, the water content of the cyclocarya paliurus leaves is 45-65wt%.

In some embodiments of the application, the conditions of the pressure treatment include:

The temperature is not more than 40 ℃;

The pressure is 100MPa to 400MPa, optionally 200MPa to 400MPa, further optionally 200MPa to 300MPa; and

The treatment time is 8min-12min.

In some embodiments of the application, before vacuum sealing, the cyclocarya paliurus leaves are subjected to drying treatment and then are further subjected to crushing treatment;

optionally, the temperature of the comminuting treatment is not more than 50 ℃;

optionally, the size of the cyclocarya paliurus leaves after the crushing treatment is 0.5 mm-4 mm.

In some embodiments of the application, the conditions of the pressure treatment include:

The temperature is not more than 40 ℃;

The pressure is 200MPa to 600MPa, and is selected to be 250MPa to 350MPa or 450MPa to 550MPa, and is further selected to be 250MPa to 350MPa; and

The treatment time is 8min-12min.

In some embodiments of the application, the material of the pressure-resistant bag comprises PE.

In some embodiments of the application, the vacuum degree of the vacuum-pumping seal is-0.05 MPa to-0.15 MPa.

Another or more embodiments of the present application provide a method of producing a cyclocarya paliurus leaf product, the method comprising the steps of:

the cyclocarya paliurus leaves are processed by adopting the processing method; and

And preparing the cyclocarya paliurus leaf product from the processed cyclocarya paliurus leaves.

In some embodiments of the application, the cyclocarya paliurus leaf product comprises tea leaves or decoction pieces of traditional Chinese medicine.

Compared with the prior art, the application has the following beneficial effects:

The cyclocarya paliurus leaves are processed by adopting a specific processing technology, so that the cyclocarya paliurus leaves have good extraction effect on temperature-sensitive active ingredients, and particularly have good extraction effect on cyclocarya paliurus polysaccharide, flavone, triterpene and saponin.

Drawings

In order to more clearly illustrate the technical solution in the embodiments of the present application and to more fully understand the present application and its advantageous effects, the following brief description will be given with reference to the accompanying drawings, which are required to be used in the description of the embodiments. It is evident that the figures in the following description are only some embodiments of the application, from which other figures can be obtained without inventive effort for a person skilled in the art.

FIG. 1 is a diagram showing the result of scanning electron microscopy observation of the structures of cyclocarya paliurus cells treated with different pressures;

fig. 2 shows the color detection results corresponding to the cyclocarya paliurus leaves subjected to different pressure treatments.

Detailed Description

The present application will be described in further detail with reference to the drawings, embodiments and examples. It should be understood that these embodiments and examples are provided solely for the purpose of illustrating the application and are not intended to limit the scope of the application in order that the present disclosure may be more thorough and complete. It will also be appreciated that the present application may be embodied in many different forms and is not limited to the embodiments and examples described herein, but may be modified or altered by persons skilled in the art without departing from the spirit of the application, and equivalents thereof are also intended to fall within the scope of the application. Furthermore, in the following description, numerous specific details are set forth in order to provide a more thorough understanding of the application, it being understood that the application may be practiced without one or more of these details.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein in the description of the application is for the purpose of describing the embodiments and examples only and is not intended to be limiting of the application.

Terminology

Unless otherwise indicated or contradicted, terms or phrases used herein have the following meanings:

The term "and/or," "and/or," as used herein, includes any one of two or more of the listed items in relation to each other, as well as any and all combinations of the listed items in relation to each other, including any two of the listed items in relation to each other, any more of the listed items in relation to each other, or all combinations of the listed items in relation to each other. It should be noted that, when at least three items are connected by a combination of at least two conjunctions selected from the group consisting of "and/or", "and/or", it should be understood that, in the present application, the technical solutions include technical solutions that all use "logical and" connection, and also include technical solutions that all use "logical or" connection. For example, "a and/or B" includes three parallel schemes A, B and a+b. For another example, the technical schemes of "a, and/or B, and/or C, and/or D" include any one of A, B, C, D (i.e., the technical schemes of all "logical or" connections), also include any and all combinations of A, B, C, D, i.e., the combinations of any two or three of A, B, C, D, and also include four combinations of A, B, C, D (i.e., the technical schemes of all "logical and" connections).

The terms "plurality", "plural", "multiple", and the like in the present application refer to, unless otherwise specified, an index of 2 or more in number. For example, "one or more" means one kind or two or more kinds.

As used herein, "a combination thereof," "any combination thereof," and the like include all suitable combinations of any two or more of the listed items.

The "suitable" in the "suitable combination manner", "suitable manner", "any suitable manner" and the like herein refers to the fact that the technical scheme of the present application can be implemented, the technical problem of the present application is solved, and the technical effect expected by the present application is achieved.

Herein, "preferred", "better", "preferred" are merely to describe better embodiments or examples, and it should be understood that they do not limit the scope of the application.

In the present application, "further", "still further", "particularly" and the like are used for descriptive purposes to indicate differences in content but should not be construed as limiting the scope of the application.

In the present application, "optional" means optional or not, that is, means any one selected from two parallel schemes of "with" or "without". If multiple "alternatives" occur in a technical solution, if no particular description exists and there is no contradiction or mutual constraint, then each "alternative" is independent.

In the present application, the terms "first", "second", "third", "fourth", etc. are used for descriptive purposes only and are not to be construed as indicating or implying a relative importance or quantity, nor as implying an importance or quantity of a technical feature being indicated. Moreover, the terms "first," "second," "third," "fourth," and the like are used for non-exhaustive list description purposes only, and are not to be construed as limiting the number of closed forms.

In the application, the technical characteristics described in an open mode comprise a closed technical scheme composed of the listed characteristics and also comprise an open technical scheme comprising the listed characteristics.

In the present application, a numerical range (i.e., a numerical range) is referred to, and optional numerical distributions are considered to be continuous within the numerical range and include two numerical endpoints (i.e., a minimum value and a maximum value) of the numerical range and each numerical value between the two numerical endpoints unless otherwise specified. Where a numerical range merely refers to integers within the numerical range, including both end integers of the numerical range, and each integer between the two ends, unless otherwise indicated, each integer is recited herein as directly, such as where t is an integer selected from 1 to 10, and where t is any integer selected from the group of integers consisting of 1,2,3, 4, 5, 6, 7, 8, 9, and 10. Further, when a plurality of range description features or characteristics are provided, these ranges may be combined. In other words, unless otherwise indicated, the ranges disclosed herein are to be understood to include any and all subranges subsumed therein.

The temperature parameter in the present application is not particularly limited, and may be a constant temperature treatment or may vary within a predetermined temperature range. It should be appreciated that the constant temperature process described allows the temperature to fluctuate within the accuracy of the instrument control. Allows for fluctuations within a range such as + -5 ℃, + -4 ℃, + -3 ℃, + -2 ℃, + -1 ℃.

In the present application,% (w/w) and wt% each represent weight percent,% (v/v) represents volume percent, and% (w/v) represents mass volume percent.

One or more embodiments of the present application provide a processing method of cyclocarya paliurus leaves, the processing method comprising:

placing cyclocarya paliurus leaves in a pressure-resistant bag, and vacuumizing and sealing; and

The vacuum-sealed cyclocarya paliurus leaves are subjected to pressure treatment for 5min to 15min (for example, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14 and 15 min) under the condition that the temperature is not more than 40 ℃ (for example, 4、5、6、7、8、9、10、11、12、13、14、15、16、17、18、19、20、21、22、23、24、25、26、27、28、29、30、31、32、33、34、35、36、37、38、39、40℃)、 the pressure is 100MPa to 600MPa (for example, 100, 125, 150, 175, 200, 225, 250, 275, 300, 325, 350, 375, 400, 425, 450, 475, 500, 525, 550, 575 and 600 MPa).

The cyclocarya paliurus leaves of the present application are not particularly limited, and may be fresh cyclocarya paliurus leaves, dried cyclocarya paliurus leaves, cyclocarya paliurus leaves without pulverization, or pulverized cyclocarya paliurus leaves. According to the actual requirements, suitable cyclocarya paliurus leaves can be selected, for example, fresh cyclocarya paliurus leaves are not easy to store and transport, the cyclocarya paliurus leaves subjected to drying treatment can be adopted, for example, efficiency and the like can be considered, and the crushed cyclocarya paliurus leaves can be selected.

In some examples, the cyclocarya paliurus leaves are also subjected to a drying treatment before vacuum sealing; optionally, the temperature of the drying process does not exceed 50 ℃ (e.g., 50, 45, 40, 35, 30, 25, 20, 15, 10, 5, 0, -5 ℃); further alternatively, the drying process is at a temperature of from 23 ℃ to 28 ℃ (e.g., 23, 24, 25, 26, 27, 28 ℃); still further alternatively, the drying process includes: air-drying; optionally, the moisture content of the dried cyclocarya paliurus leaves is no more than 12wt% (e.g., 0wt%, 1wt%, 2wt%, 3wt%, 4wt%, 5wt%, 6wt%, 7wt%, 8wt%, 9wt%, 10wt%, 11wt%, 12 wt%).

In some examples, the cyclocarya paliurus leaves are not crushed.

In some examples, the conditions of the pressure treatment include:

The temperature is not more than 40 ℃;

the pressure is 100MPa to 500MPa, optionally 250MPa to 400MPa, further optionally 200MPa to 400MPa; and

The treatment time is 8min-12min.

In some examples, before vacuum sealing, the cyclocarya paliurus leaves are not dried, or the dried cyclocarya paliurus leaves are soaked with water after the drying treatment;

Optionally, the temperature of the drying process does not exceed 50 ℃; further alternatively, the temperature of the drying treatment is 23-28 ℃; still further alternatively, the drying process includes: air-drying;

Optionally, the water content of the cyclocarya paliurus leaves is 45-65wt%.

In some examples, the conditions of the pressure treatment include:

The temperature is not more than 40 ℃;

The pressure is 100MPa to 400MPa, optionally 200MPa to 400MPa, further optionally 200MPa to 300MPa; and

The treatment time is 8min-12min.

In some examples, before vacuum sealing, the cyclocarya paliurus leaves are subjected to drying treatment and then are further subjected to crushing treatment;

optionally, the temperature of the comminuting treatment is not more than 50 ℃;

optionally, the size of the cyclocarya paliurus leaves after the crushing treatment is 0.5 mm-4 mm.

In some examples, the conditions of the pressure treatment include:

The temperature is not more than 40 ℃;

The pressure is 200MPa to 600MPa, and is selected to be 250MPa to 350MPa or 450MPa to 550MPa, and is further selected to be 250MPa to 350MPa; and

The treatment time is 8min-12min.

The material of the pressure-resistant bag is not particularly limited, and includes, but is not limited to, PE. The cyclocarya paliurus leaves of the application can be used for preparing tea or decoction pieces after being processed, and it is understood that the pressure-resistant bag is selected from food grades.

In some examples, the vacuum degree of the vacuum-pumping seal is-0.05 MPa to-0.15 MPa.

Another or more embodiments of the present application provide a method of producing a cyclocarya paliurus leaf product, the method comprising the steps of:

the cyclocarya paliurus leaves are processed by adopting the processing method; and

And preparing the cyclocarya paliurus leaf product from the processed cyclocarya paliurus leaves.

Optionally, the cyclocarya paliurus leaf product comprises tea leaves or Chinese medicinal decoction pieces.

Embodiments of the present application will be described in detail below with reference to examples. It is to be understood that these examples are illustrative of the present application and are not intended to limit the scope of the present application. The experimental methods in the following examples, in which specific conditions are not noted, are preferably referred to the guidelines given in the present application, and may be according to the experimental manual or conventional conditions in the art, the conditions suggested by the manufacturer, or the experimental methods known in the art.

In the specific examples described below, the measurement parameters relating to the raw material components, unless otherwise specified, may have fine deviations within the accuracy of weighing. Temperature and time parameters are involved, allowing acceptable deviations from instrument testing accuracy or operational accuracy.

Example 1

1. Materials and methods

1.1 Materials and instruments

Fresh cyclocarya paliurus leaves are collected at a cyclocarya paliurus Liu Chong planting base, air-dried at normal temperature (the water content is 10.38%), and then crushed (the crushing temperature is not more than 50 ℃) to form mixed powder with the particle size of 0.5-4 mm. Ultra-high pressure equipment (Tianjin Hua Thiessen vast Biotechnology Co., ltd., HPPL-500/10), ultraviolet spectrophotometers (Shanghai Meinada, UV-1800), microplate reader (U.S. Molecular devices, spectraMax i3 x), scanning electron microscopy (Zeiss, EVO 10).

1.2 Test methods

1.2.1 Ultra-high pressure treatment of cyclocarya paliurus leaves

The dried cyclocarya paliurus leaves are divided into a group (wet-pressed leaf group) soaked with pure water and a group (dry-pressed leaf group) soaked with no pure water, the wet-pressed leaf group, the dry-pressed leaf group and cyclocarya paliurus leaves are respectively placed in PE vacuum packaging bags, vacuum is rapidly extracted, 100, 200, 300, 400, 500 and 600MPa pressure treatment is carried out for 10min (the temperature is not more than 40 ℃), and then the vacuum packaging bags are sealed.

The corresponding infiltration steps of the leaf wet pressing group comprise: pure water is mixed with the air-dried cyclocarya paliurus leaves to make the water content of the cyclocarya paliurus leaves about 50% after water absorption.

1.2.2 Scanning Electron microscope observations

Taking a proper amount of the sample, adding 2.5% glutaraldehyde fixing solution with 40 times of volume, fixing in a refrigerator at 4 ℃ for more than 2 hours, washing with Phosphate Buffer Solution (PBS) for 3 times, and carrying out gradient dehydration with 50% (1 time), 70% (1 time) (4 ℃ overnight), 90% (1 time) and 100% (3 times) ethanol in sequence for 20min each time, wherein the dehydration time is 10min each time. Finally, 20. Mu.l of absolute ethanol was used to keep the sample in a wet state. And (5) drying for 1.5 hours by using a carbon dioxide critical point dryer, and taking a proper amount of samples to be adhered to a metal sample holder. The sample was gold-plated by ion sputtering, and an image was collected using a Zeiss EVO 10 scanning electron microscope.

1.2.3 Colony counts

Firstly, drying the sample soaked with pure water at 40 ℃, weighing 1g of each sample, adding 10ml of PBS, shaking for 5min, diluting the liquid with PBS according to 10 times, 100 times and 1000 times, respectively taking 100ul of the diluted liquid, coating the diluted liquid on PCA (Plate Count Agar) flat plates, and culturing overnight at 37 ℃.

1.2.4 Reflux extraction

5G of cyclocarya paliurus leaf samples treated under different pressures (wherein the wet pressed group of leaves is air-dried at normal temperature until the water content is about 10% and then reflux-extracted) are weighed, 50ml of pure water is respectively added, reflux-extraction is carried out at 40 ℃ for 1h, and the supernatant is collected after filtration with gauze. 50ml of pure water was added to the residue, extraction was repeated once, and the filtrates were combined.

1.2.5 Analysis of total polysaccharide content of cyclocarya paliurus leaf extract

The total polysaccharide content in cyclocarya paliurus leaves is measured according to the ultraviolet-visible spectrophotometry of the general rule 0401 of the edition of Chinese pharmacopoeia 2020. Firstly, 0.10ml, 0.20ml, 0.40ml, 0.60ml, 0.80ml and 1.00ml of 0.13mg/ml D-glucose standard solution are precisely sucked into a 10.00ml colorimetric tube, pure water is added to 2.00ml, 1.00ml of 5% phenol (w/v) solution is added, then 5.00ml of concentrated sulfuric acid is rapidly added, the mixture is boiled in boiling water for 15min, cooled to room temperature, reagent blank is taken as a reference, and the absorbance value is measured at the wavelength of 490 nm. And drawing a standard curve by taking the absorbance value as an ordinate and the glucose concentration as an abscissa. 1ml of the above extract was diluted 10-fold with pure water. Precisely sucking 1.0ml of the sample solution, placing in a 10.0ml colorimetric tube, and measuring the absorbance value of each sample by adopting the method.

1.2.6 Analysis of total flavone content of cyclocarya paliurus leaf extract

The total flavone content in cyclocarya paliurus leaves is measured according to the ultraviolet-visible spectrophotometry of the general rule 0401 of the edition of Chinese pharmacopoeia 2020. Firstly, drawing a standard curve: precisely weighing 0.2mg/ml of rutin solution lml, 2ml, 3ml, 4ml, 5ml and 6ml, respectively placing into 25ml measuring flask, respectively adding water to 6ml, adding 1ml of 5% sodium nitrite (w/v) solution, shaking uniformly, standing for 6min, adding 1ml of 10% aluminum nitrate (w/v) solution, shaking uniformly, standing for 6min, adding 10ml of 4% NaOH (w/v) solution, adding pure water to scale, shaking uniformly, standing for 15min, taking corresponding reagent as blank, immediately measuring absorbance at a wavelength of 500nm according to ultraviolet-visible spectrophotometry, taking absorbance as ordinate, taking concentration as abscissa, and drawing a standard curve. 1ml of the above extract was diluted 10-fold with pure water. 3.0ml of the extract was precisely aspirated and placed in 25ml, and the absorbance value of each sample was measured by the above method.

1.2.7 Analysis of total triterpene content of cyclocarya paliurus leaf extract

The total triterpene content in cyclocarya paliurus leaves is measured according to the ultraviolet-visible spectrophotometry of the general rule 0401 of the edition of Chinese pharmacopoeia 2020. Firstly, drawing a standard curve: precisely weighing 0.25mg/ml ursolic acid 0.1ml,0.2ml,0.3ml,0.4ml,0.5ml and 0.6ml, placing in a 10ml measuring flask, adding 0.5ml 5% vanillin-glacial acetic acid (w/v) and 1.2ml perchloric acid (analytically pure), mixing uniformly, sealing, heating in a 70 ℃ constant-temperature water bath for 15min, taking out cold water, cooling to room temperature, metering the volume of ethyl acetate, shaking uniformly, taking the corresponding reagent as a blank control, measuring absorbance value at 550nm, taking absorbance as an ordinate, taking the standard concentration as an abscissa, and drawing a standard curve. 1ml of the above extract was diluted 10-fold with pure water, 0.4ml of the extract solution was precisely sucked, and the absorbance value of each sample was measured by the above method.

1.2.9 Analysis of total saponins content of cyclocarya paliurus leaf extract

The total saponin content in cyclocarya paliurus leaves is measured according to the ultraviolet-visible spectrophotometry of the general rule 0401 of the edition of Chinese pharmacopoeia 2020. Firstly, drawing a standard curve: sucking 0.215mg/mL of diosgenin 0.1mL,0.2mL,0.3mL,0.4mL,0.5mL and 0.6mL into a test tube, volatilizing dry ethanol, adding 4mL of H ₂SO₄, taking concentrated H ₂SO₄ as a blank control, placing into a water bath kettle, maintaining at 70 ℃ for 30min, then carrying out ice water bath for 10min, terminating the reaction, measuring the absorbance at 410nm, taking the absorbance as an ordinate, taking the concentration of a standard substance as an abscissa, and drawing a standard curve. Taking 0.3ml of the above extract, volatilizing the liquid, and measuring the absorbance value of each sample by the above method.

1.3 Statistical analysis

Statistical analysis was performed using GRAPHPAD PRISM Project, and comparison between the two groups was statistically significant using a two-tailed t-test, with P <0.05 indicating differences.

1.4 Taste and color detection

Referring to item 1.2.1, the cyclocarya paliurus leaves are subjected to ultrahigh pressure treatment, the air-dried cyclocarya paliurus leaves are directly placed in a PE vacuum packaging bag without being crushed, vacuum is rapidly extracted, and 100, 200, 300, 400, 500 and 600MPa pressure treatment is performed for 10min. While the non-ultra-high pressure treatment was used as a control.

3G of cyclocarya paliurus leaves in each group are soaked in 400ml of water at 90 ℃ for 3 minutes, 5 minutes and 10 minutes, and then the taste and the color of the cyclocarya paliurus leaves at each soaking time level are detected.

2. Results

2.1 Cell Structure of cyclocarya paliurus leaves treated with different pressures

Fig. 1 is a diagram showing the results of scanning electron microscopy observation of structures of cyclocarya paliurus cells treated with different pressures, and fig. 1 shows:

The first row is a diagram and a diagram b in turn, and corresponds to cyclocarya paliurus leaves and leaf powder which are air-dried at normal temperature respectively; the second row is a graph c, a graph d and a graph e in sequence, the third row is a graph f, a graph g and a graph h in sequence, and the leaves corresponding to the graphs c to h are respectively subjected to pressure treatment of 100MPa, 200MPa, 300MPa, 400MPa, 500MPa and 600MPa after being soaked in pure water; the fourth row is i diagram, j diagram and k diagram in turn, the fifth row is l diagram, m diagram and n diagram in turn, and the leaves corresponding to the i diagram to the n diagram are respectively subjected to 100MPa, 200MPa, 300MPa, 400MPa, 500MPa and 600MPa pressure treatment; the sixth row is an o diagram, a p diagram and a q diagram in turn, the seventh row is an r diagram, an s diagram and a t diagram in turn, and leaf powder corresponding to the o diagram to the t diagram is respectively subjected to 100MPa, 200MPa, 300MPa, 400MPa, 500MPa and 600MPa pressure treatment.

The cell structures of cyclocarya paliurus leaves (a diagram in fig. 1) and powder (b diagram in fig. 1) which are not subjected to pressure treatment are normal, and the cell structures are full.

The cell structure of cyclocarya paliurus leaves (c to h in FIG. 1) treated with pure water and 100-600Mpa is deformed by extrusion, and the degree of damage to the cell structure of the leaves increases as the pressure increases. After the pressure is increased to 400-600 MPa, the cell wall is tightly wrapped with the cell content under the influence of the ultra-high pressure. Cyclocarya paliurus leaves (fig. 1, i to n) subjected to different pressure treatments without pure water are gradually damaged as the pressure increases. The gaps are still reserved between the leaf cells at 100MPa and 200MPa, so that the relatively normal cell morphology is seen, the cells shrink after the pressure reaches 300MPa, the structure is obviously destroyed, and the leaf cells are severely extruded and shrink and deform after the pressure reaches 400MPa-600 MPa.

After the cyclocarya paliurus leaf powder is subjected to different pressure treatments, cells deform to different degrees, and the cells deform to different degrees (o-t in fig. 1). When the pressure treatment is carried out under 100MPa-200MPa, the cyclocarya paliurus leaf powder can be seen to have distortion deformation on cell structures such as palisade tissues, spongy tissues and the like. When the pressure reaches 300MPa-400MPa, the cyclocarya paliurus leaf powder tissues and cells are severely extruded, and almost no gaps exist between the cells. When the pressure reaches 500-600 MPa, the cyclocarya paliurus leaf powder tissues and cells are more compact and are fragmented, and the whole cell morphology is not presented.

2.2 Analysis of the content of the Main ingredients of cyclocarya paliurus leaves treated with different pressures

Adding pure water and 100-300 MPa of the cyclocarya paliurus leaf extract, wherein the contents of polysaccharide, flavone, triterpene and saponin increase with increasing pressure, and the contents of the main components show a decreasing trend with increasing pressure after increasing pressure to 400-600 MPa, so that the content of saponin is obviously decreased compared with that of unpressurized groups.

The contents of polysaccharide, flavone, triterpene and saponin in the cyclocarya paliurus leaf extract which is not added with pure water and is directly treated by 100MPa-300MPa are increased along with the increase of pressure, and after the pressure is increased to 400MPa-600MPa, the contents of the main components are reduced along with the increase of pressure, but the contents of the main components of all pressurized groups are obviously higher than those of the unpressurized groups.

After cyclocarya paliurus leaf powder is subjected to different pressure treatments, the contents of polysaccharide, flavone, triterpene and saponin in the extracting solution are obviously increased compared with those in unpressurized groups. At a pressure of 300MPa, the content of the main component is increased to the highest, and after the pressure is increased to 400MPa to 600MPa, the content of the main component is not increased continuously.

The above results indicate that the polysaccharide, flavone, triterpene and saponin content in the extract is highest when the cyclocarya paliurus leaves or the powder is subjected to 300MPa pressure, and the content of the main component cannot be increased continuously after the pressure is increased continuously. In combination with electron microscopy, the possible reason is that after the pressure is increased to 400MPa, the leaf or powder is severely squeezed, and the cell wall tightly wraps the cell contents, which is disadvantageous for the precipitation of the main component.

TABLE 1 content of principal Components of cyclocarya paliurus leaves treated with different pressures

Note that P <0.05 and P <0.01 are indicated compared to the corresponding non-pressure treated group.

2.3 Total number of colonies of cyclocarya paliurus leaves treated with different pressures

The cyclocarya paliurus leaves which are not subjected to pressure treatment contain 2.00 multiplied by 10 ² CFU/g of bacteria, the colony count of cyclocarya paliurus leaves which are added with pure water and subjected to 100MPa treatment is obviously increased compared with those of cyclocarya paliurus leaves which are not subjected to pressure treatment, and the possible reasons are that the survival and the reproduction of bacteria on the leaves are facilitated after the water is added, but the pressure of 100MPa is insufficient to kill all bacteria, so that the colony count is obviously increased. When the pressure is increased to 200MPa-300MPa, the colony count is significantly reduced compared with 100MPa, but a small amount of bacteria still exist. After the pressure increased to 400MPa-600MPa, no colony was detected, indicating that bacteria and fungi were all killed.

The cyclocarya paliurus leaves which are not added with pure water and are directly treated by 100MPa-600MPa still have a small amount of bacteria and fungi only when the pressure is 100MPa, and after the pressure is increased to 200MPa-600MPa, bacterial colonies are not detected in the cyclocarya paliurus leaves, which indicates that the bacteria and the fungi are completely killed at the moment.

The cyclocarya paliurus leaf powder contains 2.20X10 ⁴ CFU/g bacteria, when the powder is subjected to 100MPa-300MPa pressure, the colony count is reduced along with the increase of the pressure, and when the pressure is 400MPa-600MPa, no colony is detected in the cyclocarya paliurus leaf powder, which indicates that the bacteria and fungi are all killed at the moment.

TABLE 2 colony count of cyclocarya paliurus leaves treated with different pressures

Note that P <0.05 and P <0.01 compared to the corresponding non-pressure treated group

In combination, the cyclocarya paliurus leaves or powder is treated under the pressure of 300MPa by combining the scanning electron microscope, the main component content, the colony count result and the economic benefit, so that the precipitation of polysaccharide, flavone, triterpene and saponin is facilitated, and the bacterial count of cyclocarya paliurus leaves or powder can be killed, thereby achieving the fresh-keeping effect.

2.4 Taste and color detection

TABLE 3 Table 3

The cyclocarya paliurus has gradually reduced bitter taste with increasing pressure, and has very moderate 300MPa taste and little bitter taste processed at 400MPa and 500MPa after 300 MPa.

As can be seen from the upper graph and color code comparison, the wall breaking effect of 300MPa is optimal, and the color change is most obvious.

[ Color card ] refer to GB/T5608-1995 "China color System".

According to experimental data of the embodiment of the application, cyclocarya paliurus leaves processed at 300MPa to 400MPa and cyclocarya paliurus leaf powder can meet the colony count sanitary standard in food standards, and the overflowed effective chemical components after wall breaking are all over 2 times to 3 times, especially, after cyclocarya paliurus Liu Ganshe is processed at 300MPa pressure (10 minutes), polysaccharide overflows nearly 10 times than that of unprocessed cyclocarya paliurus leaves (the polysaccharide plays a biological activity role in aspects of resisting tumor, resisting inflammation, resisting virus, reducing blood sugar, resisting aging, resisting coagulation, promoting immunity and the like).

The technical features of the above-described embodiments and examples may be combined in any suitable manner, and for brevity of description, all of the possible combinations of the technical features of the above-described embodiments and examples are not described, however, as long as there is no contradiction between the combinations of the technical features, they should be considered to be within the scope described in the present specification.

The above examples merely illustrate a few embodiments of the present application, which are convenient for a specific and detailed understanding of the technical solutions of the present application, but should not be construed as limiting the scope of the claims. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the application, which are all within the scope of the application. Further, it is understood that various changes and modifications of the present application may be made by those skilled in the art after reading the above teachings, and equivalents thereof are intended to fall within the scope of the present application. It should also be understood that, based on the technical solutions provided by the present application, those skilled in the art obtain technical solutions through logical analysis, reasoning or limited experiments, all of which are within the scope of protection of the appended claims. The scope of the patent is therefore intended to be covered by the appended claims, and the description and drawings may be interpreted as illustrative of the contents of the claims.

Claims (10)

1. The processing method of cyclocarya paliurus leaves is characterized by comprising the following steps of:

placing cyclocarya paliurus leaves in a pressure-resistant bag, and vacuumizing and sealing; and

The vacuum-sealed cyclocarya paliurus leaves are subjected to pressure treatment for 5 to 15 minutes under the conditions that the temperature is not more than 40 ℃ and the pressure is 100 to 600 MPa.

2. The method according to claim 1, wherein before vacuum sealing, the cyclocarya paliurus leaves are further dried;

Optionally, the temperature of the drying process does not exceed 50 ℃; further alternatively, the temperature of the drying treatment is 23-28 ℃; still further alternatively, the drying process includes: air-drying;

optionally, the moisture content of the dried cyclocarya paliurus leaves is not more than 12wt%.

3. The method of producing cyclocarya paliurus leaves according to claim 2, wherein the cyclocarya paliurus leaves are not subjected to pulverization treatment.

4. The method of processing cyclocarya paliurus leaves according to claim 3, wherein the condition of the pressurizing treatment comprises:

The temperature is not more than 40 ℃;

the pressure is 100MPa to 500MPa, optionally 250MPa to 400MPa, further optionally 200MPa to 400MPa; and

The treatment time is 8min-12min.

5. The method according to claim 1, wherein before vacuum sealing, the cyclocarya paliurus leaves are not dried or are soaked with water after the drying treatment;

Optionally, the temperature of the drying process does not exceed 50 ℃; further alternatively, the temperature of the drying treatment is 23-28 ℃; still further alternatively, the drying process includes: air-drying;

Optionally, the water content of the cyclocarya paliurus leaves is 45-65wt%.

6. The method of processing cyclocarya paliurus leaves according to claim 5, wherein the condition of the pressurizing treatment comprises:

The temperature is not more than 40 ℃;

The pressure is 100MPa to 400MPa, optionally 200MPa to 400MPa, further optionally 200MPa to 300MPa; and

The treatment time is 8min-12min.

7. The method according to claim 2, wherein before vacuum sealing, the cyclocarya paliurus leaves are dried and then crushed;

optionally, the temperature of the comminuting treatment is not more than 50 ℃;

optionally, the size of the cyclocarya paliurus leaves after the crushing treatment is 0.5 mm-4 mm.

8. The method of processing cyclocarya paliurus leaves according to claim 7, wherein the condition of the pressurizing treatment comprises:

The temperature is not more than 40 ℃;

The pressure is 200MPa to 600MPa, and is selected to be 250MPa to 350MPa or 450MPa to 550MPa, and is further selected to be 250MPa to 350MPa; and

The treatment time is 8min-12min.

9. The method according to any one of claims 1 to 8, wherein the pressure-resistant bag is made of PE; or/and the vacuum degree of the vacuumized sealing is-0.05 MPa to-0.15 MPa.

10. The production method of the cyclocarya paliurus leaf product is characterized by comprising the following steps of:

processing cyclocarya paliurus leaves by the processing method of any one of claims 1 to 9; and

Preparing cyclocarya paliurus leaf products by using processed cyclocarya paliurus leaves;

optionally, the cyclocarya paliurus leaf product comprises tea leaves or Chinese medicinal decoction pieces.