CN117959352B - Method for synergistically improving gallic acid content in phyllanthus emblica through temperature and humidity co-excitation and application of method - Google Patents
Method for synergistically improving gallic acid content in phyllanthus emblica through temperature and humidity co-excitation and application of method Download PDFInfo
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- 235000004515 gallic acid Nutrition 0.000 title claims abstract description 63
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- Preparation Of Fruits And Vegetables (AREA)
Abstract
The invention belongs to the technical field of medicines, and discloses a method for improving the content of gallic acid in phyllanthus emblica by temperature and humidity co-excitation and application thereof, wherein the method comprises the following steps: selecting phyllanthus emblica raw materials, cleaning, screening, slicing, regulating and controlling moisture content, treating by adopting a temperature and humidity co-excitation technology, vacuumizing, packaging and storing. The method of the invention adopts the temperature-humidity co-excitation technology to increase the gallic acid content in the phyllanthus emblica processed from 4.41mg/g to about 100mg/g, increases more than 20 times, is obviously higher than the requirement of Chinese pharmacopoeia (not less than 1.2) (namely 12 mg/g), and provides theoretical basis and technical support for energizing the economic value of the phyllanthus emblica. The method is based on the principle of temperature and humidity co-excitation, can efficiently improve the conversion of tannic acid in phyllanthus emblica into gallic acid, shortens the processing time by 7-10 times compared with the traditional processing time, and obviously improves the content of gallic acid as an active ingredient while shortening the processing time.
Description
Technical Field
The invention belongs to the technical field of medicines, relates to processing of food and medicine homologues, and in particular relates to a method for improving the content of gallic acid in phyllanthus emblica by temperature and humidity co-excitation and application thereof.
Background
Fructus Phyllanthi is a fruit with homology of medicine and food, is rich in active substances such as flavone, phenolic acid, tannin and alkaloid, and has good antioxidant, antiinflammatory, antitumor, antibacterial, liver protecting, immunoregulatory and diabetes preventing effects. Chebular Lin Rou acid (chebulinic acid), ellagic acid (ELLAGIC ACID), 3-ethylgallic acid (3-ethoxy-GALLIC ACID), chebular mashing acid (chebulagic acid), gallic acid (GALLIC ACID, GA) and the like are main active ingredients in phyllanthus emblica, wherein chebular acid, ellagic acid, 3-ethylgallic acid and the like are polymers of gallic acid monomers and gallic tannins formed by combining gallic acid with tannic acid and polyalcohol, wherein the structural formulas of gallic acid, tannic acid and pentagallic acid acyl glucose are as follows:
Emblic leafflower fruits are rich in gallic acid and many known medicinal phytochemicals and tannins. The phyllanthus emblica has the activity of inhibiting hepatic steatosis and hepatic fibrosis in vitro; in vivo experiments also demonstrate that gallic acid can improve high fat diet induced dyslipidemia, hepatic steatosis and oxidative stress. The gallic acid has anti-inflammatory and antioxidant effects, can inhibit metastasis and proliferation of colon cancer cells, and can protect liver from being damaged by carbon tetrachloride toxicity, so that the gallic acid is a compound with high medicinal value.
Based on the requirements of the processing specifications of Chinese pharmacopoeia 2020 edition and various places of each edition, the modern processing method of the emblic leafflower fruit mainly comprises the steps of removing impurities and drying, and only the GA content in the processed emblic leafflower fruit is restricted to be not less than 1.2 percent (namely, 12mg/g in percentage by weight after processing). The processing technique is not limited.
The common drying mode of the phyllanthus emblica mainly comprises traditional processes such as sun drying, shade drying, hot air drying, vacuum freeze drying and the like, and novel drying modes such as microwave, far infrared and inert particle fluidized bed and the like. Natural sunlight is used for drying, so that the equipment is simple and the cost is low; however, due to weather conditions, long-term sunshine is required, pollution caused by dust and pollutants is easy to occur, and nutrients in food are easy to lose. The drying in the shade is not limited by weather conditions, can be carried out indoors, and has simple equipment and low cost; but has slow drying speed and long drying time, and is easy to cause mildew and deterioration of food and loss of nutrient components. Both of these drying modes present a risk of microbial and insect infestation. The hot air drying and the drying are less influenced by natural factors such as weather, climate and the like, the drying temperature is convenient to control according to different pharmacodynamic characteristics, partial bacteria and microorganisms can be killed, the sanitary quality of food is improved, the operation is simple, the production cost is low, the energy consumption is lower than that of vacuum freeze drying, the method is suitable for industrial large-scale production, and partial nutrient substances can be decomposed. The novel drying modes such as microwaves, far infrared and inert particle fluidized beds have the problems of high equipment requirement, high production cost and the like, and are not widely applied on a large scale. The above methods have low extraction efficiency for improving the gallic acid as the target compound in the product.
In summary, the following technical problems exist in the prior art:
Firstly, the traditional processing technology mainly comprises sun drying. The traditional processed fructus Phyllanthi has the risk of GA content being insufficient (0.3-1.1% by weight) and lower than the quality standard (1.2% by weight) of medicines. Secondly, the sun-drying is carried out until the moisture content is below 13%, generally 7-10 days (sunny days), and if the sun-drying is carried out in overcast and rainy days, the sun-drying cannot be dried and is accompanied by rot and mildew. Therefore, the traditional processing technology has low technical level, long processing period and difficult quality control, and part of innovative methods have high cost and are difficult to industrially popularize and apply.
By searching, the following patent publications related to the present patent application are found:
Comparative patent 1:
Aiming at the problem that the phyllanthus emblica processed by the traditional processing technology has insufficient gallic acid content and is lower than the risk of drug quality standard, chinese patent document CN108936705A discloses a phyllanthus emblica deep processing method and a phyllanthus emblica stoning device (publication date: 2018, 12 months and 7 days), the dried phyllanthus emblica powder is prepared into a solid culture medium, and one or any combination of aspergillus oryzae, aspergillus niger, rhizopus oryzae and mucor is inoculated after sterilization for fermentation culture for 15 days, and a finished product is obtained after fermentation is finished by low-temperature drying.
Problems: (1) The fermentation mode has the advantages of large investment in the earlier stage, high cost, large technical difficulty and high cost per batch time, and has limitation on the production of large-batch phyllanthus emblica with high gallic acid content; (2) After the fermentation is finished, the method is directly subjected to low-temperature drying treatment, no sterilization operation is performed, wherein the mould and spores thereof still have activity, and the product development of the phyllanthus emblica produced by the mould and spores thereof in the later stage can cause the adverse effect of high pretreatment cost; (3) The metabolite mycotoxin produced by mould fermentation may cause central nervous system poisoning, so that the human body has the symptoms of convulsion, dizziness, muscle paralysis, convulsion, and the like, and the production cost is increased in the subsequent food processing.
Comparative patent 2:
Aiming at the problems of low technical level and difficult quality control of the processing technology, the Chinese patent document CN102274270A discloses a processing technology of traditional Chinese medicine phyllanthus emblica (the publication date is 14 days of 12 months of 2011), and the phyllanthus emblica slices are produced by adopting a vacuum freeze-drying method, wherein the production period of each batch is about 24-28 hours, and the medicinal components and the quality of the dried materials of the phyllanthus emblica can be reserved to a greater extent.
Problems: the prior researches show that the vacuum freeze drying can effectively retain various nutritional components of the emblic leafflower fruit, but has no obvious effect on improving the content of the effective medicinal components of the emblic leafflower fruit, namely gallic acid.
The content of gallic acid in fresh phyllanthus emblica is low, and the cost for producing gallic acid by industrialized separation and purification is high and the economic value is low. The lack of processing parameters (fresh dry fructus Phyllanthi, processing auxiliary materials, processing time, etc.) of fructus Phyllanthi in the processing specification of the Chinese pharmacopoeia in 2020 edition and various provinces can cause large quality difference of decoction pieces and influence the clinical effectiveness. Therefore, the reasonable, standard and controllable phyllanthus emblica processing technology and technological parameters are established, the processing time is shortened, and the gallic acid release efficiency is improved, so that the technical problem to be solved at present is primarily solved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides a method for synergistically improving the content of gallic acid in phyllanthus emblica by temperature and humidity co-excitation and application thereof.
The technical scheme adopted for solving the technical problems is as follows:
a method for synergistically improving the content of gallic acid in phyllanthus emblica through temperature and humidity co-excitation comprises the following steps:
Selecting phyllanthus emblica raw materials, cleaning, screening, slicing, regulating and controlling moisture content, treating by adopting a temperature and humidity co-excitation technology, vacuumizing, packaging and storing;
The specific treatment steps of the temperature-humidity co-excitation technology treatment are as follows:
① Regulating and controlling the moisture content: the emblic leafflower fruit slices are subjected to dishing, the dishing weight is 10-11 kg/m 2, the thickness is 1.5-2.5 cm, and the pre-freezing is carried out for 1.5-2.5 hours at the temperature of minus 20 ℃ to minus 80 ℃; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting heating to 40-70 ℃, and sublimating and drying for 13-20 hours; keeping the temperature of the materials at 25-45 ℃, regulating and controlling the moisture content of the phyllanthus emblica slices to 8-40%, and discharging;
② And (3) drying: the emblic leafflower fruit slices with the moisture content of 8-40% are palletized, the palletizing weight is 12-15 kg/m 2, the thickness is 1-2 cm, the drying temperature is controlled at 80-130 ℃, the drying environment humidity is 8-40%, and the drying time is 2-8 h.
Further, the pre-freezing is carried out for 1.5 to 2.5 hours at the temperature of minus 20 ℃ to minus 40 ℃.
Further, the specific steps are as follows:
(1) Selecting fruits: selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with the diameter of 2.5-4 cm;
(2) Cleaning: washing the surfaces of fruits with flowing water to remove leaves and dust, and draining;
(3) Screening: cleaning, screening again, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning;
(4) Slicing: cutting phyllanthus emblica into crescent slices with the thickness of 2-6 mm;
(5) And (5) treating by a temperature-humidity co-excitation technology.
Further, the specific steps are as follows:
(1) Selecting fruits: selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with the diameter of 2.5-4 cm;
(2) Cleaning: washing the surfaces of fruits with flowing water to remove leaves and dust, and draining;
(3) Screening: cleaning, screening again, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning;
(4) Slicing: cutting phyllanthus emblica into crescent slices with the thickness of 2-6 mm;
(5) The temperature and humidity co-excitation technology treatment comprises the following specific treatment steps:
① Regulating and controlling the moisture content: the emblic leafflower fruit slices are subjected to dishing, the dishing weight is 10-11 kg/m 2, the thickness is 1.5-2.5 cm, and pre-freezing is carried out for 1.5-2.5 hours at the temperature of minus 80 ℃; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting heating to 40-70 ℃, and sublimating and drying for 13-20 h; keeping the temperature of the materials at 25-45 ℃, regulating and controlling the moisture content of the phyllanthus emblica slices to 8-40%, and discharging;
② And (3) drying: the emblic leafflower fruit slices with the moisture content of 8 to 40 percent are palletized, the palletizing weight is 12 to 15kg/m 2, the thickness is 1 to 2cm, the drying temperature is controlled to be 80 to 130 ℃, the drying environment humidity (RH) is 8 to 40 percent, and the drying time is 2 to 8 hours;
(6) And (5) vacuumizing, packaging and storing.
Further, the phyllanthus emblica is of a noble plateau region of China.
The use of the method described above in the preparation of gallic acid.
The invention has the advantages and positive effects that:
1. The method adopts the temperature and humidity co-excitation technology to improve the content of Gallic Acid (GA) in the phyllanthus emblica which is processed from 4.41mg/g to about 100mg/g, increases more than 20 times, is obviously higher than the requirement of Chinese pharmacopoeia (namely 12 mg/g) by not less than 1.2 percent, and provides theoretical basis and technical support for energizing the economic value of the phyllanthus emblica. The method is based on the principle of temperature-humidity co-excitation, can efficiently improve the conversion of tannic acid in phyllanthus emblica to GA, dries until the moisture content is lower than 13% (weight percent) in the sun, takes about 7-10 days, and achieves about 24 hours when the phyllanthus emblica processed by the temperature-humidity co-excitation technology is used under the same moisture content, the time cost is shortened by 7-10 times, and the content of the active ingredient GA can be obviously improved while the processing time is shortened.
2. The moisture content of the phyllanthus emblica processed by adopting the temperature-humidity co-excitation technology is about 8% -40% when the phyllanthus emblica slices are initially dried, and the drying environment humidity is about 8% -40%, so that the stability of GA monomers and the degradation of tannins in the phyllanthus emblica are facilitated.
3. The temperature and humidity co-excitation technology of the method completely adopts a physical method, accelerates degradation of tannins (such as myrobalan acid, ellagic acid, 3-ethylgallic acid and the like in the emblic leafflower fruit) in the emblic leafflower fruit by controlling the drying environment temperature and humidity of the emblic leafflower fruit and the moisture content of the emblic leafflower fruit during initial drying, improves the GA content of the emblic leafflower fruit in a green and safe way, multiplies the content of the dried emblic leafflower acid after being treated by the technology, meets the moisture content requirement of Chinese pharmacopoeia, reduces the adverse influence and the later preservation cost of the original microorganisms in the emblic leafflower fruit, has small investment in the early stage, good repeatability and simple quality control, and is suitable for large-scale production of enterprises.
4. The phyllanthus emblica processed by adopting the temperature-humidity co-excitation processing technology is used as a processing raw material, the subsequent processing cost is low, the safety is higher, and the product has higher market competitiveness.
5. The method is based on the principle of temperature-humidity co-excitation molecular interaction, and the method promotes the conversion of tannins and tannins in the phyllanthus emblica into GA monomers by regulating and controlling the moisture content, the drying environment humidity, the drying temperature and the drying time of the phyllanthus emblica tablet so as to improve the GA content in the dried phyllanthus emblica. The technology has the advantages of simplicity, high efficiency, low cost, high yield, high safety and the like.
6. The method adopts a temperature-humidity co-excitation technology to reasonably configure the parameters such as drying time, temperature, environmental humidity and the like, so that the GA content of the phyllanthus emblica is multiplied, and the active ingredients are reserved to the greatest extent. The safety risk brought by the external pollutant dip dyeing in the drying and processing process of the emblic leafflower fruit is reduced, and the quality and the production efficiency of processed products are improved.
Drawings
FIG. 1 is a flow chart of a medium temperature and humidity co-excitation processing technology in the invention;
FIG. 2 is a graph of GA criteria in the present invention;
FIG. 3 is a graph showing the effect of different drying times on the GA content of emblic leafflower fruit after freeze-drying in the present invention;
FIG. 4 is a graph showing the effect of different processing modes on GA content in phyllanthus emblica;
FIG. 5 is a graph showing the effect of different drying humidity on GA content in the present invention; wherein RH represents the humidity of the drying environment.
Detailed Description
The invention will now be further illustrated by reference to the following examples, which are intended to be illustrative, not limiting, and are not intended to limit the scope of the invention.
The various experimental operations involved in the specific embodiments are conventional in the art, and are not specifically noted herein, and may be implemented by those skilled in the art with reference to various general specifications, technical literature or related specifications, manuals, etc. before the filing date of the present invention.
A method for synergistically improving the content of gallic acid in phyllanthus emblica through temperature and humidity co-excitation comprises the following steps:
Selecting phyllanthus emblica raw materials, cleaning, screening, slicing, regulating and controlling moisture content, treating by adopting a temperature and humidity co-excitation technology, vacuumizing, packaging and storing;
The specific treatment steps of the temperature-humidity co-excitation technology treatment are as follows:
① Regulating and controlling the moisture content: the emblic leafflower fruit slices are subjected to dishing, the dishing weight is 10-11 kg/m 2, the thickness is 1.5-2.5 cm, and the pre-freezing is carried out for 1.5-2.5 hours at the temperature of minus 20 ℃ to minus 80 ℃; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting heating to 40-70 ℃, and sublimating and drying for 13-20 hours; keeping the temperature of the materials at 25-45 ℃, regulating and controlling the moisture content of the phyllanthus emblica slices to 8-40%, and discharging;
② And (3) drying: the emblic leafflower fruit slices with the moisture content of 8-40% are palletized, the palletizing weight is 12-15 kg/m 2, the thickness is 1-2 cm, the drying temperature is controlled at 80-130 ℃, the drying environment humidity is 8-40%, and the drying time is 2-8 h.
Preferably, the pre-freezing is carried out for 1.5 to 2.5 hours at the temperature of minus 20 ℃ to minus 40 ℃.
Preferably, the specific steps are as follows:
(1) Selecting fruits: selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with the diameter of 2.5-4 cm;
(2) Cleaning: washing the surfaces of fruits with flowing water to remove leaves and dust, and draining;
(3) Screening: cleaning, screening again, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning;
(4) Slicing: cutting phyllanthus emblica into crescent slices with the thickness of 2-6 mm;
(5) And (5) treating by a temperature-humidity co-excitation technology.
Preferably, the specific steps are as follows:
(1) Selecting fruits: selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with the diameter of 2.5-4 cm;
(2) Cleaning: washing the surfaces of fruits with flowing water to remove leaves and dust, and draining;
(3) Screening: cleaning, screening again, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning;
(4) Slicing: cutting phyllanthus emblica into crescent slices with the thickness of 2-6 mm;
(5) The temperature and humidity co-excitation technology treatment comprises the following specific treatment steps:
① Regulating and controlling the moisture content: the emblic leafflower fruit slices are subjected to dishing, the dishing weight is 10-11 kg/m 2, the thickness is 1.5-2.5 cm, and pre-freezing is carried out for 1.5-2.5 hours at the temperature of minus 80 ℃; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting heating to 40-70 ℃, and sublimating and drying for 13-20 h; keeping the temperature of the materials at 25-45 ℃, regulating and controlling the moisture content of the phyllanthus emblica slices to 8-40%, and discharging;
② And (3) drying: the emblic leafflower fruit slices with the moisture content of 8-40% are palletized, the palletizing weight is 12-15 kg/m 2, the thickness is 1-2 cm, the drying temperature is controlled at 80-130 ℃, the drying environment humidity is 8-40%, and the drying time is 2-8 h;
(6) And (5) vacuumizing, packaging and storing.
Preferably, the phyllanthus emblica is of a noble plateau region of China.
The application of the method in preparing gallic acid in phyllanthus emblica is provided.
Specifically, the preparation and detection of the correlation are as follows:
Example 1
Referring to fig. 1, selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with diameters of 2.5-4 cm in the Chinese cloud precious plateau area, rinsing with running water, washing away soil, leaves and the like on the surfaces of phyllanthus emblica wild fruits, and draining; and (5) screening again after cleaning, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning. Cutting phyllanthus emblica into crescent slices with the thickness of 4mm, loading the slices with the weight of 10kg/m 2 and the thickness of 2cm, and pre-freezing the slices in a freezer at the temperature of-80 ℃ for 1.5 hours; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting to heat to 40 ℃, and sublimating and drying for 20h; keeping the temperature of the materials at 35 ℃, regulating and controlling the moisture content of the phyllanthus emblica slices to be 12+/-1%, and discharging.
And (3) drying the fresh phyllanthus emblica slices and the freeze-dried phyllanthus emblica slices (namely the treated phyllanthus emblica slices), controlling the thickness of a tray to be 1.5cm, controlling the drying temperature to be 110+/-2 ℃, controlling the drying environment humidity to be not controlled, and drying for 4, 6, 8 and 10 hours to obtain the finished product.
Pulverizing with pulverizer, sieving with 80 mesh sieve, adding processed fructus Phyllanthi powder 0.5g into 50mL centrifuge tube, adding 15mL 70% methanol solution (containing 0.1% glacial acetic acid, volume percent), standing at 60deg.C under 40Hz ultrasonic for 20min, centrifuging at 800r/min at 4deg.C for 10min, and collecting supernatant; 15mL of 70% methanol solution (containing 0.1% glacial acetic acid by volume percent) is added, the mixture is placed at 60 ℃ and the frequency is 40Hz for 20 minutes, the mixture is centrifuged at 8000r/min at 4 ℃ for 10 minutes, and the supernatants are combined; the supernatant was diluted 50-fold with a 70% methanol solution (containing 0.1% glacial acetic acid by volume) and the mobile phase and sample were filtered with 0.22 μm and 0.45 μm filters, respectively.
GA content was determined by reference to high performance liquid chromatography (chinese pharmacopoeia 2020 edition general rule 0512). The chromatographic grade GA was prepared as a standard solution at a concentration of 250. Mu.g/mL, and the standard was diluted to 15.625. Mu.g/mL with methanol in a gradient manner, and the peak area was measured. Drawing a standard curve by taking the concentration of a standard substance (mug/mL) as an abscissa and the peak area as an ordinate, and performing linear regression calculation: y=8e+07 x-73310, and r 2 =1 (wherein 8e+07 employs scientific counting, 8e+07x means 8×10 7 x, x means gallic acid concentration in standard liquid, mg/mL, and Y means liquid phase response peak area corresponding to gallic acid concentration).
As shown in FIG. 3, when the moisture content was 12%, the GA content of the emblic leafflower fruit dried at 110.+ -. 2 ℃ for 8 hours was 76.55mg/g without controlling the humidity of the drying environment, which is equivalent to the GA content (71.33 mg/g) of the fresh emblic leafflower fruit slices (i.e. emblic leafflower fruit slices not subjected to vacuum freeze-drying treatment) dried at 110.+ -. 2 ℃ for 4 hours. Showing that when the water content of the phyllanthus emblica is low, the drying time at 110+/-2 ℃ is doubled compared with the drying time required by fresh phyllanthus emblica to reach the same GA release amount.
Example 2
Referring to fig. 1, selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with diameters of 2.5-4 cm in the Chinese cloud precious plateau area, rinsing with running water, washing away soil, leaves and the like on the surfaces of phyllanthus emblica wild fruits, and draining; and (5) screening again after cleaning, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning. Then cutting phyllanthus emblica into crescent slices with the thickness of 4mm, filling the slices into a tray with the thickness of about 2cm, steaming at 100 ℃ for 4 hours, and freeze-drying until the moisture content is about 10% (weight percent).
Pre-freezing fresh phyllanthus emblica slices for 1.5 hours at-80 ℃ in a freezer, wherein the weight of the fresh phyllanthus emblica slices is 10kg/m 2, and the thickness of the fresh phyllanthus emblica slices is 2cm; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting to heat to 40 ℃, and sublimating and drying for 20h; keeping the temperature of the materials at 35 ℃, regulating and controlling the moisture content of the phyllanthus emblica slices to be 12+/-1%, and discharging.
And (3) drying the freeze-dried phyllanthus emblica slices, controlling the thickness of the tray to be 1.5cm, controlling the drying temperature to be 110+/-2 ℃, controlling the drying environment humidity not to be controlled, and drying for 4 hours to obtain a finished product.
The procedure for extraction and measurement of GA in emblic leafflower fruit was as in example 1.
As shown in fig. 4, when the heat treatment time was the same, the content of GA monomer released by the wet heat treatment (steaming at 100 ℃) was increased by about 64% as compared with that released by the dry heat treatment (baking at 110±2℃), indicating that the wet heat environment contributes to the hydrolysis of tannins of phyllanthus emblica into GA monomer.
Example 3
From the results of example 2, the effect of the heat-treated ambient humidity on the release effect of the GA monomer in phyllanthus emblica was investigated, and the specific procedure was as follows:
Referring to fig. 1, selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with diameters of 2.5-4 cm in the Chinese cloud precious plateau area, rinsing with running water, washing away soil, leaves and the like on the surfaces of phyllanthus emblica wild fruits, and draining; and (5) screening again after cleaning, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning.
Pre-freezing fresh phyllanthus emblica slices for 1.5 hours at-80 ℃ in a freezer, wherein the weight of the fresh phyllanthus emblica slices is 10kg/m 2, and the thickness of the fresh phyllanthus emblica slices is 2cm; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting to heat to 40 ℃, and sublimating and drying for different times; keeping the temperature of the materials at 35 ℃, regulating and controlling the moisture content of the phyllanthus emblica tablets to be 9+/-1%, 14+/-1% and 38+/-1% (weight percentage) respectively, and discharging. The thickness of the tray is controlled to be 1.5cm, the drying temperature is controlled to be 110+/-2 ℃, the drying environment humidity is respectively controlled to be 9+/-2%, 14+/-2% and 38+/-2%, and the finished product is obtained after drying for 4 hours.
The procedure for extraction and measurement of GA in emblic leafflower fruit was as in example 1.
As shown in FIG. 5, the release rate of the GA monomer can be obviously improved when the water content and the environmental humidity of the phyllanthus emblica are 8% -40%, and compared with fresh phyllanthus emblica which is dried for 4 hours (71.33 mg/g) at 110+/-2 ℃, the GA content is increased by about 5.5% -34.2%. In addition, the GA content was increased by about 11.6 to 15 times and 16.1 to 20.7 times as compared with those according to the conventional processing (5.99 mg/g) and the lyophilized phyllanthus emblica (4.41 mg/g).
Meanwhile, as can be seen from examples 1, 2 and 3, the water content regulating and controlling steps and the drying steps adopted in the method have a synergistic effect, so that the content of gallic acid in the emblic leafflower fruits can be synergistically improved, particularly, the water content of the emblic leafflower fruits is regulated and controlled to be 8% -40%, the drying environment humidity is obviously synergistic between 8% -40% and the drying temperature, and the content of gallic acid in the emblic leafflower fruits can be synergistically improved.
Although embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that: various substitutions, changes and modifications are possible without departing from the spirit and scope of the invention and the appended claims, and therefore the scope of the invention is not limited to the disclosure of the embodiments.
Claims (3)
1. A method for synergistically improving the content of gallic acid in phyllanthus emblica through temperature and humidity co-excitation is characterized by comprising the following steps: the method comprises the following specific steps:
(1) Selecting fruits: selecting fresh, rot-free, pest-free and mildew-free nine-ripe phyllanthus emblica fruits with the diameter of 2.5-4 cm; (2) cleaning: washing the surfaces of fruits with flowing water to remove leaves and dust, and draining; (3) screening: cleaning, screening again, and removing the phyllanthus emblica fruits with mildew or rot points found after cleaning; (4) slicing: cutting phyllanthus emblica into crescent slices with the thickness of 2-6 mm; (5) The temperature and humidity co-excitation technology treatment comprises the following specific treatment steps: ① Regulating and controlling the moisture content: the emblic leafflower fruit slices are subjected to dishing, the dishing weight is 10-11 kg/m 2, the thickness is 1.5-2.5 cm, and pre-freezing is carried out for 1.5-2.5 hours at the temperature of minus 80 ℃; vacuumizing until the absolute pressure of the system is 60-70 Pa, starting heating to 40-70 ℃, and sublimating and drying for 13-20 h; keeping the temperature of the materials at 25-45 ℃, regulating and controlling the moisture content of the phyllanthus emblica slices to 8-40%, and discharging; ② drying: the emblic leafflower fruit slices with the moisture content of 8-40% are palletized, the palletizing weight is 12-15 kg/m 2, the thickness is 1-2 cm, the drying temperature is controlled at 80-130 ℃, the drying environment humidity is 8-40%, and the drying time is 2-8 h;
(6) And (5) vacuumizing, packaging and storing.
2. The method according to claim 1, characterized in that: the phyllanthus emblica is of a region of a cloud and precious altitude in China.
3. Use of the method of claim 1 or 2 in the preparation of gallic acid.
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