Processing method of chebula juice for calamine and application thereof

Abstract

The present application relates to the mineral medicine processing and application field, specifically to a kind of prepared method and application of calumba juice prepared calamine.The prepared process of calumba juice prepared calamine described includes following two steps: step one, water extraction is carried out to calumba meat, and prepare calumba juice;Step two, the calumba juice prepared in step one is used to quench calamine.The method compared with traditional calamine processing method reduces the tedious water flying step, and calumba produces synergistic effect in processing process to calamine.The calumba juice prepared calamine product obtained using the method is better than calamine raw product, traditional processing method obtained calamine product, and has more optimal effect of promoting skin wound healing, and can be used for the treatment of skin trauma and the preparation of skin trauma treatment drugs.

Description

TECHNICAL FIELD

[0001] The present application relates to the field of mineral medicine processing and application, in particular to a kind of calomel processing method and application of juice preparation. BACKGROUND

[0002] Calomel is recorded in Chinese Pharmacopoeia 2020 edition, which is a carbonate mineral calcite group of zincite, mainly containing zinc carbonate (ZnCO3). Currently, most of the calomel on the market is hydrozincite, mainly containing basic zinc carbonate (Zn5(CO3)2(OH)6). Calomel tastes sweet and is flat in nature; it belongs to the liver and spleen meridians; it has the effects of detoxifying, clearing the eyes, removing nebula, and stopping itching and closing wounds. In clinical applications, it is often used externally after processing, or used as a raw material for external preparations, such as Ma Yinglong's musk hemorrhoid ointment and Xiongdan hemorrhoid ointment, which all use calomel as the main raw material for its effect of stopping itching and closing wounds.

[0003] After calcining calomel at high temperature, its contained components ZnCO3 or Zn5(CO3)2(OH)6 are converted into zinc oxide (ZnO), which has antibacterial, anti-inflammatory, antiseptic, and muscle-regenerating effects, and has been proven to be the main component of calomel for exerting its efficacy. The applicant has previously researched the calcined water flying and calcined quenching water flying processes of calomel. During the calcined water flying process, the calcined product needs to be crushed and then water flown with a large amount of water. Fine powder is generated during the crushing process, which can cause harm to the health of the operators and also cause loss of the product. Further, the method of calcined quenching water flying is adopted, which makes the calomel become crisp by calcined quenching, so that it can be water flown without crushing. The amount of water added during water flying is optimized to obtain the best calomel processing and production process, and one patent (CN 114259505B) has been granted.

[0004] In addition to the methods of calcined water flying and calcined quenching water flying, there is also a method of juice preparation during the processing of calomel. For example, the method of calomel prepared by Sanhuang decoction can enhance the effects of clearing heat, detoxifying, and drying dampness of calomel; the method of calomel prepared by Huanglian decoction can enhance the effects of clearing heat and drying dampness of calomel, both of which take advantage of the synergistic effect of auxiliary materials and drugs.

[0005] Based on the traditional theory of Chinese medicine and problem-oriented, the present patent application makes an in-depth exploration of calomel prepared by juice preparation of Terminalia chebula, and obtains a method of calcined quenching calomel prepared by juice preparation of Terminalia chebula, and the obtained product is used for the treatment of skin wounds and the preparation of drugs for the treatment of skin wounds. SUMMARY

[0006] The application aims to provide a processing method of calomelas prepared from Terminalia chebula juice and application thereof.

[0007] In order to achieve the above-mentioned application purposes, the application provides the following technical solutions.

[0008] The application provides a processing method of calomelas, characterized in that calomelas is prepared from Terminalia chebula juice.

[0009] Further, the method comprises the following steps:

[0010] S1, preparing Terminalia chebula juice for calcining and quenching: crushing Terminalia chebula flesh into powder, adding 8 times of water to soak, ultrasonic extraction, centrifugation, pouring out the upper extraction liquid, adding 6-8 times of water to the precipitate, ultrasonic extraction, centrifugation, pouring out the upper extraction liquid, combining the two times of Terminalia chebula extraction liquid, adding appropriate amount of water to prepare Terminalia chebula juice for calcining and quenching;

[0011] S2, calcining and quenching calomelas with Terminalia chebula juice: crushing calomelas into small pieces, putting them into a calcining furnace for calcining, immediately putting them into the Terminalia chebula juice prepared in S1 after taking them out, stirring while hot, pouring out the quenching liquid; the residue is calcined and quenched again by the above method, the quenching liquid and the residue obtained by two times are combined, concentrated to dryness and dried to constant weight, finely ground, and calomelas is prepared.

[0012] Further, the Terminalia chebula flesh is crushed into 150-200 mesh powder in S1, and the ultrasonic extraction time is 30-50 min; the centrifugation operation condition is 3000 r / min, and the centrifugation time is 10-20 min.

[0013] Further, the concentration of the Terminalia chebula juice for calcining and quenching prepared in S1 is 1-2 g / 100 mL.

[0014] Further, the amount of the Terminalia chebula juice in S2 is 3 times of the feeding amount of calomelas.

[0015] Further, the calcining condition in S2 is calcining at 700 DEG C for 20-40 min.

[0016] Further, the concentration and drying temperature in S2 are both 50 DEG C-60 DEG C.

[0017] Further, the application of the calomelas prepared from Terminalia chebula juice by the processing method in the preparation of drugs for treating skin wounds.

[0018] The application further provides a medicine for treating skin wounds, characterized in that the medicine contains the prepared calomelas prepared with Terminalia chebula juice and other pharmaceutically acceptable carriers.

[0019] Further, the preparation method of the calomelas prepared with Terminalia chebula juice comprises the following steps:

[0020] S1, crush Terminalia chebula meat into 150-200 mesh powder, take the Terminalia chebula meat powder, soak in 8 times amount of water for 1 hour, ultrasonic extraction for 30 minutes, centrifugal at 3000 r / min for 20 minutes, pour out the upper extraction liquid, add 6 times amount of water to the precipitate, ultrasonic extraction for 30 minutes, centrifugal at 3000 r / min for 20 minutes, pour out the upper extraction liquid, combine the two times of Terminalia chebula extraction liquid, add appropriate amount of water to prepare the Terminalia chebula juice with a concentration of 1 g / 100 mL, and reserve it for use;

[0021] S2, crush the calomelas into small pieces with a diameter of about 7-9 mm, put it into the calcining furnace, calcine at 700℃ for 30 minutes, immediately put it into the Terminalia chebula juice prepared in S1 with 3 times amount of the Terminalia chebula juice, stir while hot, pour out the quenching liquid; the residue is calcined and quenched again in the same way, combine the two times of quenching liquid and residue, concentrate to dryness at 60℃ and dry to constant weight, grind finely, and prepare the calomelas prepared with Terminalia chebula juice.

[0022] Compared with the prior art, the application has the following beneficial effects.

[0023] (1) The method for preparing calomelas in Chinese Pharmacopoeia is calcining and water flying, the previous improvement of the calcining and water flying method by the research group has established the calcining and quenching water flying processing technology of calomelas, but no matter calcining and water flying or calcining and quenching water flying, in order to make the product into fine powder, both need water flying operation, which is very tedious. The Terminalia chebula juice calcining and quenching calomelas, because the tannin components in Terminalia chebula have acidity, can promote the rapid decomposition of carbonates, so without water flying operation, the Terminalia chebula juice prepared calomelas product can be ground to very fine powder, so the tedious water flying operation step can be omitted.

[0024] (2) Terminalia chebula mainly contains tannin components, tannin has astringent nature, can make the protein in the exudate after wound coagulation, form a scab, and then reduce secretion and prevent infection; at the same time, tannin can make the microvessels of the wound shrink, has local hemostatic effect; in addition, tannin can coagulate protoplasm in microorganisms, so it has antibacterial effect. The Terminalia chebula juice calcining and quenching calomelas, the auxiliary material Terminalia chebula can produce synergistic effect on the antibacterial and astringent effect of calomelas, the prepared Terminalia chebula juice prepared calomelas has better treatment effect on skin wounds than the calomelas prepared by simple calcining and water flying and calcining and quenching water flying. BRIEF DESCRIPTION OF DRAWINGS

[0025] Figure 1The rat skin pathological section figure, wherein A: blank group; B: model group; C: prepared sumac juice calamine group; D: calcined water fly calamine group; E: sumac water extract group; F: calamine raw product group (20x under the microscope). DETAILED DESCRIPTION

[0026] The application will be further described in detail below with specific examples. However, it should not be understood that the scope of the above-mentioned subject matter of the application is limited to the following examples only, and any technology realized based on the content of the application falls within the scope of the application.

[0027] Example 1: Preparation of sumac juice for sumac juice calcined calamine.

[0028] Applicants previously studied the antibacterial effects of the main tannin components in sumac, such as chebulagic acid and chebulinic acid, and the results showed that both components had good inhibitory effects on gram-negative bacteria and gram-positive bacteria. Therefore, the HPLC method was used to establish the preparation process of sumac juice, with the total extraction rate of chebulagic acid and chebulinic acid as the index. The chromatographic conditions are as follows: chromatographic column: Platisil ODS column (250 mm x 4.6 mm, 5 μm), sample size: 5 μL, mobile phase: 0.1% formic acid water: acetonitrile: methanol (78:16:6), flow rate: 1 mL / min, column temperature: 30°C, detection wavelength: 280 nm.

[0029] Example 1: Preparation of sumac juice for sumac juice calcined calamine, the specific operation steps are as follows:

[0030] The sumac pulp was crushed into a 150-mesh powder, and the sumac powder was added with 8 times the amount of water and soaked for 1 h, ultrasonic extraction for 50 min, centrifugation (3000 r / min) for 10 min, and the upper extraction liquid was poured out. The precipitate was added with 8 times the amount of water, ultrasonic extraction for 30 min, centrifugation (3000 r / min) for 10 min, and the upper extraction liquid was poured out. The sumac extraction liquids of the two times were combined.

[0031] The total extraction rate of chebulagic acid and chebulinic acid was 81.7% as determined by HPLC.

[0032] Example 2: Preparation of sumac juice for sumac juice calcined calamine, the specific operation steps are as follows:

[0033] The sumac pulp was crushed into a 180-mesh powder, and the sumac powder was added with 8 times the amount of water and soaked for 1 h, ultrasonic extraction for 40 min, centrifugation (3000 r / min) for 15 min, and the upper extraction liquid was poured out. The precipitate was added with 6 times the amount of water, ultrasonic extraction for 30 min, centrifugation (3000 r / min) for 15 min, and the upper extraction liquid was poured out. The sumac extraction liquids of the two times were combined.

[0034] The total extraction rate of chebulic acid and chebulinic acid was 83.1% determined by HPLC method.

[0035] Example 3: Preparation of the juice of Terminalia chebula used for calcining and quenching of Calamine, the specific operation steps are as follows:

[0036] Take the Terminalia chebula meat powder and crush it into a 200-mesh powder. Take an appropriate amount of the Terminalia chebula meat powder and add 8 times the amount of water to soak for 1 h. Ultrasonic extraction for 30 min, centrifugation (3000 r / min) for 20 min, pour out the upper extraction liquid, add 6 times the amount of water to the precipitate, ultrasonic extraction for 30 min, centrifugation (3000 r / min) for 20 min, pour out the upper extraction liquid, and combine the two times of Terminalia chebula extraction liquid.

[0037] The total extraction rate of chebulic acid and chebulinic acid was 83.8% determined by HPLC method.

[0038] Example 2: Calcining and quenching process of Terminalia chebula juice calcining and quenching of Calamine, the specific operation steps are as follows.

[0039] The minimum double dilution method was used to observe the inhibition of the product on the representative gram-positive bacteria Staphylococcus aureus and the representative gram-negative bacteria Acinetobacter baumannii under different calcining and quenching process parameters.

[0040] The experimental method for evaluating the antibacterial effect is as follows: sterile test tubes are taken, 1 mL of beef peptone liquid medium is added to each test tube, 1 mL of sample stock solution is added to the first test tube, and mixed evenly, then the drug is subjected to 2-fold dilution by the minimum double dilution method, that is, 1 mL is taken from the first test tube and added to the second test tube, and mixed evenly by blowing, and the operation is repeated in this way until 1 mL is taken from the fourth test tube after mixing and blowing evenly and discarded. 1 mL of diluted bacterial suspension is added to each test tube, and 1 mL of beef peptone liquid medium is used instead of the sample solution as the negative control group. After incubation in a 37℃ constant temperature incubator for 16-20 h, the results are observed visually to determine the number of tubes with minimum inhibitory concentration (MIC). The beef peptone liquid medium is used as a reference solution, and the absorbance of the solution in the next tube with MIC is determined by ultraviolet absorbance spectrophotometry at 700 nm. The absorbance of the solution in the next tube with MIC of Acinetobacter baumannii and Staphylococcus aureus is used as an index for comprehensive scoring.

[0041] .

[0042] Preparation process of Terminalia chebula juice: Take Terminalia chebula pulp and grind it into 150-200 mesh powder. Take an appropriate amount of the Terminalia chebula pulp powder, add 8 times the amount of water and soak for 1 hour. Extract by ultrasonication for 30-50 minutes, centrifuge, and pour off the upper extract. Add 6-8 times the weight of the original Terminalia chebula pulp powder to the precipitate, extract by ultrasonication for 30-50 minutes, centrifuge, and pour off the upper extract. Combine the two Terminalia chebula extracts, add an appropriate amount of water, and prepare the Terminalia chebula juice for calcination. The centrifugation conditions are 3000 r / min and centrifugation time is 10-20 minutes. The obtained Terminalia chebula juice for calcination...

[0043] Example 1: The calcination and quenching process of Terminalia chebula juice with calcined calamine is described in the following steps:

[0044] Calamine is crushed into small pieces with a diameter of about 7-9 mm. A certain amount is put into a calcining furnace and calcined at 700℃ for 20 minutes. After taking it out, it is immediately put into 3 times the amount of Terminalia chebula juice with a concentration of 1 g / 100 mL. Stir while hot and pour out the quenching liquid. The residue is calcined and quenched again in the same way. The quenching liquids obtained from the two calcinations are combined with the residue, concentrated to dryness at 50℃ and dried to constant weight at 50℃, and then ground into a fine powder.

[0045] The product's antibacterial effect received a comprehensive score of 0.954.

[0046] Example 2: The calcination and quenching process of Terminalia chebula juice with calcined calamine is described in the following steps:

[0047] Calamine is crushed into small pieces with a diameter of about 7-9 mm. A certain amount is put into a calcining furnace and calcined at 700℃ for 30 minutes. After taking it out, it is immediately put into 3 times the amount of Terminalia chebula juice with a concentration of 1 g / 100 mL. Stir while hot and pour out the quenching liquid. The residue is calcined and quenched again in the same way. The quenching liquids obtained from the two calcinations are combined with the residue, concentrated to dryness at 50℃ and dried to constant weight at 50℃, and then ground into a fine powder.

[0048] The product's antibacterial effect received a comprehensive score of 0.986.

[0049] Example 3: The calcination and quenching process of Terminalia chebula juice with calcined calamine is described in the following steps:

[0050] Calamine is crushed into small pieces with a diameter of about 7-9 mm. A certain amount is put into a calcining furnace and calcined at 700℃ for 40 min. After taking it out, it is immediately put into 3 times the amount of Terminalia chebula juice with a concentration of 1 g / 100 mL. Stir while hot and pour out the quenching liquid. The residue is calcined and quenched again in the same way. The quenching liquids obtained from the two calcinations are combined with the residue, concentrated to dryness at 50℃ and dried to constant weight at 50℃, and then ground into a fine powder.

[0051] The product's antibacterial effect received a comprehensive score of 0.978.

[0052] Example 4: The calcination and quenching process of calcined calamine with Terminalia chebula juice, the specific operation steps are as follows:

[0053] The malachite is broken into small pieces with a diameter of about 7-9 mm, a certain amount is put into the calcining furnace, calcined at 700℃ for 30 min, immediately after taking out, put into 3 times the amount of concentrated gleditsia sinensis fruit juice with a concentration of 2 g / 100 mL, stir while hot, pour out the quenching liquid; the residue is calcined and quenched again in the same way, the quenching liquids obtained twice are combined, concentrated to dryness at 60℃ and dried to constant weight at 60℃, and finely ground.

[0054] The comprehensive score of the product's antibacterial effect is 0.972.

[0055] Example 5: A calcining and quenching process of gleditsia sinensis fruit juice calcining and quenching malachite, the specific operation steps are as follows:

[0056] The malachite is broken into small pieces with a diameter of about 7-9 mm, a certain amount is put into the calcining furnace, calcined at 700℃ for 40 min, immediately after taking out, put into 3 times the amount of concentrated gleditsia sinensis fruit juice with a concentration of 2 g / 100 mL, stir while hot, pour out the quenching liquid; the residue is calcined and quenched again in the same way, the quenching liquids obtained twice are combined, concentrated to dryness at 60℃ and dried to constant weight at 60℃, and finely ground.

[0057] The comprehensive score of the product's antibacterial effect is 0.969.

[0058] Example 6: A calcining and quenching process of gleditsia sinensis fruit juice calcining and quenching malachite, the specific operation steps are as follows:

[0059] The malachite is broken into small pieces with a diameter of about 7-9 mm, a certain amount is put into the calcining furnace, calcined at 700℃ for 30 min, immediately after taking out, put into 3 times the amount of concentrated gleditsia sinensis fruit juice with a concentration of 1 g / 100 mL, stir while hot, pour out the quenching liquid; the residue is calcined and quenched again in the same way, the quenching liquids obtained twice are combined, concentrated to dryness at 60℃ and dried to constant weight at 60℃, and finely ground.

[0060] The comprehensive score of the product's antibacterial effect is 0.989.

[0061] Example 3: Application of gleditsia sinensis fruit juice prepared malachite in the treatment of skin wounds.

[0062] Take rats as experimental animals, prepare skin wound models, take the product obtained in example 6 of example 2 as the research object, and observe the treatment effect on rat skin wounds. At the same time, compare its treatment effect on wounds with that of raw malachite, water quenched malachite and simple gleditsia sinensis fruit water extract, and verify that gleditsia sinensis fruit has a synergistic effect on the moisture absorption and sore closing effect of malachite in the process of gleditsia sinensis fruit juice prepared malachite. The determination indexes are the healing rate of rat skin wounds and pathological section performance.

[0063] The specific experimental steps are as follows:

[0064] SD rats were taken 36, with 20% urethane anesthesia, the lower back depilation, randomly selected 6 as a blank group, the remaining 30 in the center of the depilation layer of 1.5 cm diameter circular skin resection treatment, to establish the rat skin back wound model. Postoperative disinfection, wound natural hemostasis. 30 rats were randomly divided into 5 groups, respectively, model group, sumac juice calamine group, calcined water fly calamine group, sumac water extract group, calamine raw product group, 6 in each group. 2 h after modeling, except the blank group and the model group, each group was given the corresponding cream, 0.3 g per, 1 d / time, continuous administration for 15 d. On the 1st, 3rd, 5th, 7th, 9th, 11th, 13th, 15th day, the wound area of each group of rats was photographed. The wound area (S) of each rat was measured by ImageJ software, and the wound healing rate was calculated [healing rate (%) = (S initial wound-S measured day wound) / S initial wound × 100%]. On the 16th day of administration, the animals in each group were anesthetized with 20% urethane, and the wound skin was cut off, fixed in 4% neutral formaldehyde solution for 24 h, gradient dehydrated with ethanol, routinely embedded in paraffin, and cut into sections with a thickness of about 5 μm using a pathological sectioning machine, and then stuck to glass slides and stained by routine HE staining method. The results of promoting wound healing rate are shown in Table 1, and the pathological section of the skin of the wound site of the rat is shown in Figure 1 .

[0065] Table 1 Wound healing rate (%) of rats in each group (n=6, )

[0066] .

[0067] Note: (Δ indicates that there is a very significant difference compared with the model group, P <0.01).

[0068] The results of pathological section examination showed that the number of inflammatory cell infiltration in the skin of rats in the sumac juice calamine group, the calcined water fly calamine group and the sumac water extract group was reduced, and the repair of squamous epithelium was more complete, indicating that the above three groups of drugs all had good effect on promoting wound healing. The results of wound healing rate determination showed that the wound healing rate of the skin in the sumac juice calamine group, the calcined water fly calamine group and the sumac water extract group was very significantly different from that of the model group, indicating that the treatment effect of the sumac juice calamine group, the calcined water fly calamine group and the sumac water extract group was better than that of the model group and the calamine raw product group; and from the 7th day, the wound healing rate of the sumac juice calamine group was significantly improved, and the total healing rate at 15 days was higher than that of the calcined water fly calamine group, indicating that the sumac juice calamine indeed had a synergistic effect on the calamine in promoting wound healing.

[0069] The above merely illustrates the preferred embodiments of the present application, and is not used to limit the patent scope of the present application. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method for processing of Gypsum, characterized in that, The method comprises the following steps: S1, preparing the juice of Terminalia chebula Retz: crushing the Terminalia chebula Retz into powder, adding 8 times of water to soak, ultrasonic extraction, centrifugation, pouring out the upper extraction liquid, adding 6-8 times of water to the precipitate, ultrasonic extraction, centrifugation, pouring out the upper extraction liquid, combining the two times of Terminalia chebula Retz extraction liquid, adding appropriate amount of water to prepare the juice of Terminalia chebula Retz for calcination; S2, calcining the calamine with the juice of Terminalia chebula Retz: crushing the calamine into small pieces, putting it into the calcination furnace for calcination, immediately putting it into the juice of Terminalia chebula Retz prepared in S1 after taking it out, stirring while hot, pouring out the quenching liquid; the residue is calcined and quenched again in the above-mentioned manner, and the quenching liquid and the residue obtained in two times are combined, concentrated to dryness and dried to constant weight, and finely ground to prepare the calamine prepared with the juice of Terminalia chebula Retz.

2. The method of claim 1, wherein the processing is selected from the group consisting of: In S1, the Terminalia chebula Retz is crushed into powder with a particle size of 150-200 mesh, and the ultrasonic extraction time is 30-50 min; the centrifugation operation condition is 3000 r / min, and the centrifugation time is 10-20 min.

3. The processing method according to claim 1, characterized in that, The concentration of the juice of Terminalia chebula Retz prepared in S1 is 1-2 g / 100 mL.

4. The processing method according to claim 1, characterized in that, In S2, the amount of the juice of Terminalia chebula Retz is 3 times of the amount of the calamine.

5. The processing method according to claim 1, characterized in that, In S2, the calcination condition is calcination at 700℃ for 20-40 min.

6. The processing method according to claim 1, characterized in that, In S2, the concentration and drying temperature are both 50-60℃.

7. The use of the calamine prepared with the juice of Terminalia chebula Retz by the preparation method of claim 1 in the preparation of a drug for treating skin wounds.

8. A medicament for the treatment of skin wounds, characterized in that, The drug contains the calamine prepared with the juice of Terminalia chebula Retz prepared by the preparation method of any one of claims 1-6, and other pharmaceutically acceptable carriers.

9. The medicament according to claim 8, characterized in that, The preparation method of the calamine prepared with the juice of Terminalia chebula Retz comprises the following steps: S1, crushing the Terminalia chebula Retz into powder with a particle size of 150-200 mesh, adding an appropriate amount of Terminalia chebula Retz powder to 8 times of water to soak for 1 h, ultrasonic extraction for 30 min, centrifugation at 3000 r / min for 20 min, pouring out the upper extraction liquid, adding 6 times of water to the precipitate, ultrasonic extraction for 30 min, centrifugation at 3000 r / min for 20 min, pouring out the upper extraction liquid, combining the two times of Terminalia chebula Retz extraction liquid, adding water to prepare the juice of Terminalia chebula Retz with a concentration of 1 g / 100 mL, and reserving it; S2, crushing the calamine into small pieces with a diameter of 7-9 mm, putting it into the calcination furnace, calcining at 700℃ for 30 min, immediately putting it into the juice of Terminalia chebula Retz prepared in S1 after taking it out, stirring while hot, pouring out the quenching liquid; the residue is calcined and quenched again in the same way, and the quenching liquid and the residue obtained in two times are combined, concentrated to dryness and dried to constant weight at 60℃, and finely ground to prepare the calamine prepared with the juice of Terminalia chebula Retz.

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