A wine-processed Cornus officinalis and its preparation method

Abstract

This invention belongs to the field of traditional Chinese medicine processing technology, and relates to a method for preparing Cornus officinalis (Shanzhuyu) for wine. The method includes: mixing Cornus officinalis with rice wine at a mass ratio of 100:5-50, ultrasonicating at 20-30 kHz for 10-20 minutes, soaking for 0.5-3 hours, microwaving at high power for short periods 3-4 times, steaming at 105-120℃ for 0.5-5 hours, and drying at 50-60℃ until the moisture content is below 16 wt%. The processing method for Cornus officinalis provided by this invention produces Cornus officinalis slices with uniform color, and the quality of the Cornus officinalis is improved through optimization of the process and parameters.

Description

Technical Field

[0001] This invention belongs to the field of traditional Chinese medicine processing technology, and relates to a wine-processed Cornus officinalis and its preparation method. Background Technology

[0002] Cornus officinalis is the dried, ripe pulp of the plant Cornus officinalis Sieb. et Zucc., belonging to the Cornaceae family. It has a sour and astringent taste, is slightly warm in nature, and enters the liver and kidney meridians. Its main chemical components include iridoids and their glycosides, triterpenoids, tannins, organic acids, flavonoids, volatile oils, and other effective ingredients. It has the effects of tonifying the liver and kidneys, astringing and consolidating, and is used for dizziness and tinnitus, soreness and weakness of the lower back and knees, impotence and seminal emission, enuresis and frequent urination, metrorrhagia and leukorrhea, profuse sweating and collapse, and internal heat and thirst. Modern methods for processing Cornus officinalis include cleaning, steaming, stewing with wine, and steaming with wine. The 1985 to 2020 editions of the Chinese Pharmacopoeia revised the processing method of Cornus officinalis to "wine-processed Cornus officinalis," with the processing specification stating that "take Cornus officinalis flesh, stew or steam it with wine until the wine is completely absorbed." It also stipulates that for every 100 kg of processed product, use 10-20 kg of rice wine.

[0003] Yellow wine is a fermented wine made from grains, using wheat koji or small koji as saccharification and fermentation agents. It is a pale yellow, clear liquid with a mellow taste and fragrant aroma. The ethanol volume fraction (or alcohol content) is generally 8-20 vol%. Ethanol, as an amphiphilic solvent, can promote solubilization or adsorption of medicinal herbs after a certain period of soaking. Different concentrations of ethanol can lead to variations in the leaching effect of polysaccharides, saponins, and flavonoids, thus affecting the clinical efficacy of the medicinal herbs after processing. Studies have found that different brewing processes among different manufacturers can affect the sugar content, alcohol content, pH value, total acidity, and β-phenylethanol content of yellow wine. Yellow wine is categorized based on the raw materials used, including glutinous rice wine, millet wine, and rice wine. Based on their sugar content, rice wines are categorized into dry rice wines (total sugar content equal to or less than 15.0 g / L), semi-dry rice wines (total sugar content between 15.1 g / L and 40.0 g / L), semi-sweet rice wines (total sugar content between 40.1 g / L and 100.0 g / L), and sweet rice wines (total sugar content greater than 100.0 g / L). However, current research on the processing techniques of rice wine mainly focuses on the amount of rice wine used, alcohol content, soaking time, and steaming time, with little investigation into the impact of rice wine type and processing technology on its quality. Summary of the Invention

[0004] The purpose of this invention is to provide a preparation method for improving the quality of wine-processed Cornus officinalis products, based on traditional literature and combined with modern processing methods and analytical techniques.

[0005] To achieve the above objectives, the present invention provides a method for preparing Cornus officinalis and its preparation to meet this need in the art.

[0006] On the one hand, the present invention relates to a preparation method of Fructus Corni, which includes: mixing Fructus Corni and yellow rice wine at a mass ratio of 100:5 to 50, ultrasonicating at 20 - 30 kHz for 10 - 20 min, moistening for 0.5 - 3 h, performing high-power short-time microwave treatment 3 - 4 times, steaming in water bath at 105 - 120 °C for 0.5 - 5 h, and drying at 50 - 60 °C until the water content is lower than 16 w%.

[0007] The high-power short-time microwave is 800 - 1000 W microwave for 30 - 60 s, with an interval of 3 - 6 min each time.

[0008] The ultrasonic thermal mechanism, ultrasonic mechanical mechanism, and cavitation effect are the three theoretical bases for the application of ultrasonic technology in traditional Chinese medicine extraction. To ensure the integrity of the medicinal materials, in the preparation of Fructus Corni, Fructus Corni will not be cut into pieces before processing. Therefore, in order to better dissolve the active ingredients, the present invention uses ultrasonic waves at 20 - 30 kHz for 10 - 20 min. By utilizing the cavitation effect, it accelerates the entry of the active ingredients in Fructus Corni into the yellow rice wine, and further extraction can increase the extraction rate of the active ingredients.

[0009] Microwave technology can be used for the extraction of active ingredients from traditional Chinese medicine and natural products. As the microwave power or time increases, the extraction amount of the active ingredients will increase accordingly, but as the power or time continues to increase, the extraction rate will decrease. High-power microwave or long-time microwave will cause the material to be scorched and charred, and the processed components will be severely denatured and a large amount of impurities will be generated. The present invention uses high-power short-time microwave combined with ultrasonic treatment to solve the problem that it is difficult to dissolve the active ingredients of large-volume Fructus Corni.

[0010] On the other hand, in the preparation method of Fructus Corni provided by the present invention, the yellow rice wine is glutinous rice yellow rice wine, and the glutinous rice yellow rice wine is dry-type yellow rice wine or semi-dry-type yellow rice wine.

[0011] Preferably, in the preparation method of Fructus Corni provided by the present invention, the mass ratio of Fructus Corni to yellow rice wine is 100:15 to 30.

[0012] Preferably, in the preparation method of Fructus Corni provided by the present invention, the moistening time is 1.5 h.

[0013] Preferably, in the preparation method of Fructus Corni provided by the present invention, it is steamed in water bath at 110 - 115 °C for 1 - 3 h.

[0014] Preferably, in the preparation method of Fructus Corni provided by the present invention, the high-power short-time microwave is 900 W microwave for 30 s, with an interval of 6 min each time.

[0015] On the other hand, the present invention relates to a Fructus Corni prepared by the above preparation method.

[0016] Compared with the prior art, the present invention has the following beneficial effects or advantages:

[0017] This invention, through optimization of processes and parameters, employs high-power short-time microwave combined with ultrasonic treatment to solve the problem of difficult dissolution of effective components from large-volume Cornus officinalis fruit. Previous research on the processing technology of Cornus officinalis wine has focused on the amount of rice wine used, alcohol content, soaking time, and steaming time. This invention further verifies through experiments that glutinous rice rice wine is superior to millet rice wine or rice wine in the preparation of Cornus officinalis wine; and verifies the impact of sugar content on the quality of Cornus officinalis wine products, showing that dry or semi-dry rice wine is superior to other rice wines with higher total sugar content. Attached Figure Description

[0018] Figure 1 The images show the HPLC chromatograms of the sample and mixed reference standard prepared in Example 1. A represents the sample prepared in Example 1, and B represents the mixed reference standard.

[0019] Explanation of reference numerals in the attached diagram:

[0020] 1 is gallic acid, 2 is monoglycine, 3 is loganin, and 4 is ellagic acid. Detailed Implementation

[0021] The technical solution of the present invention will be described below with reference to the embodiments. However, the present invention is not limited to the following embodiments.

[0022] To enable those skilled in the art to better understand and implement the technical solutions of the present invention, the present invention will be further described below in conjunction with specific embodiments and accompanying drawings. However, the embodiments described are not intended to limit the present invention.

[0023] Unless otherwise specified, the experimental and detection methods described in the following embodiments are conventional methods; unless otherwise specified, the reagents and materials are commercially available.

[0024] Experimental instruments: Shimadzu HPLC system (LC-20AD high-pressure pump, CTO-20AC column oven, DGU-20A automatic degasser, SIL-20AC autosampler, SPD-20AV diode array detector; experimental data were processed using a Shimadzu LCMS solution Ver.3 workstation).

[0025] Experimental materials: Cornus officinalis was purchased from Shaanxi Boren Pharmaceutical Co., Ltd., and identified by Professor Chen Shizhong of the School of Pharmacy, Peking University, as the dried, mature pulp of Cornus officinalis Sieb. et Zucc., a plant of the Cornaceae family. Gallic acid (batch number: MUST-20061902, purity ≥99.12%) was purchased from Chengdu Manster Biotechnology Co., Ltd., mononoside (batch number: wkq20020601, purity ≥98%), loganin (batch number: wkq20022405, purity ≥98%) was purchased from Sichuan Weikeqi Biotechnology Co., Ltd., and ellagic acid (batch number: x10476-66-4-1) was purchased from Beijing Kaiguo Technology Co., Ltd. All rice wines involved were purchased from Dalian Changxingdao Winery Co., Ltd., with an alcohol content of 14 vol%.

[0026] This invention provides a method for preparing Cornus officinalis, which includes the following steps:

[0027] S1: Cleaning: Take Cornus officinalis and remove impurities and residual fruit pits;

[0028] S2: Cleaning and drying: Place the cleaned Cornus officinalis in a washing device, rinse it with running water, and then place it in a drying device to dry at 60-70℃.

[0029] S3: Processing: Place the dried Cornus officinalis fruit in a container, add rice wine and mix well. The mass ratio of Cornus officinalis fruit to rice wine is 100:5-50. Sonicate at 20-30 kHz for 10-20 minutes, let it soak for 0.5-3 hours, microwave at high power for short time 3-4 times, and steam in a pressure cooker at 105-120℃ for 0.5-5 hours. Remove and let it cool naturally.

[0030] S4: Drying: Place in an oven at 50-60℃ and dry until the moisture content is below 16w. After cooling, the wine-processed Cornus officinalis is obtained.

[0031] Example 1

[0032] This embodiment provides a method for preparing Cornus officinalis, which includes the following steps:

[0033] S1: Cleaning: Take Cornus officinalis and remove impurities and residual fruit pits;

[0034] S2: Cleaning and drying: Place the cleaned Cornus officinalis in a washing device, rinse it with running water, and then place it in a drying device to dry at 60°C.

[0035] S3: Processing: Place the dried Cornus officinalis fruit in a container, add dry glutinous rice wine and mix well. Use 5 kg of rice wine for every 100 kg of Cornus officinalis fruit. Ultrasound at 20 kHz for 10 min, let it soak for 0.5 h, microwave at 800 W for 30 s 3 times, with a 3 min interval between each time. Place it in a pressure cooker and steam at 105℃ for 0.5 h. Remove and let it cool naturally.

[0036] S4: Drying: Place in an oven at 50°C and dry until the moisture content is below 16w. After cooling, the wine-processed Cornus officinalis is obtained.

[0037] Example 2

[0038] This embodiment provides a method for preparing Cornus officinalis, which includes the following steps:

[0039] S1: Cleaning: Take Cornus officinalis and remove impurities and residual fruit pits;

[0040] S2: Cleaning and drying: Place the cleaned Cornus officinalis in a washing device, rinse it with running water, and then place it in a drying device to dry at 70°C.

[0041] S3: Processing: Place the dried Cornus officinalis fruit in a container, add dry glutinous rice wine and mix well. Use 15 kg of rice wine for every 100 kg of Cornus officinalis fruit. Ultrasound at 25 kHz for 15 min, let it soak for 1.5 h, microwave at 900 W for 30 s 4 times, with an interval of 6 min each time. Place it in a pressure cooker and steam at 110℃ for 2.5 h. Remove and let it cool naturally.

[0042] S4: Drying: Place in an oven at 60℃ and dry until the moisture content is less than 16w. After cooling, the wine-flavored Cornus officinalis is obtained.

[0043] Example 3

[0044] This embodiment provides a method for preparing Cornus officinalis, which includes the following steps:

[0045] S1: Cleaning: Take Cornus officinalis and remove impurities and residual fruit pits;

[0046] S2: Cleaning and drying: Place the cleaned Cornus officinalis in a washing device, rinse it with running water, and then place it in a drying device to dry at 70°C.

[0047] S3: Processing: Place the dried Cornus officinalis fruit in a container, add semi-dry glutinous rice wine and mix well. Use 30 kg of rice wine for every 100 kg of Cornus officinalis fruit. Ultrasound at 30 kHz for 20 min, let it soak for 3 h, microwave at 1000 W for 60 s 3 times, with a 5 min interval between each time. Place it in a pressure cooker and steam at 120 ℃ for 5 h. Remove and let it cool naturally.

[0048] S4: Drying: Place in an oven at 60℃ and dry until the moisture content is less than 16w. After cooling, the wine-flavored Cornus officinalis is obtained.

[0049] Example 4

[0050] This embodiment provides a method for preparing Cornus officinalis, which includes the following steps:

[0051] S1: Cleaning: Take Cornus officinalis and remove impurities and residual fruit pits;

[0052] S2: Cleaning and drying: Place the cleaned Cornus officinalis in a washing device, rinse it with running water, and then place it in a drying device to dry at 70°C.

[0053] S3: Processing: Place the dried Cornus officinalis fruit in a container, add dry glutinous rice wine and mix well. Use 50 kg of rice wine for every 100 kg of Cornus officinalis fruit. Ultrasound at 30 kHz for 20 min, let it soak for 3 h, microwave at 1000 W for 60 s 4 times, with a 5 min interval between each time. Place it in a pressure cooker and steam at 120 ℃ for 5 h. Remove and let it cool naturally.

[0054] S4: Drying: Place in an oven at 60℃ and dry until the moisture content is less than 16w. After cooling, the wine-flavored Cornus officinalis is obtained.

[0055] Comparative Example 1

[0056] The preparation method of this comparative example is the same as that of Example 1, except that a semi-sweet glutinous rice wine was used.

[0057] Comparative Example 2

[0058] The preparation method of this comparative example is the same as that of Example 1, except that sweet glutinous rice wine was used.

[0059] Comparative Example 3

[0060] The preparation method of this comparative example is the same as that of Example 1, except that millet rice wine was used.

[0061] Comparative Example 4

[0062] The preparation method of this comparative example is the same as that of Example 1, except that rice wine was used.

[0063] Comparative Example 5

[0064] The preparation method of this comparative example is the same as that of Example 1, except that high-power short-time microwave treatment was not performed.

[0065] Example 5

[0066] This embodiment provides product quality determination for Examples 1-4 and Comparative Examples 1-5.

[0067] Take appropriate amounts of gallic acid, monoglycoside, loganin and ellagic acid reference standards, accurately weigh them, add methanol to prepare standard stock solutions containing 26 μg, 218 μg, 84.4 μg and 50 μg per 1 mL respectively, and then dilute them 1.5 times each and store them in a refrigerator at 4℃ for later use.

[0068] Take 0.2g of the powder from the above examples or comparative examples (passed through a No. 4 sieve), weigh accurately, place in a round-bottom flask, add 25mL of 80w% methanol accurately, weigh, heat under reflux for 1 hour, cool, weigh again, make up the lost weight with methanol, shake well, filter, and the product is obtained.

[0069] Chromatographic conditions were as follows: Kromasil 100-5-C18 (4.6 x 150 mm), mobile phase: 0.2 w% formic acid (A) - acetonitrile (B), elution gradient: 0-20 min, 7%-7% B; 20-50 min, 7%-20% B; 50-60 min, 20-95% B. Flow rate: 1 mL / min, injection volume: 10 μL; column temperature: 30°C, detection wavelength: 240 nm.

[0070] Standard curves for gallic acid, monoglobulin, loganin, and ellagic acid were plotted with the mass concentration (μg / mL) of each component as the x-axis (X) and the peak area of ​​each component as the y-axis (Y). The regression equations and their linear ranges were obtained, as shown in Table 1. The HPLC chromatograms of the samples and mixed reference standards prepared in Example 1 are shown below. Figure 1 As shown.

[0071] The results showed that gallic acid, monoglucoside, loganin, and ellagic acid exhibited good linearity within their respective concentration ranges.

[0072] Table 1: Results of linear relationship investigation for each reference standard

[0073] Element Regression equation r Linear range (μg / mL) gallic acid Y = 10252X + 2558 0.9998 3.43-26.0 Monoglycoside Y = 16500X + 31454 0.9995 28.71-281.0 Strychnoside Y = 19832X + 12999 0.9990 11.12-84.44 Ellagic acid Y = 18335X - 6990 0.9991 6.58-50.0

[0074] Accurately weigh the samples from Examples 1-4 and Comparative Examples 1-5, as well as raw Cornus officinalis, and prepare test solutions according to the above method. Then, inject and analyze the samples under the same chromatographic conditions, record the peak areas, and calculate the content of each component by external analysis. Each sample was measured in triplicate, and the results are shown in Table 2.

[0075] Table 2: Content determination results (mg / g) of the four components in the examples

[0076] gallic acid Monoglycoside Strychnoside Ellagic acid raw products 0.9929 13.8168 7.5600 0.9590 Example 1 1.3019 7.0464 4.5201 1.4710 Example 2 2.5987 12.2460 7.2430 2.6343 Example 3 2.6261 11.6310 6.8660 3.4723 Example 4 2.0995 10.9934 6.0603 1.9745 Comparative Example 1 1.0656 6.3662 3.6909 1.0694 Comparative Example 2 0.9868 6.2644 3.8614 1.1131 Comparative Example 3 0.9070 5.8193 3.8936 0.9790 Comparative Example 4 0.9961 6.1460 3.7951 1.1130 Comparative Example 5 0.9730 6.1041 3.6261 0.9802

[0077] By measuring the content of four components in Examples 1-4 and Comparative Examples 1-5, the content of gallic acid and ellagic acid obtained by the preparation method of Cornus officinalis provided by the present invention is increased, which enhances the astringent and kidney-tonifying effects. The content of the effective components obtained is significantly higher (p<0.05) than that in Comparative Examples 1-5.

[0078] As described above, the present invention can be well implemented. The above embodiments are merely descriptions of preferred embodiments of the present invention and are not intended to limit the scope of the present invention. Without departing from the spirit of the present invention, all kinds of changes and improvements made by those skilled in the art to the technical solutions of the present invention should fall within the protection scope defined by the present invention.

Claims

1. A method for preparing Cornus officinalis, characterized in that, Comprising: Mixing the cornus officinalis with yellow rice wine with a mass ratio of 100:5-50, ultrasonic treatment at 20-30 kHz for 10-20 min, dampening for 0.5-3 h, high-power short-time microwave for 3-4 times, 105-120 ℃ water-sealed steaming for 0.5-5 h, and drying at 50-60 ℃ until the water content is less than 16 w%; The high-power short-time microwave is 800-1000 W microwave for 30-60 s, with an interval of 3-6 min each time. The yellow rice wine is glutinous rice yellow rice wine, and the glutinous rice yellow rice wine is dry yellow rice wine or semi-dry yellow rice wine.

2. The method of claim 1, wherein the wine-soaked meat is prepared by the steps of: The mass ratio of the cornus officinalis to the yellow rice wine is 100:15-30.

3. The method of claim 1, wherein the wine-soaked meat is prepared by the steps of: The dampening time is 1.5 h.

4. The method of claim 1, wherein the wine-soaked meat is prepared by the steps of: Water-sealed steaming at 110-115 ℃ for 1-3 h.

5. The preparation method of the wine cornus officinalis according to claim 1, wherein the high-power short-time microwave is 900 W microwave for 30 s, with an interval of 6 min each time.

6. A wine-infused meat, characterized in that, The wine cornus officinalis is prepared by the preparation method according to any one of claims 1-5.

Images