CN114848693A - Wine-washed angelica sinensis decoction pieces and processing method, quality detection method and application thereof - Google Patents
Wine-washed angelica sinensis decoction pieces and processing method, quality detection method and application thereof Download PDFInfo
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Abstract
The invention provides a wine-washed angelica sinensis decoction piece, a processing method, a quality detection method and application thereof. Mixing the raw angelica sinensis decoction pieces with the thickness of 1.5-2.5 mm with the semi-sweet yellow wine, sealing, airing to obtain the wine-washed angelica sinensis decoction pieces. The method is simple and efficient, is suitable for large-scale production of the alcohol washing angelica, and the contents of effective components such as alcohol washing angelica decoction pieces processed by the method, ferulic acid and the like are improved. The processed wine-washed angelica decoction pieces prepared by the method can be used for decocting angelica blood-enriching soup, and the corresponding quality standard is established for the processed wine-washed angelica decoction pieces so as to facilitate the subsequent application of the processed wine-washed angelica decoction pieces.
Description
Technical Field
The invention relates to a Chinese medicinal bulk drug wine washing angelica decoction piece, a preparation method and a quality detection method thereof, and application thereof in preparing a Chinese medicinal decoction for tonifying qi and generating blood.
Background
Angelica sinensis (Oliv.) Diels, an Umbelliferae plant Angelica sinensis (Oliv.) Diels, is dried root of Angelica sinensis (Oliv.) Diels, is sweet, pungent, warm in nature, and enters liver, heart and spleen channels, and is used for treating blood deficiency, sallow complexion, amenorrhea, dysmenorrhea, menoxenia, metrorrhagia, metrostaxis, etc. Dang Gui is a common bulk herb in China, and the earliest one in Erya is the one named as shan Qi. Because of its mild nature, Dang Gui belongs to the partial nature of cool with cool herbs and hot with hot herbs, so it is used in large quantities in the prescription of TCM and is said to be "ten prescriptions and nine subsitutes". The angelica blood-enriching soup is the most famous of a plurality of prescriptions containing angelica.
The processing of the traditional Chinese medicine is an indispensable step before the traditional Chinese medicine is used for clinical treatment, most of the traditional Chinese medicine exists in the original forms of underground rhizomes of plants, parts of animals, ores and the like before the traditional Chinese medicine is used for clinical treatment, and impurities such as dust and the like exist on the surface of the traditional Chinese medicine, so that the traditional Chinese medicine is not beneficial to preparation, inconvenient to take and decoction, and some traditional Chinese medicine has toxicity or serious adverse reactions after being taken. The processing of the traditional Chinese medicine can effectively avoid the situations, and has the effect of improving the curative effect on the basis of solving the problems. Generally, it is considered that Dang Gui itself has no toxicity, raw Dang Gui is sweet and warm and has its tonifying property, while wine Dang Gui is pungent and warm and has its dispersing property to enhance its blood-activating and blood-enriching effects. The processing of Dang Gui can increase or change its property, and expand its application range.
Different methods are available for processing Dang Gui in all ages, and the processing of Dang Gui is first mentioned in the "Liu Juanzi Gui Yi Fang" of Nanqi according to the literature examination. After the development and experience summarization of physicians of different generations, the processing method of Dang Gui is more and more than 20. But only wine processing, stir-frying and the like are widely used nowadays. The method for processing angelica sinensis by using wine as an auxiliary material is firstly seen in a Chinese medical literature Lei Gong Pao Zhi Lun of Liu Song times, and the document records that dust is removed firstly, the hard part of the head tip comes first and the wine is soaked for a night. However, it cannot be determined whether the wine is soaked in the wine or not, which is also understood as wine washing. In the period of Tang dynasty and Song dynasty, except for the wine soaking and stir-frying method in the spirit of physicians before use, the processing technology and auxiliary materials have been developed. The radix Angelicae sinensis wine can be prepared by washing with wine, processing with wine, and baking with wine. In the jin Yuan period, the processing method used before Song is basically followed except the wine-steaming method developed in the wine-making process. The book entitled "the ideas of soaking in wine and assisting law" is presented in the book "herbal decoction" of original dynasty, royal good ancient times, and points out: "if the disease is on the head, face and skin of hand, it should be stir-baked with wine and the spirit should be used to promote the disease. The findings reflect that different processing methods should be used for different purposes of the angelica, and actively promote the development of the preparation method of the angelica wine. The Ming physicians have paid attention to the systematic arrangement and research of theories, and some of the ideas still have important guiding significance so far. Wherein, the book Ben Cao Meng quan proposes that Lu Miao Xiao Jing and alcohol wine are used for refining. When washing the exterior, the Chinese angelica wine is considered to be prepared into the essence. However, it is uncertain whether the angelica soaking is the same as the angelica wine washing, and the angelica wine processing technology is developed by wine boiling and wine drying after the Qing Dynasty. The experience and knowledge of the processing of Dang Gui in these past generations provides a lot of reference for alcohol washing of Dang Gui. In recent times, the stir-frying method is not used in other ways except for the stir-frying method. But doctors in this period make a systematic comprehensive summary of the angelica cannon. The theory of ascending wine stir-frying and guiding blood to return to the source is said.
At present, the processed angelica variety recorded in 'Chinese pharmacopoeia' 2020 edition is wine-fried angelica, and for wine-washed angelica, the standards made by drug supervision and management departments in different provinces, autonomous regions and direct jurisdictions are different, and the obtained wine-washed angelica has no definite quality standard. Therefore, it is necessary to standardize the processing method and establish the corresponding quality standard for different uses of angelica.
Disclosure of Invention
The invention aims to provide a wine-washed angelica sinensis decoction piece, a processing method, a quality detection method and application thereof. The method is simple and efficient, is suitable for large-scale production of the alcohol washing angelica, and the contents of effective components such as alcohol washing angelica decoction pieces processed by the method, ferulic acid and the like are improved. The processed wine-washed angelica decoction pieces prepared by the method can be used for decocting angelica blood-enriching soup, and the corresponding quality standard is established for the processed wine-washed angelica decoction pieces so as to facilitate the subsequent application of the processed wine-washed angelica decoction pieces.
The invention is realized by the following technical scheme:
1. the processing method of the angelica sinensis decoction pieces washed with the wine specifically comprises the following steps:
taking raw angelica sinensis decoction pieces without removing root barks, enabling the thickness of the raw angelica sinensis decoction pieces to be between 1.5mm and 2.5mm, uniformly mixing angelica sinensis and a proper amount of yellow wine, sealing and stewing thoroughly, fully absorbing moisture to enable the yellow wine to be fully absorbed, drying in the air to obtain wine-washed angelica sinensis decoction pieces, wherein the wine-washed angelica sinensis decoction pieces after drying in the air have strong bouquet, the surface of the wine-washed angelica sinensis decoction pieces is brownish yellow, and the water content of the wine-washed angelica sinensis decoction pieces is not higher than 15%.
Preferably, the preparation method of the angelica decoction pieces washed with the wine comprises the following steps of taking raw angelica decoction pieces without removing root barks, wherein the thickness of the raw angelica decoction pieces is 1.5-2.5 mm, and mixing the raw angelica decoction pieces: the yellow wine is 10 g: uniformly spraying a proper amount of semi-sweet yellow wine in a proportion of 1g into angelica, sealing and thoroughly soaking, fully sucking and moistening for 4-6 h to enable the yellow wine to be fully absorbed, air-drying to obtain wine-washed angelica decoction pieces, wherein the air-dried wine-washed angelica decoction pieces have strong wine aroma, the surfaces of the wine-washed angelica decoction pieces are brownish yellow, and the water content is not higher than 15%.
The wine-washed angelica decoction pieces for the angelica blood-enriching decoction obtained by the processing technology have the advantages that the dissolution speed of active ingredients such as ferulic acid, volatile oil and the like is accelerated, the safety and the effectiveness of the processed angelica in clinical application are ensured, the processing process is simple and feasible, and the quality control and the large-scale production are easy.
In the processing technology, the thickness of the angelica decoction pieces used is between 1.5mm and 2.5mm, the slice thickness can influence the volatilization of water during drying and the dissolution of effective components during extraction, the effective components can be adsorbed again when the decoction pieces are too thin, and the decoction pieces are too soft and difficult to form due to the adsorption of too much solvent.
In the processing technology, the proportion of the angelica and the yellow wine is 10 g: 1g, adding a proper amount of yellow wine can fully promote the dissolution of the effective components, but if the amount of the yellow wine is excessive, the effective components are dissolved and lost. The research result of the invention shows that when the proportion of the angelica and the yellow wine is 10 g: when 1g is used, the content of the effective components is the highest.
The auxiliary materials used for processing in the processing technology are semi-sweet yellow wine which has higher alcohol concentration and is beneficial to dissolving out the effective components in the angelica decoction pieces, and the yellow wine has moderate sugar content and cannot generate overhigh influence on the medicine property of the angelica.
In the processing technology, the angelica and the yellow wine are required to be fully mixed, sealed and moistened for 4-6 hours, so that the decoction pieces have bouquet.
In the processing technology, the angelica sinensis decoction pieces washed with the wine are dried in the air, and experimental results show that the effective component content of other methods such as drying and stir-drying is higher in the air-drying process, the production process is easy to control, and the effective components can be retained to the maximum extent.
The wine-washed angelica decoction pieces prepared by the processing technology have the ferulic acid content of 0.092-0.109%, have obvious blood enriching effect, can be used as tonifying agent angelica blood enriching soup and other tonifying agent Chinese medicinal decoction pieces, and can also be used as raw materials of natural medicines, Chinese patent medicines and health care products.
2. A Chinese medicinal decoction for tonifying blood is prepared from radix Angelicae sinensis decoction pieces and radix astragali decoction pieces washed with wine as raw materials, and is prepared from radix Angelicae sinensis: 1g of astragalus: 5g of Chinese angelica blood-enriching soup is produced by the specific method:
soaking 6g of the Chinese angelica decoction pieces washed with the wine and 30g of the astragalus decoction pieces in 400mL of water for 30min, decocting the medicinal materials for 30min by strong fire after the water absorption of the medicinal materials is saturated, and collecting the obtained decoction. Adding 200mL of water into the residue, decocting with slow fire for 30min, and mixing the two decoctions to obtain the final product.
The application of the angelica sinensis blood-enriching decoction comprises other angelica sinensis blood-enriching decoction products, such as angelica sinensis blood-enriching decoction, granules, capsules, formula granules and the like.
3. Qualitative identification of ferulic acid and ligustilide in the radix Angelicae sinensis decoction pieces after washing with wine by thin layer chromatography, content determination of ferulic acid in the radix Angelicae sinensis decoction pieces after washing with wine by high performance liquid chromatography, investigation of radix Angelicae sinensis processing technology, and specification of radix Angelicae sinensis processing production program.
(1) Thin layer chromatography identification method
The obtained angelica decoction pieces washed with wine are taken and are identified according to a thin-layer identification method under the term of the angelica medicinal material in 2020 edition Chinese pharmacopoeia, the prepared angelica decoction pieces washed with wine are identified by taking an angelica reference medicinal material, ferulic acid and ligustilide as reference substances, and the same fluorescent spots are shown on the corresponding positions in the thin-layer chromatogram of the prepared angelica decoction pieces washed with wine compared with the reference medicinal material and the reference substance.
(2) High performance liquid chromatography
S1, preparation of control solutions: adding appropriate amount of ferulic acid into a volumetric flask, adding methanol to dissolve to constant volume to obtain ferulic acid reference solution, and storing at 4 deg.C.
S2, preparation of a test solution: taking a proper amount of the Chinese angelica decoction pieces washed with the wine, crushing, precisely adding methanol, heating, refluxing and extracting, weighing after the sample is cooled, complementing the weight loss by using a solvent, shaking up, filtering, and filtering a subsequent filtrate through a 0.45 mu m microporous filter membrane to obtain the Chinese angelica decoction pieces.
S3, injecting the ferulic acid reference substance solution and the test solution into a high performance liquid chromatograph for determination.
The chromatographic conditions of the high performance liquid chromatography are as follows:
the chromatographic column takes octadecylsilane chemically bonded silica as a filler and acetonitrile (A): 0.1% aqueous phosphoric acid (B) ═ 13:87 is a mobile phase with the flow rate of 0.5-1.0 mL/min; column temperature: 30-35 ℃; detection wavelength: 280-320 nm; sample introduction amount: 10 μ L.
Preferably, in the method for measuring the content of the angelica sinensis decoction pieces washed with wine, the ferulic acid reference solution in the step S1 is prepared by the following steps: precisely weighing ferulic acid, placing in a volumetric flask, fixing the volume to the scale with methanol, shaking up, and making into ferulic acid reference solution of 200 μ g/mL.
Preferably, in the method for measuring the content of the angelica sinensis decoction pieces washed with wine, the method for preparing the test solution in the step S2 comprises the following steps: placing 0.2g of the prepared wine-washed radix Angelicae sinensis powder in a conical flask with a stopper, adding 20mL of methanol precisely, reflux-extracting for 30min, cooling the sample, adding methanol to make up the lost weight, and filtering with 0.45 μm microporous membrane.
Compared with the prior art, the invention has the following beneficial effects:
the invention prepares the angelica sinensis bulk drug decoction piece wine-washed angelica sinensis for decocting the angelica sinensis blood-enriching decoction by adopting the most suitable type of yellow wine and drying mode. The effective components such as ferulic acid can be fully dissolved out, and compared with radix Angelicae sinensis decoction pieces, the obtained radix Angelicae sinensis decoction pieces have greatly increased effective component content.
The prepared angelica sinensis decoction pieces washed with wine have good activity of generating and replenishing blood, and can fully exert the effects of the angelica sinensis blood-replenishing decoction on tonifying qi and replenishing blood.
The invention adopts thin-layer chromatography and high performance liquid chromatography to carry out quality detection on the processed angelica decoction pieces, and the obtained thin-layer chromatogram has clear spots. A content determination method of the alcohol-washed Chinese angelica is established by using a high performance liquid chromatography, acetonitrile-0.1% phosphoric acid aqueous solution is used as a mobile phase for elution, a chromatogram base line is stable, a chromatogram peak pattern is good, methodology investigation results such as linear relation investigation, precision, stability, repeatability, sample adding recovery, system applicability and the like are good, the quality of the obtained alcohol-washed Chinese angelica can be objectively and accurately detected and evaluated, and the processing process of the Chinese angelica is standardized.
The angelica processed by the method can be used for decocting angelica blood-enriching soup which is the 51 st party in ancient classical directory (the first group) established by the national Chinese medicine administration and the national drug administration, and has good effects of tonifying qi and generating blood.
Drawings
FIG. 1 shows the processing of wine-washed Chinese angelica and the processed wine-washed Chinese angelica;
FIG. 210 is a graph showing the measurement of the contents of crude Dang Gui decoction pieces;
FIG. 3 is a diagram illustrating the optimization of the type of wine used for processing radix Angelicae sinensis washed with wine;
FIG. 4 is a graph showing the optimization of the amount of alcohol used for processing radix Angelicae sinensis washed with alcohol;
FIG. 5 optimization of drying mode of wine-washed Chinese angelica;
FIG. 6 is a diagram illustrating the optimization of the types of yellow rice wine for processing angelica after wine washing;
FIG. 715 is a thin-layer identification of wine-washed Chinese angelica decoction pieces and reference medicinal materials, wherein 1-15 of the decoction pieces are wine-washed Chinese angelica decoction pieces, and 16 of the reference medicinal materials are Chinese angelica;
FIG. 815 is a thin-layer identification chart of radix Angelicae sinensis decoction pieces and reference substances, wherein 1 is ligustilide reference substance, 2 is ferulic acid reference substance, and 3-15 are radix Angelicae sinensis decoction pieces washed with wine;
FIG. 9 optimization of the content determination and extraction method of wine-washed Chinese angelica;
FIG. 10 optimization of extraction solvent for determination of content of wine-washed Angelica sinensis;
FIG. 11 shows HPLC chromatogram A of ferulic acid control solution and HPLC chromatogram B of radix Angelicae sinensis decoction piece content measurement;
FIG. 12 is a standard graph of ferulic acid in alcohol-washed radix Angelicae sinensis decoction pieces;
FIG. 13 systematic adaptation HPLC profile of ferulic acidWherein A is the results of an Extend-C18 column experiment, B is the results of a Hypersil-C18 column experiment, and C is Newmate TM C18 chromatographic column experimental results.
Detailed Description
For a further understanding of the invention, reference will now be made to the following examples, which are provided to illustrate further features and advantages of the invention, and are not intended to limit the scope of the invention as set forth in the following claims.
The instruments and reagents used in the examples were as follows:
experimental equipment
1. Instrument for measuring the position of a moving object
An LC-20(UV) high-efficiency liquid chromatograph of Shimadzu instrument (Suzhou, China) corporation comprises an LC-20 liquid feeding unit, an SIL-20 automatic sample injector, an SPD-20 ultraviolet visible detector, a CTO-20 liquid storage box integrated column temperature box, a YM-100S type numerical control ultrasonic cleaner (Shenzhen Fang ao microelectronics Co., Ltd.), a JA2603B electronic analytical balance (Shanghai Tianmei balance instruments Co., Ltd.), an LE204E/02 electronic balance (Mettler Torre instruments Co., Ltd.), a JCS-600 electronic balance (Kaifeng group Co., Ltd.), a BLSB-5 circulating pump (Nanjing David instruments and equipments Co., Ltd.), an RS-FS1406 multifunctional pulverizer (Heifengying Shida Xiao Co., Ltd.), and an HH-8 numerical display constant-temperature water bath (Nantan instruments and low temperature cooling factories, Jintani).
2. Drugs and reagents
The crude radix Angelicae sinensis decoction pieces and ferulic acid (batch number 110773-; ligustilide (batch: 91980008) reference substance was purchased from Shanghai' an spectral laboratory science and technology, Inc.; methanol (analytically pure); phosphoric acid (chromatographically pure); acetonitrile (chromatographically pure); 50% edible alcohol, a certain brand of yellow wine (semi-sweet type) and a certain brand of strong aromatic white spirit (58% vol) are all purchased from chain supermarkets.
Example 1: processing the angelica decoction pieces for preparing the angelica blood-enriching decoction:
weighing raw angelica sinensis decoction pieces with the thickness of 1.5-2.5 mm, weighing the raw angelica sinensis decoction pieces, weighing the half-sweet yellow wine which is equivalent to one tenth of the weight of the angelica sinensis, and placing the half-sweet yellow wine in a sprinkling can. Firstly, flatly paving raw angelica sinensis decoction pieces in a proper container, uniformly spraying semi-sweet yellow wine on the angelica sinensis decoction pieces, sealing and stewing for 4 hours until the two surfaces of the angelica sinensis decoction pieces are completely wetted, and completely infiltrating the interior of the angelica sinensis decoction pieces with the yellow wine until the interior of the angelica sinensis decoction pieces is thoroughly infiltrated; air drying at room temperature until radix Angelicae sinensis decoction pieces are easily broken and have strong bouquet, and the processing process and the obtained radix Angelicae sinensis decoction pieces are shown in figure 1.
Example 2: content determination of raw angelica decoction pieces
Purchasing 10 batches of angelica decoction pieces from three regions, and performing content of purchased raw angelica decoction pieces according to relevant regulations in 'Chinese pharmacopoeia' 2020 edition, wherein the chromatographic conditions are as follows: octadecylsilane chemically bonded silica is used as a filler, and acetonitrile: 0.085% phosphoric acid solution (17: 83) was used as the mobile phase, the detection wavelength was 316nm, and the column temperature was 35 ℃. The producing area and the batch number of 10 purchased angelica decoction pieces are shown in table 1, and the content measurement results of 10 raw angelica are shown in table 1 and fig. 2.
TABLE 110 measurement results of the origin, lot number and content of the crude angelica
According to the regulations of pharmacopeia, the ferulic acid content in dried raw angelica decoction pieces is not less than 0.050%, the ferulic acid content in the purchased angelica decoction pieces is between 0.064 and 0.081 percent, and the purchased angelica decoction pieces meet the pharmacopeia standards.
Example 3: the processing method of the processing technique of the wine-washed angelica decoction pieces with the functions of enriching the blood and generating the blood is carried out according to the following method.
Performing primary evaluation on the processed radix Angelicae sinensis by HPLC, precisely weighing 0.2g sample, precisely adding 20mL water, performing ultrasonic treatment for 30min, and sampling the filtrate with 0.45 μm microporous membrane. The processing of angelica was initially evaluated according to the chromatographic conditions described in table 2. HPLC chromatographic conditions: the chromatographic column was Hypersil C18 ODS, and the mobile phases were 0.08% phosphoric acid aqueous solution (A) and acetonitrile (B), respectively, flow rates: 1.0mL/min -1 SPD-20AV uv-vis detector detection wavelength: 316nm, sample size: 10 mu L of the solution; column temperature: at 30 ℃.
TABLE 2 preliminary evaluation of gradient elution conditions for the processing procedure
(1) Selection of types of the processing wine:
the invention selects three types of wine of 50 percent edible alcohol, yellow wine (semi-sweet type) and white wine (58 percent vol), respectively spreads angelica decoction pieces in a proper vessel according to the proportion of 10:1 (g: g) of angelica and wine, uniformly sprays the wine on the angelica decoction pieces, seals and smoothes for 4 hours until both sides of the angelica are completely wetted, and the inside of the angelica is completely soaked by the wine to be transparent; air drying at normal temperature until radix Angelicae sinensis decoction pieces are easily broken and have strong bouquet. And (4) carrying out quality evaluation on the processed wine-washed angelica decoction pieces by using an HPLC method. Samples were prepared as described in example 1 and eluted and analyzed as shown in table 2, with the results shown in table 3 and figure 3.
TABLE 3 measurement results of the effect of processing radix Angelicae sinensis decoction pieces with different wines
The results show that the effective components such as ferulic acid obtained by processing the angelica decoction pieces with yellow wine have the highest content. Therefore, the yellow wine is selected as the auxiliary material for processing the angelica decoction pieces washed with the wine.
(3) Influence of the wine adding amount on the processing effect of the wine-washed angelica decoction pieces:
taking 3 batches of crude angelica decoction pieces, 50g of each batch, spreading the angelica decoction pieces in a proper container, adding yellow wine according to the proportion of 10:1, 10:2 and 10:3 (g: g) of angelica and yellow wine respectively, sealing and stewing for 4 hours until the two sides of the angelica are completely wetted, and the inside of the angelica decoction pieces is also completely soaked by the wine until the angelica is thoroughly soaked; and (5) drying at normal temperature. The quality of the processed alcohol-washed angelica pieces was evaluated by HPLC, samples were prepared as described in example 1, and eluted and analyzed as shown in table 2, and the results are shown in table 4 and fig. 4.
TABLE 4 determination of ferulic acid content in samples of Angelica keiskei with different alcohol addition
The results show that: the ratio of the angelica and the yellow wine is 10: the highest ferulic acid content was found at 1 (g: g). The addition of a proper amount of yellow wine can sufficiently promote the dissolution of the effective components, but if the amount of the yellow wine is excessive, the effective components are dissolved and lost. The research result of the invention shows that when the ratio of the angelica and the yellow wine is 10:1 (g: g), the content of the effective component is the highest.
(4) Influence of stir-drying, airing and drying on alcohol washing of angelica decoction pieces:
taking 3 batches of crude angelica decoction pieces, each 50g, spreading the angelica decoction pieces in a proper container, adding yellow wine according to the ratio of 10:1 (g: g) of the angelica to the yellow wine, sealing and stewing for 4 hours until both sides of the angelica are completely wetted, and the inside of the angelica decoction pieces is also completely soaked by the wine to be transparent; drying the obtained radix Angelicae sinensis decoction pieces by different methods. The quality of the processed alcohol-washed angelica decoction pieces was evaluated by HPLC, samples were prepared as described in example 1, and eluted and analyzed as shown in table 2, and the results are shown in table 5 and fig. 5.
TABLE 5 Effect of different drying regimes on ferulic acid content in wine washed Angelica sinensis samples
The results show that: the content of active ingredients in the dried decoction pieces is higher than that of the effective ingredients in the angelica sinensis after stir-frying and drying, and the effective ingredients in the angelica sinensis can be lost due to overhigh temperature, so the angelica sinensis decoction pieces washed with the wine is selected to be dried in the air.
(5) Selecting the types of yellow rice wine for processing:
taking 3 batches of crude angelica decoction pieces, 50g of each batch, spreading the angelica decoction pieces in a proper container, respectively and uniformly adding semi-dry yellow wine, semi-sweet yellow wine and sweet yellow wine according to the proportion of 10:1 (g: g) of angelica and wine, sealing and stewing for 4 hours until the two sides of the angelica are completely wetted, and completely infiltrating the inside of the angelica by the wine until the angelica is thoroughly soaked; air drying at normal temperature until radix Angelicae sinensis decoction pieces are easily broken and have strong bouquet. The quality of the processed angelica sinensis decoction pieces washed with wine was evaluated by HPLC, samples were prepared as described in example 1, and HPLC content measurement was performed under the optimized chromatographic conditions in example 4, and the results are shown in table 6 and fig. 6.
TABLE 6 determination results of processing Chinese angelica decoction pieces with different types of yellow wine
The results show that the ferulic acid content of the angelica sinensis decoction pieces prepared by processing the half-sweet yellow wine is the highest. The yellow wine has high alcohol concentration, is beneficial to dissolving out effective components in the angelica decoction pieces, has moderate sugar content, and cannot generate overhigh influence on the medicine property of the angelica. Therefore, the processed angelica decoction pieces washed with wine are selected from semi-sweet yellow wine as an auxiliary material.
(6) The process summary is as follows: weighing raw angelica sinensis decoction pieces with the thickness of 1.5-2.5 mm, weighing the raw angelica sinensis decoction pieces, weighing the half-sweet yellow wine which is equivalent to one tenth of the weight of the angelica sinensis, and placing the half-sweet yellow wine in a sprinkling can. Firstly, flatly paving angelica sinensis decoction pieces in a proper container, uniformly spraying yellow wine on the angelica sinensis decoction pieces, sealing and stewing for 4 hours until both surfaces of the angelica sinensis are completely wetted, and completely infiltrating the inside of the angelica sinensis decoction pieces with the yellow wine until the angelica sinensis is thoroughly soaked; air drying at normal temperature until radix Angelicae sinensis decoction pieces are easily broken and have strong bouquet.
Example 4: the quality standard of the angelica sinensis decoction pieces washed with the wine is that the angelica sinensis decoction pieces washed with the wine are qualitatively identified by adopting a thin-layer chromatography, and the ferulic acid in the angelica sinensis decoction pieces washed with the wine is quantitatively analyzed by adopting a high performance liquid chromatography.
(1) The qualitative analysis of the wine-washed angelica by thin-layer chromatography is carried out according to the following method:
the obtained angelica decoction pieces washed with wine are taken and are identified according to a thin-layer identification method under the term of the angelica medicinal material in 2020 edition Chinese pharmacopoeia, the prepared angelica decoction pieces washed with wine are identified by taking an angelica reference medicinal material, ferulic acid and ligustilide as reference substances, and the same fluorescent spots are shown at corresponding positions in the thin-layer chromatogram of the prepared angelica decoction pieces washed with wine compared with the reference medicinal material and the reference substances, which are detailed in figures 7 and 8. The experimental result shows that compared with the raw angelica decoction pieces, the obtained angelica decoction pieces washed with wine have no loss of effective components.
(2) High performance liquid chromatography quantitative analysis of ferulic acid:
s1, preparation of control solutions: precisely weighing ferulic acid, placing in a volumetric flask, fixing the volume to the scale with methanol, shaking up, and making into ferulic acid reference solution of 200 μ g/mL.
S2, preparation of a test solution: adding 0.2g of the prepared wine-washed radix Angelicae sinensis powder into a conical flask with a stopper, adding 20mL of methanol precisely, reflux-extracting for 30min, cooling the sample, adding methanol to make up the lost weight, and filtering with 0.45 μm microporous membrane.
According to the invention, through experimental comparison of different extraction methods (ultrasonic and reflux) and different extraction solvents (50% methanol water solution, 50% ethanol water solution, methanol, water and ethanol), the results show that the separation degree of the ferulic acid peak obtained by reflux extraction is good, and the content of the ferulic acid obtained is high, so that the reflux extraction method is adopted, and the detailed chart is shown in figure 9; the investigation of the extraction solvent shows that the methanol extraction has the highest ferulic acid content, so methanol is selected for extraction, and the details are shown in FIG. 10.
S3, liquid chromatography conditions: the chromatographic column takes octadecylsilane chemically bonded silica as a filler and acetonitrile (A): 0.1% aqueous phosphoric acid (B) ═ 13:87 is a mobile phase with the flow rate of 0.5 mL/min; column temperature: 35 ℃; detection wavelength: 316 nm; sample introduction amount: 10 μ L.
The present invention selects a flow rate of 0.5mL/min, since the flow rate (0.5mL/min, 0.8mL/min, 1.0mL/min) was selected, and it was found that the peak area of the obtained ferulic acid was the largest when the flow rate was 0.5 mL/min.
The invention compares the elution effects of a plurality of different elution systems, such as methanol-water, acetonitrile-water, methanol-0.1% of phosphoric acid water, acetonitrile-0.2% of phosphoric acid water, acetonitrile-0.1% of formic acid and the like. As a result, it was found that the peak shape of ferulic acid was good when acetonitrile and 0.1% phosphoric acid water were used as the mobile phase, and acetonitrile and 0.1% phosphoric acid water were finally selected as the mobile phase.
The invention compares the elution effects of different mobile phase ratios, namely 13:87 acetonitrile-0.1% phosphoric acid water, 17:83 acetonitrile-0.1% phosphoric acid water and 20:80 acetonitrile-0.1% phosphoric acid water, and the experimental result shows that when the mobile phase is acetonitrile-0.1% phosphoric acid water, 13:87, the ferulic acid peak can be completely separated and the time consumption is short, and the chromatographic peak of the obtained ferulic acid reference product and the chromatogram of the solution of the ferulic acid sample are shown in figure 11 in detail.
The optimized chromatographic conditions are as follows: the chromatographic column takes octadecylsilane chemically bonded silica as a filler, and acetonitrile (A): 0.1% aqueous phosphoric acid (B) ═ 13:87 is a mobile phase with the flow rate of 0.5 mL/min; column temperature: 35 ℃; detection wavelength: 316 nm; sample introduction amount: 10 μ L.
S4, methodology review:
(1) examination of the linear relationship: 10.00 mu g/mL, 20.00 mu g/mL, 30.00 mu g/mL, 40.00 mu g/mL and 100.00 mu g/mL of ferulic acid reference solution are respectively prepared, sample injection analysis is carried out, the peak area of a ferulic acid chromatogram is recorded, the result is shown in Table 7, the ordinate is the peak area, the abscissa is the sample injection concentration, a standard curve is drawn, and the detail is shown in a graph 12, and linear regression is carried out. The regression equation is: Y55126.4X (R0.9996). The result shows that the ferulic acid reference substance solution has good linear relationship between 10.00 and 100.00 mu g/mL.
TABLE 7 Ferulic acid Linear test results
(2) Precision investigation: and (3) diluting the ferulic acid reference solution to prepare a sample solution of 40 mu g/mL, carrying out sample injection for 6 times according to the optimized chromatographic conditions in the example 4, determining the area of the ferulic acid peak, and calculating the RCD value, wherein the result is shown in Table 8, and the RSD is 0.788%, which indicates that the method has good precision.
TABLE 8 Ferulic acid precision experiment Peak area Retention time and Peak area experiment results
(3) And (3) reproducibility investigation: preparing a test solution from the same batch of angelica powder washed with wine, preparing 6 samples in parallel, injecting samples for 1 time respectively according to the optimized chromatographic conditions under the item of the example 4, recording the peak area of ferulic acid, and calculating the RSD of the chromatographic peak area of the ferulic acid to be 0.425%, which indicates that the method has good reproducibility
TABLE 9 Ferulic acid reproducibility experiment Peak area Retention time and Peak area experiment results
(4) Stability test: preparing a test solution from the same batch of angelica powder washed with wine, performing sample injection analysis for 0, 2, 4, 8, 12 and 24 hours according to the optimized chromatographic conditions under the item of example 4, recording the chromatographic peak area, and calculating the RSD of the chromatographic peak area of ferulic acid to be 1.417%, which indicates that the sample is stable within 24 hours, and the results are shown in Table 10.
TABLE 10 Ferulic acid stability experiment Peak area Retention time and Peak area experiment results
(5) Sample adding and recovering experiment: taking about 0.1g of the known content of angelica powder washed with wine, weighing 6 parts, precisely weighing, sequentially adding 1.0mL of standard solution containing 100% of ferulic acid concentration to 6 groups, shaking up, preparing a sample solution according to the preparation method, carrying out sample injection analysis according to the optimized chromatographic condition under the embodiment 4, recording the chromatographic peak area, calculating the recovery rate, wherein the average recovery rate is 96.33%, and the result shows that the recovery rate of the method is good and is shown in Table 11.
TABLE 11 Ferulic acid sample recovery test results
(6) And (3) system adaptability experiment: take extended-C185 μm (250X 4.6mm), Hypersil ODS 5 μm (250X 4.6mm), Newmate in sequence TM C18(250 x 4.6mm) octadecylsilane chemically bonded silica chromatographic columns produced by three different manufacturers, 100 mu g/mL of reference substance and test solution are taken and sample injection is carried out according to the chromatographic conditions optimized in the example 4, the results are shown in Table 12 and FIGS. 13A-C, and it can be seen that the ferulic acid content difference measured by different chromatographic columns is small, the RSD value of the ferulic acid content difference is 3.78% and is less than 5%, and the method has good system adaptability.
TABLE 12 Ferulic acid System Adaptation Experimental results
S5, preparing a sample solution from 10 batches of prepared alcohol-washed Chinese angelica decoction pieces, injecting the sample solution into a high performance liquid chromatograph for analysis according to the method in the embodiment 4, and recording a chromatogram; the results are shown in Table 13.
TABLE 1310 content of Ferulic acid in wine washed Angelica sinensis
The results show that the prepared angelica decoction pieces processed by the wine have higher ferulic acid content than the raw angelica decoction pieces, the ferulic acid content is between 0.096 and 0.109 percent, the average content is 0.101 percent, and the content of the ferulic acid in the angelica decoction pieces processed by the invention is regulated to be not less than 0.080 percent according to the mark that the average content is lower than 20 percent.
Example 5 classic famous formula angelica sinensis soup for enriching the blood and preparation method of its reference sample lyophilized powder
Weighing 30g of astragalus decoction pieces and 6g of wine-washed angelica decoction pieces, mashing the astragalus decoction pieces and 6g of wine-washed angelica decoction pieces, sieving the smashed angelica decoction pieces by a sieve with 10 meshes, putting the crushed astragalus decoction pieces into a decoction pot, and adding 400mL of water into the decoction pot to soak the decoction pieces for 30 min. Decocting with strong fire for 30min, cooling, and filtering. Adding water 200mL, decocting with slow fire for 30min, cooling, and filtering. Mixing the two decoctions to obtain GUIBUXUE decoction;
and (3) carrying out spray freeze-drying on the obtained angelica blood-enriching soup at a feeding flow rate of 15mL/min and a freezing temperature of-35 ℃ without concentrating to obtain the angelica blood-enriching soup reference sample freeze-dried powder.
Example 6: preparation method of angelica sinensis blood-enriching granules
Weighing 30g of astragalus decoction pieces and 6g of wine-washed angelica decoction pieces, mashing the astragalus decoction pieces and 6g of wine-washed angelica decoction pieces, sieving the smashed angelica decoction pieces by a sieve with 10 meshes, putting the crushed astragalus decoction pieces into a decoction pot, and adding 400mL of water into the decoction pot to soak the decoction pieces for 30 min. Decocting with strong fire for 30min, cooling, and filtering. Adding water 200mL, decocting with slow fire for 30min, cooling, and filtering. Mixing the two decoctions to obtain GUIBUXUE decoction; and (3) carrying out spray freeze-drying on the obtained angelica blood-enriching soup at a feeding flow rate of 15mL/min and a freezing temperature of-35 ℃ without concentrating to obtain the angelica blood-enriching soup reference sample freeze-dried powder. Adding a proper amount of dextrin into the freeze-dried powder, using 75-80% ethanol as a bonding agent, and carrying out wet granulation, drying and granule finishing to obtain the freeze-dried powder.
Example 7: the application of the alcohol-washed angelica sinensis decoction pieces is used for preparing angelica sinensis blood-enriching soup and angelica sinensis blood-enriching granules with the effects of tonifying qi and generating blood.
Taking 10 batches of the medicines in the items of the embodiment 5 and the embodiment 6, each batch is 0.2g, precisely weighing, precisely adding 10mL of methanol, weighing, refluxing and extracting for 30min, supplementing the weight loss with methanol after the sample is cooled, and filtering with a 0.45-micron microporous membrane to obtain the medicine.
The sample injection analysis was performed according to the optimized chromatographic conditions of example 4, and the results are shown in Table 14.
TABLE 1410 radix Angelicae sinensis decoction for tonifying blood/radix Angelicae sinensis granule for tonifying blood
Therefore, the prepared wine-washed angelica decoction pieces can be used for preparing the angelica blood-enriching decoction with the functions of tonifying qi and generating blood and the modern preparation angelica blood-enriching granules of the angelica blood-enriching decoction, and the prepared preparation has stable and reliable quality.
Example 8 magnitude transfer study of Ferulic acid between crude radix Angelicae sinensis, alcohol washed radix Angelicae sinensis, radix Angelicae sinensis blood replenishing decoction lyophilized powder, and radix Angelicae sinensis blood replenishing granule
The method is characterized in that the content of the main index component ferulic acid is used as an index, the quantity value transfer of the ferulic acid from raw angelica sinensis decoction pieces to prepared angelica sinensis decoction pieces, the angelica sinensis decoction pieces to angelica blood-enriching decoction freeze-dried powder and the angelica blood-enriching decoction granules is calculated, and the experimental results obtained in the examples 2, 4 and 7 are combined, and the transfer rate is calculated according to the formula (M/M) 100%, wherein M is the content of the index component in the next-stage substance, namely the angelica sinensis, the freeze-dried powder and the granules, and M is the content of the index component in the previous-stage substance, namely the raw angelica sinensis, the angelica sinensis and the freeze-dried powder. The transfer condition of ferulic acid in raw angelica-alcohol washed angelica decoction pieces-freeze-dried powder-granules is researched, and a theoretical basis is provided for developing angelica blood-enriching decoction from traditional decoction into modern granules.
As shown in Table 15, the transfer rate of ferulic acid from crude radix Angelicae sinensis decoction pieces to processed radix Angelicae sinensis decoction pieces was 117.72-150.00%, the average transfer rate was 135.03%, and the RSD value was 7.78%. The transfer rate of ferulic acid from processed angelica decoction pieces to angelica blood-enriching decoction freeze-dried powder is between 62.96 and 73.12 percent, the average transfer rate is 66.03 percent, and the transfer rate RSD value is 5.58 percent. The transfer rate of ferulic acid from angelica sinensis blood-enriching decoction freeze-dried powder to angelica sinensis blood-enriching granules is 19.12-20.63%, the average transfer rate is 19.94%, and the transfer rate RSD value is 2.51%. As can be seen, the transfer rate of the ferulic acid is not discrete data, and is very high, which indicates that the processing technology is excellent, can retain the effective components in the medicinal materials and promote dissolution to the greatest extent, and can ensure the stability and reliability of the medicine quality in the subsequent application of the angelica.
TABLE 15 magnitude transfer study of ferulic acid in Angelica sinensis
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention, and these changes and modifications are all within the scope of the invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The processing method of the angelica sinensis decoction pieces washed with wine is characterized by comprising the following steps: mixing the raw angelica sinensis decoction pieces with the thickness of 1.5-2.5 mm with the semi-sweet yellow wine, sealing, airing to obtain the wine-washed angelica sinensis decoction pieces.
2. The processing method of the angelica sinensis decoction pieces washed with the wine as claimed in claim 1, wherein the mass ratio of the raw angelica sinensis decoction pieces to the semi-sweet yellow wine is 10: 1.
3. the alcohol-washed angelica decoction pieces obtained by the processing method of claim 1 or 2.
4. The alcohol washed angelica decoction pieces of claim 3, wherein the ferulic acid content in the alcohol washed angelica decoction pieces is 0.092-0.109%.
5. The quality inspection method of alcohol washing angelica decoction pieces as claimed in claim 3 or 4, which comprises the following steps:
qualitatively identifying ferulic acid and ligustilide in radix Angelicae sinensis decoction pieces washed with wine by thin layer chromatography;
the high performance liquid chromatography is used for measuring the content of ferulic acid in the alcohol washing angelica decoction pieces:
s1, preparing ferulic acid reference solution and alcohol washing angelica decoction piece test solution;
s2, respectively carrying out high performance liquid chromatography determination on the ferulic acid reference solution and the test solution of the alcohol washing angelica decoction pieces; chromatographic conditions are as follows: acetonitrile-0.1% phosphoric acid water is used as a mobile phase, and the flow rate is 0.5-1.0 mL/min.
6. The method for detecting the quality of the angelica sinensis decoction pieces washed with the wine as claimed in claim 5, wherein the volume ratio of acetonitrile to 0.1% phosphoric acid water is 13:87, and the flow rate is 0.5 mL/min.
7. The method for detecting the quality of angelica sinensis decoction pieces washed with wine as claimed in claim 5, wherein octadecylsilane chemically bonded silica is used as filler in a chromatographic column used in high performance liquid chromatography.
8. The method for detecting the quality of the alcohol washed angelica decoction pieces as claimed in claim 5, wherein the preparation of the test solution of the alcohol washed angelica decoction pieces comprises the following steps: pulverizing the decoction pieces, adding methanol, heating under reflux, cooling, weighing, adding methanol to balance the weight, shaking, filtering, and filtering with 0.45 μm microporous membrane to obtain the sample solution.
9. The quality detection method of alcohol washing angelica decoction pieces as claimed in claim 5, wherein the preparation of ferulic acid reference solution comprises the following steps: dissolving ferulic acid with methanol to set concentration to obtain ferulic acid reference solution.
10. A Chinese medicinal prescription, DANGGUIBUXUE decoction, is prepared from the wine-washed decoction pieces of radix Angelicae sinensis and the decoction pieces of radix astragali of claim 3 or 4 at a mass ratio of 1: 5, soaking in water, decocting with strong fire, then adding water and decocting with slow fire, and mixing the two decoctions to obtain the angelica blood-enriching soup.
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