Optimal alcohol extraction process of angelica sinensis and caulis spatholobi decoction obtained through AHP-entropy weight method
Optimizing the alcohol extraction process through the AHP-entropy weight method and orthogonal design method, determining the best process parameters, solving the problems of the extraction efficiency and poor product quality of traditional Chinese medicine compound prescriptions in the prior art, and achieving more efficient extraction results and better product quality.
Patent Information
- Application Number
- CN202411753888.6
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-02
- Publication Date
- 2025-02-11
AI Technical Summary
The existing Chinese medicine compound extraction process is difficult to comprehensively evaluate the extraction effect of various active ingredients, and the extraction efficiency and product quality are average.
The AHP-entropy weight method combined with orthogonal design method is used to optimize the alcohol extraction process and determine the optimal alcohol extraction process parameters, such as ethanol concentration 65%, material-liquid ratio 1:10, extraction temperature 70℃, extraction times 3 times, extraction time 2h.
It improves extraction efficiency and product quality, and is suitable for the industrial production of Angelica Chicken Blood Vine Soup.
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Figure CN119406092A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of extracting ingredients from Chinese herbs, and in particular to an optimal alcohol extraction process for obtaining Angelica Sinensis Millettia Spatholobi decoction by using an AHP-entropy weight method. Background Art
[0002] Angelica and Millettia Soup is from the Chinese Traumatology. It is composed of 6 Chinese herbs: Angelica, Millettia, Rehmannia glutinosa, Salvia miltiorrhiza, White Peony Root and Longan. It is mainly used to treat patients with weak Qi and blood in the late stage of bone injury; patients with leukopenia and thrombocytopenia during chemotherapy or radiotherapy. In the traditional Chinese medicine compound extraction process, decoction is a common extraction method.
[0003] In the comprehensive evaluation process of the extraction process of traditional Chinese medicine compound, it is very important to assign reasonable weights to the selected indicators. The current indicator weighting methods can be roughly divided into two categories, namely subjective weighting method and objective weighting method. Among the subjective weighting methods, the analytic hierarchy process (AHP) has clear ideas, is concise and practical, and is widely used; among the objective weighting methods, the entropy weight method has strong mathematical theory support and high indicator weighting accuracy.
[0004] However, in order to better exert the effect of Danggui Jixueteng Decoction on replenishing qi and nourishing blood, the extraction process of the main active ingredients needs to be optimized. The existing extraction process is difficult to fully evaluate the extraction effect of multiple active ingredients in the compound, and the extraction efficiency and product quality are average.
[0005] Therefore, it is necessary to provide an optimal alcohol extraction process for Angelica Millettia Spatholobi decoction by using the AHP-entropy weight method, aiming to optimize the alcohol extraction process by combining the AHP-entropy weight method with the orthogonal design method to improve the extraction efficiency and product quality. Summary of the invention
[0006] In order to solve the above technical problems, the present invention provides an optimal alcohol extraction process for Danggui Millettia Spatholobi decoction by using an AHP-entropy weight method. By investigating the extraction process of the main active ingredients, it is determined that the alcohol extraction process is used to extract the effective substances in DJD. The components with higher content are used as evaluation indicators. On the basis of single factor investigation, orthogonal design is used to screen the optimal extraction process, and the optimal extraction process of the DJD compound is obtained.
[0007] The optimal alcohol extraction process for obtaining Angelica Sinensis Millettia Decoction by using the AHP-entropy weight method provided by the present invention comprises the following steps:
[0008] S1. Determine the evaluation index of the extraction process and establish the method for determining the content of the index components;
[0009] S2. Use the analytic hierarchy process (AHP) to subjectively weight the importance of each evaluation indicator, construct a priority judgment matrix for pairwise comparison, and calculate the weight coefficient of each evaluation indicator;
[0010] S3. Calculate the objective weighting of each evaluation index using the entropy weight method to determine the information entropy and weight coefficient of each evaluation index;
[0011] S4, combining the weight coefficients obtained by the AHP method and the entropy weight method to determine the comprehensive weight coefficient of each evaluation index;
[0012] S5. Conduct a single factor investigation on the extraction process and use orthogonal design to screen the best extraction process: take ethanol concentration, solid-liquid ratio and extraction temperature as investigation factors, conduct a 3-factor 3-level combination experiment, take the content of each evaluation index as the evaluation index, use the comprehensive weight coefficient to comprehensively score the index, and screen out the best alcohol extraction process: ethanol concentration of 65%, solid-liquid ratio of 1:10, extraction temperature of 70°C, extraction times of 3 times, and extraction time of 2h.
[0013] Preferably, the evaluation indexes of the extraction process include: the contents of epicatechin, peony lactone glycosides, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide.
[0014] Preferably, the method for determining the content of the indicative component comprises the following steps: setting chromatographic conditions; preparing a mixed reference solution; preparing a test solution; under the set chromatographic conditions, taking the reference solution and the test solution to determine the peak area of the indicative component to examine the specificity of the content determination method.
[0015] Preferably, the steps of single factor investigation of extraction process are as follows:
[0016] According to the prescription ratio, 0.69 g of DJD prescription medicinal materials were weighed and the warm immersion method was used. The peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide were used as evaluation indicators. With the increase of the number of extractions, the content of each component showed an upward trend. In order to fully extract the effective ingredients, the number of extractions was finally determined to be 3 times. The solid-liquid ratio (A), ethanol concentration (B) and extraction temperature (C) in the extraction process were investigated single-factor.
[0017] Preferably, the steps of using orthogonal design to screen the best extraction process are as follows:
[0018] Based on the single factor experiment, L9(3 3 ) orthogonal experiment, with solid-liquid ratio, ethanol concentration and extraction temperature as investigation factors, a three-factor three-level combination experiment was carried out, and the contents of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide were used as evaluation indicators. The AHP-entropy weight method was used to comprehensively score the indicators and screen the optimal alcohol extraction process.
[0019] Preferably, the chromatographic conditions are:
[0020] Chromatographic column: ChromCore AQ C18 column (5μm, 4.6×250mm), mobile phase is acetonitrile-0.1% phosphoric acid aqueous solution, gradient elution: 0-21min, 7%A→15%A; 21-32min, 15%A→20%A; 33-43min, 20%A→25%A; 43-48min, 25%A→40%A; 48-62min, 40%A→95%A; volume flow rate 1.0mL / min, column temperature 30°C, measurement wavelength 232nm, injection volume 10μl, equilibrated for 20min under its initial conditions before injection.
[0021] Preferably, the preparation method of the mixed reference solution is:
[0022] Accurately weigh appropriate amounts of epicatechin, abiogenin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide reference substances, add methanol (chromatographic grade) solution, ultrasonicate for 15 min to dissolve them completely, then oscillate to mix them evenly to prepare a mixed reference substance solution containing 40.0 μg / mL of epicatechin, 80.0 μg / mL of abiogenin, 555.5 μg / mL of paeoniflorin, 30.0 μg / mL of ferulic acid, 56.0 μg / mL of PGG, 30.2 μg / mL of lithospermic acid, 375.0 μg / mL of salvianolic acid B, and 293.0 μg / mL of ligustilide.
[0023] Preferably, the preparation method of the test solution is:
[0024] Weigh the slices according to the prescription, add 8 times of water, reflux and extract for 2h, extract 3 times, filter and concentrate, take the extract and dilute it to a certain multiple, and then spin at 12000r·min -1 Centrifuge for 5 min and filter through a 0.45 μm microporous membrane to obtain the test solution.
[0025] Preferably, the steps of measuring the reference solution and the test solution are:
[0026] P1. Take different concentrations of the reference substance solutions respectively, determine the peak area according to the above chromatographic conditions, draw the standard curve with the concentration as the abscissa (X) and the peak area as the ordinate (Y), and determine the regression equation and linear range of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide;
[0027] P2. Take the test solution and inject it continuously for 6 times according to the above chromatographic conditions, calculate the RSD of the peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide, and examine the precision of the instrument;
[0028] P3. Take 6 samples of the prepared test solution for testing, calculate the RSD of the peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide, and examine the repeatability of the method;
[0029] P4. Take the test solution and inject it at 0, 2, 4, 8, 12, and 24 hours respectively, calculate the RSD of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B, and ligustilide content, and determine the 24-hour stability of the sample;
[0030] P5. Taking the contents of epicatechin, albiflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide obtained from the repeatability test as the sample content, take 12 portions of DJD sample, accurately add the reference stock solution of each component in a gradient of 80%, 100%, and 120% of the content of each component in the sample, pass through a 0.22μm filter membrane, prepare the test solution, inject the sample, determine the recovery rate, calculate the average sample recovery rate, and examine the accuracy of the method.
[0031] Compared with the related art, the optimal alcohol extraction process of Angelica Millettia Spatholobi Decoction obtained by the AHP-entropy weight method provided by the present invention has the following beneficial effects:
[0032] The present invention uses AHP and entropy weight method in a comprehensive manner, which can not only reduce the subjective error of AHP method, but also combine the test data with mathematical thinking, and is very suitable for the study of multi-index evaluation of traditional Chinese medicine compound.
[0033] The present invention uses the contents of epicatechin, peony lactone glycosides, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide as comprehensive evaluation indicators, and adopts orthogonal design combined with AHP-entropy weight method to optimize the alcohol extraction process of DJD, in order to provide a reference for the subsequent development of DJD preparations;
[0034] The process of the invention has the advantages of simple operation, high extraction efficiency, good product quality, etc., and is suitable for the industrial production of angelica and millettia reticulata soup. BRIEF DESCRIPTION OF THE DRAWINGS
[0035] Figure 1 It is a schematic diagram of the changes in the content of each evaluation index component in the present invention.
[0036] Figure symbols: A: DJD test solution; B: standard; 1: epicatechin; 2: paeoniflorin; 3: paeoniflorin; 4: ferulic acid; 5: PGG; 6: lithospermic acid; 7: salvianolic acid B; 8: ligustilide. DETAILED DESCRIPTION
[0037] The present invention will be further described below in conjunction with the accompanying drawings and implementation modes.
[0038] The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by the AHP-entropy weight method proposed in the present invention is as follows:
[0039] 1. Establishment of the determination method of index component content
[0040] 1.1 Chromatographic conditions
[0041] Chromatographic column: ChromCore AQ C18 column (5 μm, 4.6×250 mm), mobile phase: acetonitrile (A)-0.1% phosphoric acid aqueous solution (B), gradient elution: 0-21 min, 7% A→15% A; 21-32 min, 15% A→20% A; 33-43 min, 20% A→25% A; 43-48 min, 25% A→40% A; 48-62 min, 40% A→95% A. Volume flow rate: 1.0 mL / min, column temperature: 30°C, measurement wavelength: 232 nm, injection volume: 10 μL, equilibrated for 20 min under the initial conditions before injection.
[0042] 1.2 Preparation of mixed reference solution
[0043] Accurately weigh appropriate amounts of epicatechin, abiogenin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide reference substances, add methanol (chromatographic grade) solution, ultrasonicate for 15 min to dissolve them completely, then oscillate and mix them to prepare a mixed reference substance solution containing 40.0 μg / mL of epicatechin, 80.0 μg / mL of abiogenin, 555.5 μg / mL of paeoniflorin, 30.0 μg / mL of ferulic acid, 56.0 μg / mL of PGG, 30.2 μg / mL of lithospermic acid, 375.0 μg / mL of salvianolic acid B, and 293.0 μg / mL of ligustilide.
[0044] 1.3. Preparation of test solution
[0045] Weigh the slices according to the prescription, add 8 times of water, reflux and extract for 2h, extract 3 times, filter and concentrate, take the extract and dilute it to a certain multiple, and then spin at 12000r·min -1 Centrifuge for 5 min and filter through a 0.45 μm microporous membrane to obtain the test solution.
[0046] 1.4 Methodological Investigation
[0047] The reference solution under item "1.2" and the test solution under item "1.3" are measured according to the chromatographic conditions under item "1.1" to examine the specificity of the content determination method.
[0048] Take different concentrations of the reference solution series respectively, determine the peak area according to the chromatographic conditions under "1.1", draw the standard curve with concentration as the horizontal axis (X) and the peak area as the vertical axis (Y), and determine the regression equation and linear range of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide.
[0049] The test solution was taken and continuously sampled and measured 6 times according to the chromatographic conditions under "1.1", and the RSD of the peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide was calculated to examine the precision of the instrument.
[0050] Prepare the test solution according to the method under "1.3", take 6 samples for measurement, calculate the RSD of the peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide, and examine the repeatability of the method.
[0051] The test solution was sampled and measured at 0, 2, 4, 8, 12, and 24 h, and the RSD of the contents of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B, and ligustilide was calculated to determine the 24 h stability of the sample.
[0052] Taking the contents of epicatechin, albiflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide obtained from the repeatability test as the sample content, 12 portions of DJD samples were taken, and the reference stock solution of each component was accurately added at a gradient of 80%, 100%, and 120% of the content of each component in the sample. The solution was filtered through a 0.22μm filter membrane to prepare the test solution. The sample was injected, the recovery rate was determined, and the average sample recovery rate was calculated to investigate the accuracy of the method.
[0053] Table 1 Investigation on the methodological approach for determining the content of index components
[0054]
[0055] 2. Comprehensive evaluation
[0056] 2.1 AHP subjective weighting
[0057] In this experiment, epicatechin, peony lactone glycosides, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide contents were used as evaluation indicators. The importance of each evaluation indicator was divided into three levels, with the priority order being salvianolic acid B content > paeoniflorin content > ligustilide content > PGG content > epicatechin content > ferulic acid = lithospermic acid content > peony lactone glycoside content, and a priority judgment matrix for pairwise comparison was constructed, as shown in Table 2. SPSSAU software was used to measure the weight coefficients ωAHP of each evaluation indicator, which were 0.0618, 0.0316, 0.2775, 0.0555, 0.0703, 0.0559, 0.3425 and 0.1050, respectively, and the consistency ratio CR = 0.055 < 0.10, indicating that the judgment matrix score has good consistency and the weight coefficient is effective.
[0058] Table 2 Judgment Matrix
[0059]
[0060] 2.2 Objective weighting by entropy weight method
[0061] The entropy weight method is a method to determine the weight of indicators based on the amount of information provided by each factor and the amount of information provided by each indicator value. The entropy weight method can determine the degree of dispersion of indicator components, thereby reflecting the impact of indicator components on comprehensive evaluation. The data of each indicator are standardized and translated, and the original data are converted into a probability matrix (Pij), so as to calculate the information entropy (Hj) of each indicator, and finally obtain the entropy weight coefficient (Wj).
[0062]
[0063]
[0064]
[0065] 2.3. Comprehensive determination of weight coefficients using the AHP-entropy weight method
[0066] The AHP method focuses on subjective evaluation and is greatly influenced by subjectivity, while the entropy weight method focuses on mining the objective information contained in the data itself, but cannot reflect the compatibility relationship between the main, secondary, adjuvant and envoy of each medicine in the prescription. Taking the subjective weight coefficient and the objective weight coefficient into consideration can reduce the bias of using a single weighting method and make the results more comprehensive and reasonable.
[0067] Use α and β to represent the relative importance of subjective weight and objective weight respectively. Here we will use the idea of matrix to calculate the importance coefficient α of subjective weight and objective weight. i and β i, where i = 1, 2, ..., n, the formula is as follows,
[0068] α i =v i / (v i +w j ) (4)
[0069] β i =w j / (v i +w j ) (5)
[0070] where v i is the weight obtained by the hierarchical analysis method, w j is the weight obtained by entropy method.
[0071] Comprehensive weight Z j The formula is as follows:
[0072]
[0073] The comprehensive weight (Wj) was calculated according to the above formula. The comprehensive weight coefficients of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide were 0.1615, 0.0536, 0.1898, 0.1113, 0.0919, 0.0593, 0.2382 and 0.0942, respectively.
[0074] 2.4. AHP-entropy weight method to determine the comprehensive score
[0075] The G1-entropy weight method is used to give a comprehensive score (Pj) to the index components, which is calculated according to formula (7).
[0076]
[0077] In formula (7), y j represents the jth evaluation index, y jmax Represents the maximum value of the jth evaluation index.
[0078] 3. Study on the extraction process of Angelica Sinensis Millettia Soup
[0079] 3.1. Single factor investigation of extraction process
[0080] According to the prescription ratio, 0.69 g of DJD prescription medicinal materials were weighed and the warm immersion method was used. The peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide were used as evaluation indicators. With the increase of the number of extractions, the content of each component showed an upward trend. In order to fully extract the effective ingredients, the number of extractions was finally determined to be 3 times. The solid-liquid ratio (A), ethanol concentration (B) and extraction temperature (C) in the extraction process were investigated by single factor, and the investigated factors are shown in Table 3.
[0081] Table 3 Factor Levels Table 1
[0082]
[0083] The results of the single factor test show that, taking the content of the ingredient as the evaluation index, the content is highest in the 1:8 solid-liquid ratio. With the increase of the alcohol addition multiple, the content first increases and then stabilizes, so 1:6, 1:8 and 1:10 are selected as the orthogonal design. The ethanol concentration is highest at 85%. With the increase of ethanol concentration, the content first increases and then decreases, so 65%, 75%, 85% are selected as the orthogonal design. In the extraction temperature, the content gradually increases with the increase of extraction temperature, so 90℃ is selected as the orthogonal design.
[0084] 3.2. Orthogonal design to screen the best extraction process
[0085] Based on the single factor experiment, L9(3 3 ) Orthogonal test, with solid-liquid ratio (A), ethanol concentration (B) and extraction temperature (C) as the investigation factors, a 3-factor 3-level combination experiment was carried out, and the contents of epicatechin (Y1), paeoniflorin (Y2), paeoniflorin (Y3), ferulic acid (Y4), PGG (Y5), lithospermic acid (Y6), salvianolic acid B (Y5) and ligustilide (Y6) were used as evaluation indicators. The AHP-entropy weight method was used to comprehensively score the indicators (Y) to screen the optimal alcohol extraction process. The factor level table is shown in Table 4, the orthogonal experimental design and results are shown in Table 5, and the variance analysis is shown in Table 6.
[0086] Table 4 Factor levels Table II
[0087]
[0088] Table 5 Orthogonal experimental design and results
[0089]
[0090] Table 6 Analysis of variance of comprehensive scores of orthogonal experiments
[0091]
[0092] From the intuitive analysis of Table 5, it can be seen that the order of influence of each factor on the comprehensive score of the experimental results is B>C>A, and the mean size of each factor is B1>B2>B3, C1>C3>C2, A3>A2>A1; from the variance analysis results of Table 6, it can be seen that the solid-liquid ratio factor has no significant effect on the comprehensive score of the experimental results when the test level α=0.05. This may be because considering the decoction conditions of traditional Chinese medicine, the factor level spacing is not large, so the difference in the obtained results is not obvious. In order to extract the ingredients in the compound to the greatest extent, ensure the therapeutic effect, and take into account the time and cost in production, the present invention selects the group with the highest comprehensive score, that is, the extraction process is A3B1C1, that is, the solid-liquid ratio is 10 times, the ethanol concentration is 65%, the extraction temperature is 70°C, and the number of extractions is 3 times.
[0093] Compared with the related art, the optimal alcohol extraction process of Angelica Millettia Spatholobi Decoction obtained by the AHP-entropy weight method provided by the present invention has the following beneficial effects:
[0094] In the early stage of the present invention, the extract obtained by the traditional water decoction method and the alcohol extraction method were compared by liquid chromatography. The content of the components obtained in the alcohol extraction method was not much different from that of the water decoction method, and fat-soluble components were detected in the high organic phase. Therefore, the alcohol extraction method was selected for process optimization. In addition, the present invention also investigated the influence of gradient elution of different mobile phases (methanol-0.1% phosphoric acid solution and acetonitrile-0.1% phosphoric acid solution) on the experimental results. The results showed that when gradient elution was performed with acetonitrile-0.1% phosphoric acid solution as the mobile phase, the chromatographic peak separation and symmetry of each component in DJD were good, and the baseline was stable. In wavelength selection, the prepared test solution was diluted to a certain concentration and then wavelength scanning was performed. The test solution was measured at 232, 254, 286, and 315 nm. The peak height and peak area of the chromatogram at 232 nm were much larger than those at 286, 254, and 315 nm, but ligustilide also had strong absorption at 286 nm. After comprehensive consideration, the components were determined at 232 nm.
[0095] The present invention adopts a single factor experiment to investigate the influence of different factors on the index components, and then adopts the AHP-entropy weight method to determine the weight coefficients of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide indicators, and combines the orthogonal design to optimize the alcohol extraction process parameters of DJD. The optimal alcohol extraction process obtained by optimization is stable and feasible, which can provide a reference for the preparation and research of DJD.
[0096] The above descriptions are merely embodiments of the present invention and are not intended to limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made using the contents of the present invention specification and drawings, or directly or indirectly applied in other related technical fields, are also included in the patent protection scope of the present invention.
Claims
1. An optimal alcohol extraction process for Danggui Millettia Spatholobi decoction obtained by AHP-entropy weight method, characterized in that: The following steps are involved: S1. Determine the evaluation index of the extraction process and establish the method for determining the content of the index components; S2. Use the analytic hierarchy process (AHP) to subjectively weight the importance of each evaluation indicator, construct a priority judgment matrix for pairwise comparison, and calculate the weight coefficient of each evaluation indicator; S3. Calculate the objective weighting of each evaluation index using the entropy weight method to determine the information entropy and weight coefficient of each evaluation index; S4, combining the weight coefficients obtained by the AHP method and the entropy weight method to determine the comprehensive weight coefficient of each evaluation index; S5. Conduct a single factor investigation on the extraction process and use orthogonal design to screen the best extraction process: take ethanol concentration, solid-liquid ratio and extraction temperature as investigation factors, conduct a 3-factor 3-level combination experiment, take the content of each evaluation index as the evaluation index, use the comprehensive weight coefficient to comprehensively score the index, and screen out the best alcohol extraction process: ethanol concentration of 65%, solid-liquid ratio of 1:10, extraction temperature of 70°C, extraction times of 3 times, and extraction time of 2h.
2. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method according to claim 1, characterized in that: The evaluation indicators of the extraction process included the contents of epicatechin, peony lactone glycosides, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide.
3. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method according to claim 1, characterized in that: The method for determining the content of an index component includes the following steps: setting chromatographic conditions; preparing a mixed reference solution; preparing a test solution; under the set chromatographic conditions, taking the reference solution and the test solution to determine the peak area of the index component to examine the specificity of the content determination method.
4. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method according to claim 1, characterized in that: The steps of single factor investigation of extraction process are as follows: According to the prescription ratio, 0.69 g of DJD prescription medicinal materials were weighed and the warm immersion method was used. The peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide were used as evaluation indicators. With the increase of the number of extractions, the content of each component showed an upward trend. In order to fully extract the effective ingredients, the number of extractions was finally determined to be 3 times. The solid-liquid ratio (A), ethanol concentration (B) and extraction temperature (C) in the extraction process were investigated single-factor.
5. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method according to claim 1, characterized in that: The steps for screening the best extraction process using orthogonal design are as follows: Based on the single factor experiment, L9(3 3 ) orthogonal experiment, with solid-liquid ratio, ethanol concentration and extraction temperature as investigation factors, a three-factor three-level combination experiment was carried out, and the contents of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide were used as evaluation indicators. The AHP-entropy weight method was used to comprehensively score the indicators and screen the optimal alcohol extraction process.
6. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method as claimed in claim 3, characterized in that: The chromatographic conditions are: Chromatographic column: ChromCore AQ C18 column (5μm, 4.6×250mm), mobile phase is acetonitrile-0.1% phosphoric acid aqueous solution, gradient elution: 0-21min, 7%A→15%A; 21-32min, 15%A→20%A; 33-43min, 20%A→25%A; 43-48min, 25%A→40%A; 48-62min, 40%A→95%A; volume flow rate 1.0mL / min, column temperature 30°C, measurement wavelength 232nm, injection volume 10μl, equilibrated for 20min under its initial conditions before injection.
7. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method as claimed in claim 3, characterized in that: The preparation method of the mixed reference solution is: Accurately weigh appropriate amounts of epicatechin, albiflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide reference substances, add methanol (chromatographic grade) solution, ultrasonicate for 15 min to dissolve them completely, then oscillate to mix them evenly to prepare a mixed reference substance solution containing 40.0 μg / mL of epicatechin, 80.0 μg / mL of albiflorin, 555.5 μg / mL of paeoniflorin, 30.0 μg / mL of ferulic acid, 56.0 μg / mL of PGG, 30.2 μg / mL of lithospermic acid, 375.0 μg / mL of salvianolic acid B, and 293.0 μg / ml of ligustilide.
8. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method as claimed in claim 3, characterized in that: The preparation method of the test solution is: Weigh the slices according to the prescription, add 8 times of water, reflux and extract for 2h, extract 3 times, filter and concentrate, take the extract and dilute it to a certain multiple, and then spin at 12000r·min -1 Centrifuge for 5 min and filter through a 0.45 μm microporous membrane to obtain the test solution.
9. The optimal alcohol extraction process of Danggui Millettia Spatholobi Decoction obtained by AHP-entropy weight method as claimed in claim 3, characterized in that: The steps for determining the reference solution and the test solution are as follows: P1. Take different concentrations of the reference substance solutions respectively, determine the peak area according to the above chromatographic conditions, draw the standard curve with the concentration as the abscissa (X) and the peak area as the ordinate (Y), and determine the regression equation and linear range of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide; P2. Take the test solution and inject it continuously for 6 times according to the above chromatographic conditions, calculate the RSD of the peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide, and examine the precision of the instrument; P3. Take 6 samples of the prepared test solution for testing, calculate the RSD of the peak areas of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide, and examine the repeatability of the method; P4. Take the test solution and inject it at 0, 2, 4, 8, 12, and 24 hours respectively, calculate the RSD of epicatechin, paeoniflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B, and ligustilide content, and determine the 24-hour stability of the sample; P5. Taking the contents of epicatechin, albiflorin, paeoniflorin, ferulic acid, PGG, lithospermic acid, salvianolic acid B and ligustilide obtained from the repeatability test as the sample content, take 12 portions of DJD sample, accurately add the reference stock solution of each component in a gradient of 80%, 100%, and 120% of the content of each component in the sample, pass through a 0.22μm filter membrane, prepare the test solution, inject the sample, determine the recovery rate, calculate the average sample recovery rate, and examine the accuracy of the method.
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