CN111956679A - Preparation method of processed epimedium - Google Patents
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Abstract
The invention discloses a preparation method for processing epimedium, which comprises the steps of adding epimedium medicinal materials into butter and frying; the addition amount of the butter is 10 to 20 percent of the weight percentage of the epimedium herb, the frying temperature is 140 to 180 ℃, and the frying time is 4 to 8 minutes; the herba Epimedii is herba Epimedii. The invention has the beneficial effects that: the invention provides a preparation method of processed epimedium, which integrates various data indexes such as icariin content, total flavone content, 5 main flavone content, alcohol extract content, DPPH free radical scavenging activity and the like, designs and preferably selects an optimal epimedium processing technology through orthogonal experiments, has clear preparation technological parameters, small error and strong repeatability, and can effectively promote the industrial production of processed epimedium.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine preparation, in particular to a preparation method for processing epimedium.
Background
The Epimedium is derived from dried leaves of Epimedium brevicomum maxim, Epimedium sagittatum (Sieb. et Zucc.) Maxim, Epimedium pubescens Maxim or Epimedium koreanum Nakai of berberidaceae, and alcohol extract and total flavone of the dried leaves have obvious pharmacological activity. Modern pharmacological studies show that the epimedium alcohol extract has the effects of oxidation resistance and neuroprotection; herba Epimedii total flavone has effects of resisting osteoporosis, resisting oxidation, enhancing immunity, protecting nerve, resisting aging and protecting kidney.
Researches show that the main active ingredient of epimedium is flavonoid, wherein the contents of epimedin A-C, icariin and baohuoside I are higher, and epimedin A has antibacterial and antioxidant activities; the epimedin B has anti-osteoporosis, antibacterial and antioxidant activities; the epimedin C has the activities of resisting osteoporosis, oxidation, bacteria and tumors; icariin has effects of resisting osteoporosis, protecting nerve, resisting tumor, resisting inflammation and resisting oxidation; baohuoside I has anti-tumor, anti-osteoporosis, blood sugar lowering and antioxidant activities.
The factors influencing the content of the effective components of the epimedium herb are more, and comprise varieties, habitat of the producing area, harvesting time, storage methods, producing area processing methods, processing methods and the like, wherein the epimedium herb is processed after harvesting, and different processing methods have different influences on the chemical component content of the epimedium herb. The processing method of epimedium is described in leigong treatise on processing, leigong yun: when the physician is to take the herb, the four flower branches at the side of the herb should be removed with a knife, and every jin should be stir-fried with two or four mutton tallow until the fat is exhausted. Until the Qing Dynasty, there are about 20 kinds of processing methods of epimedium herb recorded in the past, which relates to the ancient medicine literature, No. 40. The mutton tallow stir-frying method is used all the time, which shows that the mutton tallow stir-frying method has universality in the past, but the records of the epimedium mutton tallow stir-frying method in the past herbal medicine are general, the control of the decoction piece processing process is always based on the subjective judgment of an operator, and the stability of the quality of the decoction pieces is difficult to control. The technology of mutton fat roasted epimedium decoction pieces is only recorded in the Chinese pharmacopoeia of 2015 edition, and a large amount of documents research the technology of mutton fat roasted epimedium at present.
The auxiliary material used in the preparation method is ghee. The records of stir-baked herba Epimedii are recorded in Rui Zhu Tang Jing Yan Fang of the original generation, Pu Ji Fang of the Ming Dynasty and Liang Ming Hui of the Qing Dynasty. Butter is the essence of Tibetan food, is a dairy product like butter, and is fat extracted from cow milk and goat milk. Ghee can increase digestion and absorption capacity in the body, lubricate connective tissue, increase mobility, improve brain function and memory, and transport the medicinal properties of herbs into tissues throughout the body. In addition, ghee has removed all the milk proteins during milk extraction, and therefore, it is an excellent substitute milk for lactose intolerant people. The processing specification of traditional Chinese medicine in Gansu province is also recorded in shortbread of herba Epimedii, and the preparation method comprises taking the shortbread, heating and melting with slow fire in a pot, pouring herba Epimedii shreds, stir-frying uniformly, taking out, spreading out, and cooling. Every 100kg of epimedium uses 25kg of butter, but no specific parameters of temperature and stir-frying time exist, the invention embodies the epimedium stir-frying process and preferably selects a method for processing the epimedium.
Disclosure of Invention
The invention aims to provide a preparation method for processing epimedium aiming at the defects in the prior art; aims to determine each index weight coefficient by using icariin content, total flavone content, 5 main flavone (epimedin A-C, icariin and baohuoside I, 5 flavones) content, alcohol extract content and DPPH free radical scavenging activity as indexes on the basis of heart-leaf epimedium (hereinafter abbreviated as epimedium), and adopting an analytic hierarchy process-index correlation-based weight determination method (AHP-CRITIC) mixed weighting method, and optimally selecting an epimedium processing process through orthogonal experimental design so as to provide theoretical basis for industrial production of roasted epimedium.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a method for preparing processed herba Epimedii comprises adding herba Epimedii into butter and parching; the addition amount of the butter is 10 to 20 percent of the weight percentage of the epimedium herb, the frying temperature is 140 to 180 ℃, and the frying time is 4 to 8 minutes; the herba Epimedii is herba Epimedii.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 10 percent by weight of the medicinal material of the epimedium herb, the frying temperature is 140 ℃, and the frying time is 4 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 10 percent by weight of the medicinal material of the epimedium herb, the frying temperature is 160 ℃, and the frying time is 6 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 10 percent by weight of the medicinal material of the epimedium herb, the frying temperature is 180 ℃, and the frying time is 8 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 15 percent of the weight percentage of the medicinal material of the epimedium herb, the frying temperature is 140 ℃, and the frying time is 6 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 15 percent by weight of the medicinal material of the epimedium herb, the frying temperature is 160 ℃, and the frying time is 8 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 15 percent of the weight percentage of the medicinal material of the epimedium herb, the frying temperature is 180 ℃, and the frying time is 4 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 20 percent of the weight percentage of the medicinal material of the epimedium herb, the frying temperature is 140 ℃, and the frying time is 8 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 20 percent of the weight percentage of the medicinal material of the epimedium herb, the frying temperature is 160 ℃, and the frying time is 4 minutes.
Further, in the preparation method of the processed epimedium herb, the addition amount of the ghee is 20 percent of the weight percentage of the medicinal material of the epimedium herb, the frying temperature is 180 ℃, and the frying time is 6 minutes.
The invention has the beneficial effects that: the invention provides a preparation method of processed epimedium, which integrates various data indexes such as icariin content, total flavone content, 5 main flavone content, alcohol extract content, DPPH free radical scavenging activity and the like, designs and optimizes an optimal processing process of the epimedium through orthogonal experiments, has the advantages of cleaning preparation process parameters, small error and strong repeatability, and can effectively promote the industrial production of the processed epimedium.
Detailed Description
Example 1:
1 reagents, instruments and medicinal materials
1.1 reagents
Epimedin A (110623-72-8), epimedin B (110623-73-9), epimedin C (110642-44-9), icariin (489-32-7) and baohuoside I (113558-15-9) reference substances are all purchased from Chenguan Biotechnology GmbH of Baoji city; methanol, acetonitrile (Oceanpak, sweden), acetonitrile and acetic acid are chromatographically pure; other reagents were analytically pure.
1.2 instruments
One-tenth-ten-thousandth analytical balance (sidoris scientific instruments, beijing ltd); agilent 1260 II high performance liquid chromatograph; an ultrasonic cleaning instrument (KQ-400KDE type high power numerical control ultrasonic cleaning instrument); ultraviolet spectrophotometer (UV-1700, Shimadzu); FA2004 analytical electronic balance (shanghai lianghua instruments ltd).
1.3 herbs
The epimedium medicinal material is collected from the dam village in the gift county of Gansu province, and the collection time is as follows: 6.10.2019, provided by the spring pharmaceutical industry in Li county, and identified as the leaf of Epimedium brevicomu Maxim by pharmacist in Yangtze cang, a hospital affiliated to the university of traditional Chinese medicine in Gansu.
2 methods and results
2.1 content and determination of five flavones
HPLC method is adopted to determine the content of 5 kinds of flavone according to the determination method of icariin and baohuoside I content in roasted epimedium herb under the item of epimedium herb in 2015 edition of Chinese pharmacopoeia.
2.1.1 sample preparation
Preparing a sample solution according to the rules of pharmacopoeia.
Weighing 0.2g of medicinal materials, precisely weighing, placing in a conical flask with a plug, precisely adding 20mL of dilute ethanol, weighing, ultrasonically extracting (20 ℃, frequency 160HZ) for 1 hour, cooling, weighing again, supplementing the lost weight with dilute ethanol, shaking, filtering, taking the subsequent filtrate, and filtering with 0.45 μ L of filter membrane to obtain the final product.
2.1.2 chromatographic conditions
A chromatographic column: an Agilent ZORBAX Eclipse XDB-C18 column;
column temperature: 30 ℃;
sample introduction amount: 20 mu L of the solution;
detection wavelength: 270 nm;
mobile phase: acetonitrile-water
The elution procedure is shown in table 1.
TABLE 1
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0～29 | 75 | 25 |
| 29～30 | 75～59 | 25～41 |
| 30～55 | 59 | 41 |
2.1.3 assay
Accurately weighing appropriate amount of reference substances of epimedin A, epimedin B, epimedin C, icariin and baohuoside I, respectively adding methanol to dissolve and fix the volume to 5mL volumetric flasks, respectively sucking 200 μ L, placing in 1mL volumetric flasks, mixing uniformly to obtain mixed reference substance solutions containing A, B, C of epimedin, 0.59, 0.54, 0.50 and 0.52mg/mL of icariin and baohuoside I, respectively, diluting into a series of mixed reference substance solutions, respectively injecting the series of reference substance solutions into a liquid chromatograph with 20 μ L, and respectively drawing standard curves according to peak areas. Injecting 10 μ L sample solution into high performance liquid chromatograph, and measuring flavone content according to each standard curve.
2.2 measurement of Total Flavonoids content
The total flavonoids are determined according to a determination method under the item of epimedium herb in 'Chinese pharmacopoeia' of 2015 edition.
2.2.1 sample preparation
The same as "2.1.1".
2.2.2 preparation of control solutions
Collecting icariin 2.50mg as control, adding methanol to obtain solution containing 0.50mg per mL to obtain control solution. Respectively taking 0, 100, 200, 300, 400 and 500 mu L of reference substance stock solution, placing in a 10mL volumetric flask, adding methanol to constant volume to scale to obtain standard substance series solution.
2.2.3 drawing of Standard Curve
Measuring absorbance A of the serial reference substance solutions at 270nm with zero blank solvent, measuring for three times, averaging, and drawing standard curve with icariin reference substance concentration as abscissa and absorbance as ordinate.
2.2.4 measurement of content
Precisely sucking 50 mu L of the test solution, placing the test solution in a 5mL volumetric flask, adding methanol to a constant volume to a scale, and uniformly mixing. And (5) measuring the light absorption value A, paralleling the three parts, and calculating the content of the total flavone according to the light absorption value A.
2.3 determination of alcohol extract content
The measurement is carried out according to the measurement method under the item of alcohol leaching matters in the fourth part of China pharmacopoeia 2015 edition.
2.4 DPPH radical scavenging Rate determination
The extraction method comprises the following steps: the same as "2.1.1".
The determination method comprises the following steps: the 20mgDPPH and absolute ethyl alcohol are dissolved in a 250mL volumetric flask to obtain DPPH stock solution. Diluting the sample solution by 10 times and taking 1 mL; add 1mLDPPH stock solution. Mixing, reacting in dark for 30min, and measuring absorbance A at 517nmSample (I)Using absolute ethyl alcohol to substitute sample solution to measure blank group light absorption value ABlank space。
Clearance rate ═ aBlank space-ASample (I))/ABlank space×100％
2.5 orthogonal Experimental design
By combining factors influencing the herba epimedii processing process, selecting ghee adding amount% (A), frying temperature (B) and frying time (C) as investigation factors, and designing three-factor three-level orthogonal experiments by taking icariin content, total flavone content, 5 flavone content sum, alcohol extract content and DPPH free radical scavenging activity as indexes, wherein the factor level is shown in table 2, and the orthogonal experiment design and results are shown in table 3.
TABLE 2
TABLE 3
2.6 determination of the weights of the indices
2.6.1 AHP method for determining weights
According to the active ingredient investigation of epimedium, the icariin content, the total flavone content, the 5 flavone contents, the alcohol extract content and the DPPH free radical clearance rate are selected as weight indexes and quantified, the evaluation indexes are divided into 5 levels, and the priority of each index is determined as follows: the icariin total flavone content is greater than 5 flavone contents, the alcohol extract content is greater than DPPH free radical clearance rate, a pairwise comparison priority judgment matrix is constructed, each index is endowed with relative scores, and the pairwise comparison priority judgment matrix is shown in table 4.
TABLE 4
According to the scoring results in table 4, the icariin content, the total flavone content, the 5 flavone content, the alcohol extract content and the DPPH free radical clearance weight coefficients are calculated by an analytic hierarchy process as 0.4241, 0.2436, 0.1414, 0.1060 and 0.0848, the maximum characteristic value CI is calculated as 0.0423, the random consistency row scaling factor RI is found as 0.9, the consistency ratio CR is found as 0.01 as 0.1, and the two-by-two comparison shows that the matrix consistency is good, and the obtained weight coefficients are reasonable and effective.
2.6.2 CRITIC method for determining weights
The CRITIC method (criterion impact Through intercritical Correlation) is an objective weighting method proposed by Diakoulaki, and comprehensively measures the objective weight of an evaluation index on the basis of the contrast strength between certain characteristic classes and the conflict between the characteristics, and the CRITIC method is adopted in the experiment to determine the weight between the indexes. Carrying out linear interpolation on data for standardization, wherein index component values are [ (measured value-minimum value)/(maximum value-minimum value) ] × 100, eliminating unit dimensions, then processing the data according to SPSS 22.0 software to obtain a correlation coefficient matrix A, calculating contrast strength (si), conflict (i), comprehensive weight (Ci) and weight coefficient (omega i) among all indexes by adopting SPSS 22.0 software, and calculating objective weight coefficients of icariin content, total flavone content, 5 flavone content sum, alcohol extract content and DPPH free radical clearance rate by a CRITIC method to obtain 0.1770, 0.2841, 0.1384, 0.2714 and 0.1291 respectively.
2.6.3 AHP-CRITIC mixed weighting method for determining index weight
The AHP method quantifies the strength information of pharmacological action between every two indexes to a certain extent, obtains a weight coefficient based on subjective evaluation, but has strong subjectivity and ignores the information of actual sample data, namely the influence of interaction between the indexes on the overall sampling effect. The CRITIC method can embody objective data information, but often neglects the actual weight relationship among indexes, and has poor discrimination of samples. The AHP-CRITIC mixed weighting method combines the advantages of the AHP method and the CRITIC method, and the comprehensive weight is calculated by combining the AHP method and the CRITIC method, so that the subjective and objective effects are considered, and the data information can be comprehensively and objectively evaluated. The AHP-CRITIC mixed weight calculation formula is as follows:
(ω Integrated ij) ═ ω AHPij ω CRITICij/∑ ω AHPij ω CRITICij
The compound weight coefficients of five indexes of icariin content, total flavone content, 5 flavone content, alcohol extract content and DPPH free radical clearance rate calculated according to a formula are 0.3687, 0.3399, 0.0961, 0.1413 and 0.0538 respectively.
2.7 comparison of the results of the comprehensive evaluation
The experimental results are comprehensively scored by using the weighting coefficients obtained by analysis of an AHP method, a CRITIC method and an AHP-CRITIC mixed weighting method, and the comprehensive scoring results of the three weighting methods are shown in Table 5. The results of the 3 scoring methods are visually analyzed to be small in difference, through correlation coefficient analysis, the correlation coefficient between the AHP method and the CRITIC method is 0.9941, the correlation coefficient between the AHP method and the mixed weighting method is 0.9977, the correlation coefficient between the CRITIC method and the mixed weighting method is 0.9929, the correlation of the three methods is obvious (P <0.05), and the scoring results obtained by the 3 weighting methods are consistent. From the weight coefficient analysis, the correlation coefficient between the AHP method and the CRITIC method is 0.0877, the correlation between the AHP method and the CRITIC method is not significant (P >0.05), and the reflected information has no superposition. In a comprehensive way, the AHP-CRITIC mixed weighting method carries out comprehensive evaluation from 2 aspects of subjectivity and objectivity, the embodied information amount is more comprehensive, and therefore the comprehensive evaluation result is more scientific and reasonable.
TABLE 5
2.8 determination of processing technology
The visual analysis result shows that the influence sequence of all factors on the epimedium processing technology is A>C>B, i.e. the amount of shortening added>Frying time>And (5) frying. Analysis of variance showed that A, B, C factors all had no significant difference (p >0.05) in the processing technique. The preferred optimal processing technology is as follows: a. the1B1C1Adding crisp oil 10%, parching at 140 deg.C for 4min is the same as the formula (I). The results of the visual analysis are shown in Table 6 and the results of the analysis of variance are shown in Table 7.
TABLE 6
TABLE 7
| Origin of origin | Sum of squares | df | Mean square | F | Significance of |
| A | 82.128 | 2 | 41.064 | 15.122 | 0.179 |
| B | 98.003 | 2 | 49.001 | 18.045 | 0.164 |
| C | 15.187 | 2 | 7.594 | 2.796 | 0.389 |
| Error of the measurement | 2.716 | 2 | 2.716 |
2.9 comparison of the clearance rates of the ingredients in Epimedium herb processed with butter and mutton fat and DPPH free radical
The research shows that when the addition amount of the ghee is 10 percent, the content of the effective components is the highest, and the DPPH free radical clearance rate is the strongest. The addition of mutton fat in the mutton fat-fried epimedium herb is 20% recorded in Chinese pharmacopoeia, the experiment design compares the mutton fat and the butter-fried epimedium herb with the same proportion (10%, 140 ℃, 4min), the preparation samples S10 and S11 are compared with the raw decoction pieces S12 of the epimedium herb respectively. The results are shown in table 8, and the results prove that compared with the raw epimedium decoction pieces, the active ingredient content of 10% of the epimedium fried with mutton fat and ghee is higher, and the DPPH free radical clearance rate is higher. The ghee-fried epimedium has higher content of effective components and stronger DPPH free radical clearance than the ghee-fried sample, and is a good choice for being more easily accepted by consumers in order to find that the ghee-fried epimedium has special fragrance and the sheepskin-fried epimedium has the sheepy odor in the processing process.
TABLE 8
2.9 comparison of Epimedium decoction pieces prepared by adding adeps Caprae Seu Ovis at different ratios
In order to verify whether the conclusion is suitable for the epimedium fried with mutton tallow or not, the experiment designs that samples S13, S14 and S15 are prepared by adopting optimal temperature and time (140 ℃ and 4nin) under different addition amounts of mutton tallow (10%, 15% and 20%), and the contents of the icariin, the total flavone and the 5 flavones, the content of the alcohol extract and the DPPH free radical removal rate are determined, and data prove that when the addition amount of the mutton tallow is 10%, the contents of the icariin, the total flavone and the 5 flavones, the contents of the alcohol extract and the DPPH free radical removal rate are all highest, and the DPPH free radical removal rate is strongest. The results are shown in Table 9.
TABLE 9
3 small knot
The invention aims to design an orthogonal test and a preferable processing technology based on epimedium herb and by taking icariin, total flavone, 5 flavone contents, alcohol extract content and DPPH free radical clearance as indexes. The establishment of the weight coefficient is always the problem that the multi-index evaluation in the traditional Chinese medicine processing process needs to be considered, the current commonly used method comprises a subjective comprehensive evaluation method, a total evaluation normalization method, an AHP analytic hierarchy process and a CRITIC method, the AHP analytic hierarchy process provided by the experiment of the invention is easily influenced by the subjective judgment of experimenters, the information of actual sample data can be neglected sometimes in the presence of one-sidedness, the CRITIC method objectively utilizes the data information but often neglects the light relation among indexes, particularly the traditional Chinese medicine with complex components, the AHP-CRITIC mixed weighting method combines the advantages of different types of weighting methods, not only emphasizes subjectivity, but also does not lose objectivity, can distinguish sample data more than a single weighting method, the embodied data information is more comprehensive, the uniform dispersion of data points is ensured, the result is stable and reliable, the process preferred by the experiment of the invention is that the crisp oil adding amount is 10%, the frying temperature is 140 ℃, the stir-frying time is 4min, the processing method is simple and controllable, and theoretical basis can be provided for industrial production of roasted epimedium herb.
The comparative data of the operation process and the final product effect of the epimedium processing method provided by the invention and the epimedium processing method in the prior art are shown in the table 10.
Watch 10
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that changes may be made in the embodiments and/or equivalents thereof without departing from the spirit and scope of the invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method for processing epimedium is characterized in that epimedium medicinal materials are added with butter and fried; the addition amount of the butter is 10 to 20 percent of the weight percentage of the epimedium herb, the frying temperature is 140 to 180 ℃, and the frying time is 4 to 8 minutes; the herba Epimedii is herba Epimedii.
2. The method for preparing the processed epimedium herb according to claim 1, wherein the butter is added in an amount of 10 percent by weight of the epimedium herb, the frying temperature is 140 ℃, and the frying time is 4 minutes.
3. The method for preparing processed epimedium herb according to claim 1, wherein the butter is added in an amount of 10 percent by weight of epimedium herb, the frying temperature is 160 ℃, and the frying time is 6 minutes.
4. The method for preparing processed epimedium herb according to claim 1, wherein the butter is added in an amount of 10% by weight of epimedium herb, the frying temperature is 180 ℃, and the frying time is 8 minutes.
5. The method for preparing the processed epimedium herb according to claim 1, wherein the butter is added in an amount of 15 percent by weight of the epimedium herb, the frying temperature is 140 ℃, and the frying time is 6 minutes.
6. The method for preparing processed epimedium herb according to claim 1, wherein the butter is added in an amount of 15 percent by weight of epimedium herb, the frying temperature is 160 ℃, and the frying time is 8 minutes.
7. The method for preparing processed epimedium herb according to claim 1, wherein the butter is added in an amount of 15 percent by weight of epimedium herb, the frying temperature is 180 ℃, and the frying time is 4 minutes.
8. The method for preparing the processed epimedium herb according to claim 1, wherein the butter is added in an amount of 20 percent by weight of the epimedium herb, the frying temperature is 140 ℃, and the frying time is 8 minutes.
9. The method for preparing processed epimedium herb according to claim 1, wherein the butter is added in an amount of 20% by weight of epimedium herb, the frying temperature is 160 ℃, and the frying time is 4 minutes.
10. The method for preparing processed epimedium herb according to claim 1, wherein the butter is added in an amount of 20% by weight of epimedium herb, the frying temperature is 180 ℃, and the frying time is 6 minutes.
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| CN114767726A (en) * | 2022-05-19 | 2022-07-22 | 重庆迈德凯医药有限公司 | Processing method for improving content of major components of epimedium wushanense |
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| CN111557963A (en) * | 2020-06-05 | 2020-08-21 | 天津中医药大学 | Processing method of herba epimedii and mutton tallow oil for processing herba epimedii |
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