CN110496155B - Processing method of rhizoma polygoni cuspidati processed with ginger and quality detection method of processed product of rhizoma polygoni cuspidati processed with ginger - Google Patents
Processing method of rhizoma polygoni cuspidati processed with ginger and quality detection method of processed product of rhizoma polygoni cuspidati processed with ginger Download PDFInfo
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Abstract
The invention discloses a processing method of ginger processed giant knotweed and a quality detection method of a processed product thereof, comprising the following steps: taking a giant knotweed medicinal material, adding ginger juice accounting for 16-17% of the weight of the giant knotweed, moistening for 50min, and frying at 230-240 ℃ for 10-11 min to obtain the giant knotweed tea. According to the invention, the optimal processing method of the ginger processed giant knotweed rhizome is screened out by comparing and screening different processing technologies in a large quantity, so that the content of effective components can be improved. The quality detection method for the rhizoma polygoni cuspidati processed product prepared by ginger is screened out by a large number of inventions, particularly, the optimum analysis conditions such as mobile phase composition, flow rate, detection wavelength, chromatographic column, column temperature and the like are screened out by a large number of inventions, and shown by methodological verification, the quality detection method for the rhizoma polygoni cuspidati prepared by ginger has the advantages of simple method, good stability, high precision, good reproducibility and the like.
Description
Technical Field
The invention relates to a processing method of traditional Chinese medicines, in particular to a processing method of ginger processed giant knotweed and a quality detection method of a processed product thereof.
Background
Polygonum cuspidatum cuspidoum Sieb. et Zucc. is dried root and rhizome parts of Polygonum plant PolgohumL of Polygonum of Polygonaceae. There are many documents on the efficacy of giant knotweed, the "herb property treatise" is recorded with "clearing away heat and toxic material", the "Rihuazi materia Medica" is recorded with "promoting blood circulation and removing obstruction in channels", the "research of invention of traditional Chinese medicine" is recorded with "dispelling wind and promoting diuresis", and the "blood stasis removing and pain relieving" is recorded in the "folk prescription medicine Collection of Guizhou province". In famous medical records of Han dynasty, ancestors have recorded that giant knotweed rhizome is used as a medicine, which is the record of the initial giant knotweed rhizome in China for medical purposes. The book of Qianjin winged Fang is the medical great book recorded in the earliest time in China for the processing of Polygonum cuspidatum. In medical books of all ages, many records about the processing technology of giant knotweed rhizome are recorded, but the processing technology of giant knotweed rhizome is mainly washed, filed and dried, even since the country is built, the processing method of giant knotweed rhizome in pharmacopoeia of the people's republic of China and the specifications of provinces and cities basically mainly comprises soaking, slicing and drying, and the processing method of giant knotweed rhizome is rarely related to the co-preparation with auxiliary materials although the processing method is developed and changed, and is single. The study on the wine-processed giant knotweed rhizome, the vinegar-processed giant knotweed rhizome and the salt-processed giant knotweed rhizome in Zhangi et al and the study result on the bean juice-processed giant knotweed rhizome in Li Benjun et al show that the processing technology of the giant knotweed rhizome can not be limited to the single treatment in the past, and the content of the effective components in the giant knotweed rhizome can be changed by co-processing with different auxiliary materials, so that the giant knotweed rhizome is more suitable for clinical application. Processed with ginger can inhibit the bitter and cold property of rhizoma Polygoni Cuspidati, reduce the damage to spleen yin, and enhance the curative effect of the medicine.
In the process of optimizing the rhizoma polygoni cuspidati ginger roasting process, the influence of three factors of the ginger juice dosage, the roasting temperature and the roasting time on the quality of the rhizoma polygoni cuspidati needs to be investigated, the roasting process is optimized according to the investigation result, and the interaction among the three factors cannot be measured by adopting a single-factor investigation method with fixed variables. The uniform design and the orthogonal invention design can indicate the value direction of a certain factor, but the design method adopts a linear model, when the two optimization methods enter a preferred area, namely an area near the optimal process, the linear fitting may have limitation, and the relevance of the fitting of the curved effect surface model of the preferred area is reduced. At this time, the central composite design-response surface method (RSM-CCD) shows the advantage of the method in dealing with nonlinear model fitting, and the degree of correlation of the method to the response surface model with the bending of the preferred region is better.
Polydatin, resveratrol and emodin are effective components of rhizoma Polygoni Cuspidati, wherein polydatin and emodin are detection indexes under content determination item of current version pharmacopoeia, and resveratrol can be converted with polydatin in vivo to keep balance. One of the effective components of the giant knotweed rhizome for promoting blood circulation, removing obstruction in channels, dissipating blood stasis and relieving pain is polydatin and resveratrol which play an important role in regulating a blood system and protecting a nervous system. Therefore, the research of the invention adopts polydatin, resveratrol and emodin as investigation indexes.
Disclosure of Invention
The purpose of the invention is as follows: the invention aims to solve the defects of the prior art and provides a processing method of rhizoma polygoni cuspidati with ginger, which is reasonable in processing technology and stable in processing technology, and particularly can improve the effective components of polydatin, resveratrol and emodin. The invention also aims to provide a quality detection method of the processed ginger giant knotweed rhizome product. The detection method can objectively and accurately evaluate the quality of the rhizoma polygoni cuspidati processed by ginger and the processed products thereof, and has important significance for ensuring the clinical curative effect.
The technical scheme is as follows: in order to achieve the purpose, the invention adopts the technical scheme that:
a processing method of rhizoma Polygoni Cuspidati processed with ginger comprises the following steps:
taking a giant knotweed medicinal material, adding water to dilute ginger juice, uniformly scattering the diluted ginger juice into the giant knotweed medicinal material, moistening, frying and cooling to obtain the giant knotweed medicinal material.
Preferably, the processing method of rhizoma polygoni cuspidati processed with ginger is characterized by comprising the following steps: taking a giant knotweed medicinal material, adding ginger juice accounting for 16-17% of the weight of the giant knotweed, moistening for 50min, and frying at 230-240 ℃ for 10-11 min.
Preferably, the processing method of rhizoma polygoni cuspidati processed with ginger is characterized by comprising the following steps: mixing rhizoma Polygoni Cuspidati with 16.602% succus Zingiberis recens, moistening for 50min, and parching at 238.810 deg.C for 10.863 min.
The quality detection method of the processed product of the ginger processed giant knotweed rhizome comprises the following steps:
(1) preparation of control solutions
Adding 1.14mg of resveratrol which is precisely weighed into a 5mL volumetric flask, adding methanol to dissolve and dilute to a scale mark, and preparing a resveratrol reference product mother solution of 0.228 mg/mL;
adding 10.26mg of polydatin precisely weighed into a 5mL volumetric flask, adding methanol to dissolve and dilute to scale marks, and preparing 2.052mg/mL polydatin reference product mother liquor;
adding 1.95mg of accurately weighed emodin into a 10mL volumetric flask, adding methanol to dissolve and dilute to a scale mark, and preparing 0.195mg/mL emodin reference mother liquor;
precisely measuring 4mL of resveratrol reference product mother liquor, 4mL of polydatin reference product mother liquor and 8mL of emodin reference product mother liquor, and mixing to obtain mixed reference product mother liquor containing 0.057mg/mL of resveratrol, 0.513mg/mL of polydatin and 0.098mg/mL of emodin respectively;
(2) preparation of test solution
Adding precisely weighed dried rhizoma Polygoni Cuspidati powder 0.1g sieved with 65 mesh sieve into conical flask with plug, precisely adding methanol 20mL, weighing, performing ultrasonic treatment at 24 deg.C with 100W power for 30min, refluxing in 79 deg.C water bath for 20min, weighing again, if the weight is reduced, adding methanol, shaking, filtering, and collecting filtrate;
(3) preparation of the Standard Curve
Taking the mixed standard reference substance mother liquor in the step (1), respectively precisely transferring 4mL, 3mL, 2mL, 1mL and 0.5mL into 5mL volumetric flasks, diluting with methanol to scale marks, shaking up, preparing into a series of mixed standard reference substance solutions with concentration, respectively injecting 10 mu L of sample, analyzing by HPLC, and drawing a standard curve by taking the peak area as the ordinate and the concentration as the abscissa;
(4) determination of content
And (3) taking 10 mu L of the rhizoma polygoni cuspidati test solution prepared from the ginger in the step (2), injecting into a high performance liquid chromatograph for analysis, and calculating the content of resveratrol, polydatin and emodin in the test solution according to the linear regression equation prepared in the step (3).
Preferably, in the method for detecting the quality of the processed ginger processed giant knotweed rhizome, the chromatographic conditions of the high performance liquid chromatograph in the steps (3) and (4) are as follows:
a chromatographic column: purospher STAR LP RP-18endcapped, 4.6 × 250mm, 5 μm; mobile phase: pure water is phase A-acetonitrile is phase B, and gradient elution is carried out; the flow rate is 0.6mL min < -1 >; the detection wavelength is 306nm, and the column temperature is 40 ℃.
Preferably, in the quality detection method of the poria cocos, cassia twig and rhizoma atractylodis decoction, the gradient elution condition is 0-15 min, and B% is 5% → 25%; 15-51 min: b% 25% → 37%; 51-75 min: b% is 37% → 85%.
Preferably, in the method for detecting the quality of the processed product of rhizoma polygoni cuspidati processed with ginger, the linear regression equation of the polydatin prepared in step (3) is y ═ 2E +07x-319.3, and R is20.9999; the linear regression equation of resveratrol is 1E +08x-19725, R20.9998; the linear regression equation of emodin is that y is 3E +07x +102440, R2＝0.9993。
The screening of the processing technology is as follows:
one, one factor investigation
1. Dosage factor of ginger juice
1.1 preparation of ginger juice
Taking 100g of ginger, slicing, juicing by using a juicer, adding water into residues, juicing again, and combining ginger juice to prepare 1g/mL ginger juice. 1.2 examination of the amount of ginger juice
Taking 100g of rhizoma Polygoni Cuspidati 3 parts, respectively taking 5mL, 10mL and 20mL of succus Zingiberis recens, diluting with water to 40mL, uniformly spreading in rhizoma Polygoni Cuspidati, moistening for 50min, and parching at 220 deg.C for 10 min. Taking rhizoma Polygoni Cuspidati processed with different ginger juice dosages, precisely adding methanol, weighing, performing ultrasonic treatment at 24 deg.C water temperature for 30min with 100W power, refluxing in 79 deg.C water bath for 20min, weighing again, if the weight is reduced, adding methanol to complement, shaking, filtering to obtain sample solution, then respectively injecting 10 μ L of sample under the chromatographic conditions of the above steps (3) and (4) to HPLC for analysis, and respectively calculating polydatin, resveratrol and emodin contents according to the standard curves of resveratrol, polydatin and emodin, the results are shown in Table 1.
TABLE 1 consideration table of dosage factor of ginger juice
| The amount of ginger juice/%) | Polydatin/mg g-1 | Resveratrol/mg g-1 | Emodin/mg g-1 |
| 5 | 31.792 | 2.751 | 5.341 |
| 10 | 35.855 | 3.914 | 9.561 |
| 20 | 35.261 | 3.484 | 7.695 |
The rhizoma Polygoni Cuspidati is processed with 10 times of rhizoma Zingiberis recens juice, and has high content of polydatin, resveratrol and emodin.
1.3 frying temperature factor
Collecting rhizoma Polygoni Cuspidati 100g by 3 parts, collecting 10mL succus Zingiberis recens, diluting with water to 40mL, spreading into rhizoma Polygoni Cuspidati uniformly, moistening for 50min, and parching at 140 deg.C, 220 deg.C and 300 deg.C for 10 min. Precisely adding methanol into rhizoma Polygoni Cuspidati at different parching temperatures, weighing, performing ultrasonic treatment at 24 deg.C with 100W power for 30min, refluxing in water bath at 79 deg.C for 20min, weighing again, if the weight is reduced, adding methanol, shaking, filtering to obtain sample solution, performing HPLC analysis by injecting 10 μ L of sample under the chromatographic conditions of steps (3) and (4), and calculating polydatin, resveratrol and emodin content according to the standard curves of resveratrol, polydatin and emodin, respectively, with the results shown in Table 2.
TABLE 2 investigation table of frying temperature factors
| Parching temperature/deg.C | Polydatin/mg g-1 | Resveratrol/mg g-1 | Emodin/mg g-1 |
| 180 | 46.159 | 4.120 | 8.347 |
| 220 | 53.032 | 5.538 | 11.168 |
| 260 | 44.617 | 4.272 | 10.663 |
Rhizoma Polygoni Cuspidati obtained by parching at 220 deg.C has high content of polydatin, resveratrol and emodin.
1.4 frying time factor
Taking 100g of rhizoma Polygoni Cuspidati 3 parts, taking 10mL of succus Zingiberis recens, diluting with water to 40mL, spreading into rhizoma Polygoni Cuspidati uniformly, moistening for 50min, parching at 220 deg.C for 5min, 10min, and 20min respectively. Accurately adding methanol into rhizoma Polygoni Cuspidati under different parching time, weighing, performing ultrasonic treatment at 24 deg.C with 100W power for 30min, refluxing in 79 deg.C water bath for 20min, weighing again, if the weight is reduced, adding methanol, shaking, filtering to obtain sample solution, performing HPLC analysis by injecting 10 μ L of sample under the chromatographic conditions of steps (3) and (4), and calculating polydatin, resveratrol and emodin content according to the standard curves of resveratrol, polydatin and emodin, respectively, with the results shown in Table 3.
TABLE 3 examination table of frying time factors
| Frying time/min | Polydatin/mg g-1 | Resveratrol/mg g-1 | Emodin/mg g-1 |
| 5 | 29.768 | 5.235 | 11.967 |
| 10 | 52.425 | 5.799 | 6.157 |
| 20 | 45.569 | 4.673 | 10.128 |
Design scheme of two, star point
1. Three factors which are key to the research on the processing technology of the ginger processed giant knotweed are determined by single factor investigation and are the dosage of ginger juice, the frying temperature and the frying time. Therefore, the three independent variables selected by the invention are respectively as follows: the processing process conditions of the giant knotweed rhizome ginger processed product are optimized by using the ginger juice dosage (A), the frying time (B) and the frying temperature (C) and using a Design method of Central Composite under the Response Surface item in Design-expert V.8.0.6.1 software, and the level of the Design factors is shown in a table 4.
TABLE 4 response surface design factor level
Note: the actual operation physical quantity is rounded according to a theoretical value
Determination of Polydatin (Y)1) Resveratrol (Y)2) Emodin (Y)3) Is the response value. When the model only has one index, the processing process route of the rhizoma polygoni cuspidati roasted by ginger can be directly optimized according to the result, but the index of the invention is polydatin (Y)1) Resveratrol (Y)2) Emodin (Y)3) The total number of the 3 indexes is 3, the 3 indexes can influence each other, so that the optimization process of one index is not necessarily the optimization process of the other two indexes, and therefore, the total score 'normalization value' (OD) is selected as the comprehensive effect of the indexes. Because the polydatin (Y) is optimized in the processing route of rhizoma Polygoni Cuspidati1) Resveratrol (Y)2) Emodin (Y)3) The larger the values of the 3 indexes are, the better, so that when the OD value is calculated by using the Hassan method, d is adoptedmax＝(yi-ymin)/(ymax-ymin) And calculating the OD value. The results are shown in Table 5.
TABLE 5 inventive designs and results
2. Data analysis and model fitting
Adopting Design-ExpertV.8.0.6.1 software to treat selected polydatin (Y)1) Resveratrol (Y)2) Emodin (Y)3) And performing multiple linear regression and quadratic polynomial fitting on the three factors and the total evaluation OD value. Polydatin (Y)1) The multiple linear regression equation is: y is1＝-2.60A-0.1954B-1.27C+45.97,R20.1046; the second order polynomial equation is: y is1＝-2.60A-0.1954B-1.27C+2.60AB-4.70AC-0.2555BC-5.40A2-4.37B2-1.61C2+53.97,R20.9178. From this, polydatin (Y) is known1) The nonlinear fitting result of (2) is better than the linear fitting result, the R of quadratic polynomial fitting2The value is greatly improved. Resveratrol (Y)2) The multiple linear regression equation is: y is2＝0.6343A+0.2124B+0.0261C+4.86,R20.3514; the second order polynomial equation is: y is2＝0.6343A+0.2124B+0.0261C+0.1678AB+0.2229AC-0.1156BC-0.4218A2-0.0413B2-0.3127C2+5.41,R20.6112. From this, resveratrol (Y) was found2) The nonlinear fitting result of (2) is better than the linear fitting result, the R of quadratic polynomial fitting2The value is greatly improved. Emodin (Y)3) The multiple linear regression equation is: y is3＝1.57A+1.54B-0.6633C+12.29,R20.4049; the second order polynomial equation is: y is3＝1.57A+1.54B-0.6633C+0.9489AB-0.2256AC+0.4424BC-1.76A2-0.0555B2+0.7030C2+13.07,R20.7978. Thus, emodin (Y) can be seen3) The nonlinear fitting result of (2) is better than the linear fitting result, the R of quadratic polynomial fitting2The value is greatly improved.
The multiple linear regression equation of the total evaluation OD value is as follows: y is(OD)＝0.0659A+0.0733B-0.0613C+0.4671,R20.1575; the second order polynomial equation is: y is(OD)＝0.0659A+0.0733B-0.0613C+0.0545AB-0.0460AC+0.0222BC-0.2021A2-0.0771B2-0.0397C2+0.6904,R20.7691. Therefore, the nonlinear fitting result of the total evaluation OD value is better than the linear fitting result, and the R of quadratic polynomial fitting is better than the linear fitting result2The value is greatly improved. Because the total OD value is resveratrol (Y)1) Polydatin (Y)2) Emodin (Y)3) The second-order polynomial fitting result of the total evaluation OD value is better, so that the second-order polynomial of the total evaluation OD value is determined to be a final mathematical model. The results of the analysis of variance of the quadratic regression model of the total OD values are shown in Table 6.
TABLE 6 analysis of variance of quadratic regression model for OD values
Note: p < 0.05 shows that the factor has significance
3. Analysis of effect surface
The method adopts three factors of ginger juice consumption (A), frying time (B) and frying temperature (C) as independent variables, and the contour map and the three-dimensional map can only measure the influence of two factors on the total evaluation OD value of the comprehensive index, so that one factor of the ginger juice consumption (A), the frying time (B) and the frying temperature (C) is respectively fixed as the median value of the three-dimensional map, the contour map and the three-dimensional map of the dependent variable effect surface are drawn for the other two factors by using software, and the interaction among the factors and the influence of the factors on the total evaluation OD value of the comprehensive index are examined.
The contour diagrams can visually show the interactive influence of three factors, namely the ginger juice dosage (A), the frying temperature (B) and the frying time (C), the contour diagrams of the influence of all the factors on the OD value are approximate to an ellipse, and the interaction effect of the three factors is obvious. On the basis of the finally determined mathematical model, the processing technology of the polygonum cuspidatum roasted with ginger is optimally designed through Design-expert V.8.0.6.1 software, and the finally obtained processing technology of the polygonum cuspidatum roasted with ginger is 16.602% of the dosage of ginger juice, 238.810 ℃ of frying temperature and 10.863min of frying time. Under the ginger processing conditions, the giant knotweed theoretically contains polydatin 53.184mg g < -1 >, resveratrol 5.432mg g < -1 >, emodin 15.169mg g < -1 >, and the total OD value is 0.743. Based on controllability of parching temperature and parching time, the optimal process can be adjusted to 17% of ginger juice, parching temperature of 240 deg.C, and parching time of 11 min.
Has the advantages that:
1. according to the invention, different processing technologies are screened by comparing a large number of different processing technologies, and the optimal processing method for screening the ginger processed giant knotweed rhizome can improve the contents of the effective components such as resveratrol, polydatin, emodin and the like.
2. In addition, the quality detection method for screening the processed rhizoma polygoni cuspidati products prepared from ginger is provided by a large number of inventions, particularly, the optimal analysis conditions such as mobile phase composition, flow rate, detection wavelength, chromatographic column, column temperature and the like are screened by a large number of inventions, and shown by methodological verification, the quality detection method for rhizoma polygoni cuspidati provided by the invention has the advantages of simple method, good stability, high precision, good reproducibility and the like.
3. The quality detection method of the processed ginger processed giant knotweed rhizome product provided by the invention can comprehensively, objectively and accurately detect and evaluate the quality of the ginger processed giant knotweed rhizome, and has important significance for ensuring the clinical curative effect of the ginger processed giant knotweed rhizome.
Drawings
FIG. 1 is a mixed standard reference HPLC chromatogram
Detailed Description
Embodiments of the present invention will be described in detail with reference to examples, in which specific conditions are not specified, according to conventional conditions or conditions recommended by manufacturers. The reagents or apparatuses are not indicated by manufacturers, and are all conventional products which can be obtained commercially.
Example 1
A processing method of rhizoma Polygoni Cuspidati processed with ginger comprises the following steps: mixing rhizoma Polygoni Cuspidati with 17% succus Zingiberis recens, moistening for 50min, and parching at 240 deg.C for 11 min.
Example 2
A processing method of rhizoma Polygoni Cuspidati processed with ginger comprises the following steps: mixing rhizoma Polygoni Cuspidati with 16.602% succus Zingiberis recens, moistening for 50min, and parching at 238.810 deg.C for 10.863 min.
Embodiment 3 a method for detecting the quality of a processed product of ginger processed giant knotweed rhizome, which comprises the following steps:
(1) preparation of control solutions
Adding 1.14mg of resveratrol which is precisely weighed into a 5mL volumetric flask, adding methanol to dissolve and dilute to a scale mark, and preparing a resveratrol reference product mother solution of 0.228 mg/mL;
adding 10.26mg of polydatin precisely weighed into a 5mL volumetric flask, adding methanol to dissolve and dilute to scale marks, and preparing 2.052mg/mL polydatin reference product mother liquor;
adding 1.95mg of accurately weighed emodin into a 10mL volumetric flask, adding methanol to dissolve and dilute to a scale mark, and preparing 0.195mg/mL emodin reference mother liquor;
precisely measuring 4mL of resveratrol reference product mother liquor, 4mL of polydatin reference product mother liquor and 8mL of emodin reference product mother liquor, and mixing to obtain mixed reference product mother liquor containing 0.057mg/mL of resveratrol, 0.513mg/mL of polydatin and 0.098mg/mL of emodin respectively;
(2) preparation of test solution
Adding precisely weighed and dried rhizoma Polygoni Cuspidati powder 0.1g obtained by processing in example 1 and example 2 and sieving with 65 mesh sieve into a conical flask with a plug, precisely adding 20mL of methanol, weighing, performing ultrasonic treatment at 24 deg.C with 100W power for 30min, performing reflux in water bath at 79 deg.C for 20min, weighing again, if the weight is reduced, adding methanol, shaking, filtering, and collecting the filtrate to obtain the sample solution of examples 1 and 2;
(3) preparation of the Standard Curve
Taking the mixed standard reference substance mother liquor in the step (1), respectively precisely transferring 4mL, 3mL, 2mL, 1mL and 0.5mL into 5mL volumetric flasks, diluting with methanol to scale marks, shaking up, preparing into a series of mixed standard reference substance solutions with concentration, respectively injecting 10 mu L of the mixed standard reference substance solutions, analyzing by HPLC, and drawing a standard curve by taking a peak area as a vertical coordinate and a concentration as a horizontal coordinate as shown in figure 1; the linear regression equation of polydatin is that y is 2E +07x-319.3, R20.9999; the linear regression equation of resveratrol is 1E +08x-19725, R20.9998; the linear regression equation of emodin is that y is 3E +07x +102440, R2＝0.9993。
(4) Determination of content
And (3) respectively injecting 10 mu L of the two rhizoma polygoni cuspidati test solution prepared from ginger in the step (2) into a high performance liquid chromatograph for analysis, and calculating the contents of polydatin 53160mg g-1, polydatin 5.428 mg-g-1 and emodin 15.129 mg-g-1 in the test solution in the example 1 according to the linear regression equation prepared in the step (3).
The content of resveratrol, polydatin and emodin in the test solution in the example 2 is calculated to contain 53.185mg g-1 of polydatin, 5.433mg g-1 of resveratrol and 15.169mg g-1 of emodin in sequence.
The chromatographic conditions of the high performance liquid chromatograph in the step (3) and the step (4) are as follows:
a chromatographic column: purospher STAR LP RP-18endcapped, 4.6 × 250mm, 5 μm; mobile phase: pure water is phase A, acetonitrile is phase B, and gradient elution is carried out (0-15 min: B% is 5% → 25%; 15-51 min: B% is 25% → 37%; 51-75 min: B% is 37% → 85%); the flow rate is 0.6mL min < -1 >; the detection wavelength is 306nm, and the column temperature is 40 ℃.
Example 4 methodology examination
1. Precision survey
Taking the rhizoma polygoni cuspidati prepared in example 1, adding 0.1g of precisely weighed and dried rhizoma polygoni cuspidati powder which is sieved by a 65-mesh sieve into a conical flask with a plug, precisely adding 20mL of methanol, weighing, carrying out ultrasonic treatment with 100W power for 30min at the water temperature of 24 ℃, carrying out water bath reflux at the temperature of 79 ℃ for 20min, weighing again, if the weight is reduced, complementing the weight with methanol, shaking up, filtering, taking a subsequent filtrate to obtain a sample solution, carrying out continuous sample injection for 6 times, and measuring the peak area according to the chromatographic conditions of example 3. The results show that the RSD of the polydatin is 1.62 percent, the RSD of the resveratrol is 2.11 percent, the RSD of the emodin is 2.37 percent, and the precision of the instrument is good.
2. Stability survey
Taking the rhizoma polygoni cuspidati prepared in example 1, adding 0.1g of precisely weighed and dried rhizoma polygoni cuspidati powder which is sieved by a 65-mesh sieve into a conical flask with a plug, precisely adding 20mL of methanol, weighing, carrying out ultrasonic treatment with 100W power for 30min at the water temperature of 24 ℃, carrying out water bath reflux at the temperature of 79 ℃ for 20min, weighing again, if the weight is reduced, complementing the weight with methanol, shaking up, filtering, taking the subsequent filtrate to obtain a sample solution, carrying out sample injection once respectively for 0, 2, 4, 6, 8, 12 and 24h, and measuring the peak areas according to the chromatographic conditions of example 3, wherein the result shows that the RSD of polydatin is 2.12%, the RSD of resveratrol is 2.22%, the RSD of emodin is 2.07%, and the sample is stable within 24 h.
3. Repeatability survey
Taking the rhizoma polygoni cuspidati prepared in example 1, adding 0.1g of precisely weighed and dried rhizoma polygoni cuspidati powder which is sieved by a 65-mesh sieve into a conical flask with a plug, precisely adding 20mL of methanol, weighing, carrying out ultrasonic treatment with 100W power for 30min at the water temperature of 24 ℃, carrying out water bath reflux at the temperature of 79 ℃ for 20min, weighing again, if the weight is reduced, complementing the weight with methanol, shaking up, filtering, and taking a subsequent filtrate to obtain a sample solution, injecting the sample solution into a high performance liquid chromatograph, and carrying out content measurement according to the chromatographic conditions in example 3, wherein the result shows that the RSD of polydatin is 1.52%, the RSD of resveratrol is 4.56%, the RSD of emodin is 3.49%, and the method has good repeatability.
4. Investigation of sample application and recovery
The sample loading recovery results show that the average sample loading recovery rates of the polydatin, the resveratrol and the emodin are 99.62%, 99.15% and 99.22% respectively, and the RSD values are 1.75%, 1.91% and 2.11% respectively, which shows high accuracy.
The results of the invention show that the quality detection method for the ginger processed giant knotweed rhizome provided by the invention has the advantages of good stability, high precision and good repeatability, can comprehensively and objectively evaluate the quality of the ginger processed giant knotweed rhizome, and has important significance for ensuring the clinical curative effect.
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.
Claims (2)
1. A quality detection method for a processed product of ginger processed giant knotweed rhizome is characterized by comprising the following steps:
(1) preparation of control solutions
Adding 1.14mg of resveratrol which is precisely weighed into a 5mL volumetric flask, adding methanol to dissolve and dilute to a scale mark, and preparing a resveratrol reference product mother solution of 0.228 mg/mL;
adding 10.26mg of polydatin precisely weighed into a 5mL volumetric flask, adding methanol to dissolve and dilute to scale marks, and preparing 2.052mg/mL polydatin reference product mother liquor;
adding 1.95mg of accurately weighed emodin into a 10mL volumetric flask, adding methanol to dissolve and dilute to a scale mark, and preparing 0.195mg/mL emodin reference mother liquor;
precisely measuring 4mL of resveratrol reference product mother liquor, 4mL of polydatin reference product mother liquor and 8mL of emodin reference product mother liquor, and mixing to obtain mixed reference product mother liquor containing 0.057mg/mL of resveratrol, 0.513mg/mL of polydatin and 0.098mg/mL of emodin respectively;
(2) preparation of test solution
Adding precisely weighed dried rhizoma Polygoni Cuspidati powder 0.1g sieved with 65 mesh sieve into conical flask with plug, precisely adding methanol 20mL, weighing, performing ultrasonic treatment at 24 deg.C with 100W power for 30min, refluxing in 79 deg.C water bath for 20min, weighing again, if the weight is reduced, adding methanol, shaking, filtering, and collecting filtrate;
(3) preparation of the Standard Curve
Taking the mixed standard reference substance mother liquor in the step (1), respectively precisely transferring 4mL, 3mL, 2mL, 1mL and 0.5mL into 5mL volumetric flasks, diluting with methanol to scale marks, shaking up, preparing into a series of mixed standard reference substance solutions with concentration, respectively injecting 10 mu L of sample, analyzing by HPLC, and drawing a standard curve by taking the peak area as the ordinate and the concentration as the abscissa;
(4) determination of content
Taking 10 mu L of the rhizoma polygoni cuspidati test sample solution prepared from ginger in the step (2), injecting the solution into a high performance liquid chromatograph for analysis, and calculating the content of resveratrol, polydatin and emodin in the test sample solution according to the linear regression equation prepared in the step (3);
the chromatographic conditions of the high performance liquid chromatograph in the step (3) and the step (4) are as follows:
a chromatographic column: purospher STAR LP RP-18endcapped, 4.6 × 250mm, 5 μm; mobile phase: pure water is phase A, acetonitrile is phase B, and gradient elution is carried out under the condition that the gradient elution is 0-15 min, wherein the content of B% is 5% → 25%; 15-51 min: b% 25% → 37%; 51-75 min: b% 37% → 85%; flow rate of flowIs 0.6 mL/min-1(ii) a The detection wavelength is 306nm, and the column temperature is 40 ℃;
the ginger processed giant knotweed rhizome is prepared by the following method: diluting rhizoma Polygoni Cuspidati with water, adding rhizoma Zingiberis recens juice 17 wt% of rhizoma Polygoni Cuspidati, spreading into rhizoma Polygoni Cuspidati, moistening, parching at 240 deg.C for 11min, and cooling.
2. The method for detecting the quality of processed ginger processed giant knotweed rhizome according to claim 1, wherein the linear regression equation of polydatin obtained in step (3) is y =2E +07x-319.3, R2= 0.9999; the linear regression equation of resveratrol is y =1E +08x-19725, R2= 0.9998; the linear regression equation of emodin is y =3E +07x +102440, R2=0.9993。
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| Polygonum cuspidatum extracts as bioactive antioxidaion, anti-tyrosinase, immune stimulation and anticancer agents;Chih-Chen Lee et al.;《Journal of Bioscience and Bioengineering》;20141012;第119卷(第4期);第464-469页 * |
| 虎杖不同炮制品的实验研究;江海燕等;《中医药学刊》;20020831;第20卷(第4期);第426-427页，尤其是第426页右侧第3-5行 * |
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