CN110441414B - Method for establishing fingerprint of Jinshui Liujun decoction - Google Patents
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Abstract
The invention relates to the technical field of traditional Chinese medicine detection, and particularly discloses a method for establishing fingerprint of Jinshui Liujun decoction, which comprises the following steps: a. preparation of a test solution: weighing radix rehmanniae Preparata, radix Angelicae sinensis, radix Glycyrrhizae Preparata, Poria, rhizoma Pinelliae and pericarpium Citri Tangerinae according to the weight ratio of each component in the decoction of six principal drugs of Jinshui, soaking in water and rhizoma Zingiberis recens slice, decocting, and filtering to obtain filtrate as sample solution; b. preparation of control solutions: weighing hesperidin and ammonium glycyrrhizinate, and dissolving with methanol to obtain a mixed solution, i.e. a reference solution; c. performing high performance liquid chromatography determination on the test solution and the reference solution respectively to obtain effective constituent fingerprint of JINSHUILIUJUN decoction. The method provided by the invention can carry out qualitative analysis on chemical components in the Jinshuihuijun decoction, provides a basis for evaluating the quality of the Jinshuihuijun decoction, sets specific quality standards for the Jinshuihuijun decoction and lays a foundation for excavating drug effect substances of the Jinshuihuijun decoction.
Description
Technical Field
The invention relates to the technical field of traditional Chinese medicine detection, in particular to a method for establishing fingerprint of Jinshui Liujun decoction.
Background
The Jinshuihuijun decoction is mainly used for treating diseases such as lung-kidney deficiency cold, water flooding phlegm, cough and nausea and the like, is composed of six medicines such as Chinese angelica, prepared rehmannia root, dried orange peel, pinellia tuber and Indian buead, and honey-fried licorice root, is mainly used for diseases mainly clinically manifested by cough and asthma in modern clinic, has abundant clinical curative effect basis, and is one of the prescriptions carried in ancient classic famous prescription catalogues (the first batch) issued by the State administration of traditional Chinese medicine.
At present, the quality standards of traditional Chinese medicines are difficult to unify, the main effective components of the same traditional Chinese medicine are different when the same traditional Chinese medicine is used for treating different diseases, and the classical famous prescription requires that the quality of medicinal materials in a prescription is uniform and stable, so that the determination of the primordium of each traditional Chinese medicine before research and development has very important significance in deep examination and confirmation of the clinical medication condition, the source change of the medicinal materials and the revision condition of Chinese pharmacopoeia of the calendar edition. The quality standard of the traditional Chinese medicine is mainly to measure the contents of active ingredients and effective parts, but the traditional Chinese medicine components are complex, the quality of the traditional Chinese medicine is difficult to clarify by a single active ingredient or effective part, and the focus of attention is on how to establish the quality standard of the traditional Chinese medicine composition and whether to establish a relatively recognized evaluation standard.
Therefore, in order to better reflect the medicinal quality of the classic famous prescription, namely the Jinshuijiujun decoction, the establishment of the fingerprint of the Jinshuihuijun decoction is very necessary.
Disclosure of Invention
Aiming at the problem that the quality and evaluation standard of the existing Jinshui Liujun decoction cannot be unified, the invention provides a method for establishing a Jinshui Liujun decoction fingerprint.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
the method for establishing the Jinshuihuijun decoction fingerprint comprises the following steps:
a. preparation of a test solution: weighing radix rehmanniae Preparata, radix Angelicae sinensis, radix Glycyrrhizae Preparata, Poria, rhizoma Pinelliae and pericarpium Citri Tangerinae according to the weight ratio of each component in the decoction of six principal drugs of Jinshui, soaking in water and rhizoma Zingiberis recens slice, decocting, and filtering to obtain filtrate as sample solution;
b. preparation of control solutions: dissolving hesperidin and ammonium glycyrrhizinate with solvent to obtain mixed solution as reference solution;
c. and (3) high performance liquid chromatography detection: respectively detecting the test solution and the reference solution by using high performance liquid chromatography to obtain the fingerprint of the Jinshuihuliujun decoction, wherein the conditions of the high performance liquid chromatography are as follows:
stationary phase: a C18 chromatography column;
mobile phase: the mobile phase A is acetonitrile, and the phase B is 0.1-0.3 wt% phosphoric acid solution;
the gradient elution conditions were: 0-10min, 5-8 vol% of phase A and 95-92 vol% of phase B; 10-35min, 8-14 vol% of phase A and 92-86 vol% of phase B; 35-50min, 14-16 vol% of phase A and 86-84 vol% of phase B; 50-65min, 16-21 vol% of phase A and 84-79 vol% of phase B; 65-85min, 21-32 vol% of phase A and 79-68 vol% of phase B; 85-95min, 32-40 vol% of phase A and 68-60 vol% of phase B; 95-120min, 40-65 vol% of phase A and 60-35 vol% of phase B; 120-125min, 65-5 vol% of phase A and 35-95 vol% of phase B; 125 ℃ for 130min, 5 vol% of the phase A and 95 vol% of the phase B.
Compared with the prior art, the method for establishing the effective component fingerprint of the Jinshuihuijun decoction provided by the invention has the advantages that the similarity between the obtained Jinshuihuijun decoction fingerprint and the comparison fingerprint is more than 0.9, the stability is good, the repeatability is good, the difference between different batches is small, the uniformity and the stability are good between the same batch, the obtained fingerprint information is large, the spectrum peak information is rich, the number of the common peaks can reach 12, each common peak is an effective medicinal component in the Jinshuihuijun decoction, the integral medicinal component information of the Jinshuihuijun decoction can be completely provided, the method is favorable for preparing the related specific quality standard for the Jinshuihuijun decoction, and the foundation is laid for the identification and the medicinal effect substance excavation of the later-stage Jinshuihuijun decoction.
The stationary phase adopts a C18 chromatographic column, the phase A of the mobile phase is acetonitrile, the phase B is 0.1-0.3 wt% of phosphoric acid solution, the combination of the stationary phase and the mobile phase can increase the separation degree of each active ingredient in the gold water six monarch decoction extract by matching with the specific elution condition, the number of the common peaks of the fingerprint spectra can be effectively increased, the information content of the gold water six monarch decoction fingerprint spectra is increased, the peak shape and the separation degree of the common peaks are better, the response of the chromatographic peaks is good, even if water is used as an extraction solvent and the extract is directly subjected to high performance liquid chromatography, the chromatographic effect can be achieved, the addition of organic solvents such as organic extraction solvents and organic extraction solvents is omitted, and the universality and the effectiveness of fingerprint spectrum detection are ensured.
The method for establishing the Jinshuihuliujun decoction fingerprint spectrum can be used for qualitatively analyzing certain chemical components in the substance standard and provides an important basis for evaluating the quality of the substance standard.
Preferably, the adding amount of water in the step a is 7-8 times of the weight of the Liujun decoction, and the soaking time is 20-30 min; the decocting process comprises the following steps: decocting with strong fire for 8-10min, and decocting with slow fire for 20-22 min.
The method for establishing the fingerprint of the effective ingredients of the Jinshuihujun decoction ensures the ancient decoction process, the original decoction is injected into a liquid phase for analysis, the ancient decoction process is improved, and the medicine can be decocted to the optimal state by setting a specific decoction mode and decoction time, so that the extract yield of the medicine is maximized.
Preferably, the solvent in step b is 80-100 vol% methanol solution.
Preferably, the stationary phase of the high performance liquid chromatography adopts an elette C18 chromatographic column; a mobile phase A of the high performance liquid chromatography is acetonitrile, and a phase B of the high performance liquid chromatography is 0.1 wt% of phosphoric acid solution.
An elette C18 chromatographic column is adopted, and an acetonitrile-0.1 wt% phosphoric acid solution is used as a mobile phase, so that the separation degree between common peaks of the established fingerprint is highest, and the peak shape is best.
Preferably, the flow rate of the mobile phase of the high performance liquid chromatography in the step c is 0.7-0.8ml/min, the column temperature of the chromatographic column is 34-36 ℃, and the detection wavelength is 260-270 nm.
The column temperature and the flow rate of the mobile phase of the chromatographic column can be set to increase the separation degree of corresponding components in the chromatogram.
Preferably, the flow rate of the mobile phase is 0.8 ml/min.
The flow rate of 0.8ml/min just meets the separation speed of chromatographic columns to each component in the Jinshuijuijun decoction.
Preferably, the column temperature of the high performance liquid chromatography is 35 ℃, and the detection wavelength is 260 nm.
The wavelength of 260nm is the optimal absorption wavelength established by the fingerprint of the Liujun decoction of Jinshui, and under the condition of the wavelength, the base line of each common peak is stable and the response is good.
Drawings
FIG. 1 is a high performance liquid chromatogram of a sample solution prepared by decocting Liujun decoction with gold water in an embodiment of the invention;
FIG. 2 is a high performance liquid chromatogram of a control solution in an example of the invention;
FIG. 3 is a fingerprint of 17 batches of Jinshui Liujun Jian in the example of the present invention; wherein R is a common mode;
FIG. 4 is a 17 batches of Jinshui Liujun Jian fingerprint clustering tree-like relation chart in the embodiment of the invention;
FIG. 5 is a fingerprint chromatogram macadam of 17 batches of Jinshui Liujun decoction in the example of the invention;
FIG. 6 is a main component analysis chart according to 12 common peak-peak areas in fingerprint of Liujun decoction of 17 batches of Jinshui in the example of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
Method for establishing fingerprint of Jinshui Liujun decoction
1. Instrument and reagent
The instrument comprises the following steps: shimadzu LC-20AT HPLC, SPD-20 UV detector, Shimadzu Labsolution workstation, AUW220D electronic balance (one hundred thousandth, Shimadzu corporation, Japan); BS224S model electronic balance (one in ten thousand, Sartorius); KQ250DB model digital control ultrasonic cleaner (Steuer City Zeihua Instrument, Inc.); KQ5200 type water bath (Kunshan ultrasonic instruments Co., Ltd.);
reagent testing: acetonitrile (pure chromatogram) (Shanghai Shaxing chemical industry Co., Ltd.), phosphoric acid (West Long chemical Co., Ltd., Shanguang Shantou city, Guangdong province), hesperidin control (lot number: 0856-; the collected prescription drug taste information is shown in table 1:
TABLE 1 prescription drug taste information
Randomly combining the collected prescription drug flavor information into 17 batches of Jinshuijiuni decoction, as shown in Table 2:
TABLE 2 randomly combined 17 batches of Jinshui Liujun decoction
2. Method and results
Preparing a test solution: taking 15g of prepared rehmannia root, 7.5g of Chinese angelica, 3.75g of honey-fried licorice root, 7.5g of tuckahoe, 7.5g of pinellia tuber, 7.5g of dried orange peel and 3 pieces of ginger, adding 400mL of water, soaking for 20min, decocting for 9 min with strong fire, decocting for 21 min with slow fire and filtering to obtain the traditional Chinese medicine;
preparation of a reference solution: respectively weighing 5.45mg of hesperidin and 3.75mg of ammonium glycyrrhizinate, precisely weighing, placing in a 25mL measuring flask, dissolving and diluting with 100 vol% methanol to obtain a mixed solution containing 0.218mg of hesperidin and 0.15mg of ammonium glycyrrhizinate per 1 mL;
and (3) high performance liquid chromatography detection: adopting Shimadzu LC-20AT high performance liquid chromatograph with stationary phase of elette C18 chromatographic column (4.6 × 250mm, 4.6 μm) and mobile phase of acetonitrile (A) -0.1% phosphoric acid (B); the gradient elution conditions were: 0-10min, 5-8 vol% of phase A and 95-92 vol% of phase B; 10-35min, 8-14 vol% of phase A and 92-86 vol% of phase B; 35-50min, 14-16 vol% of phase A and 86-84 vol% of phase B; 50-65min, 16-21 vol% of phase A and 84-79 vol% of phase B; 65-85min, 21-32 vol% of phase A and 79-68 vol% of phase B; 85-95min, 32-40 vol% of phase A and 68-60 vol% of phase B; 95-120min, 40-65 vol% of phase A and 60-35 vol% of phase B; 120-125min, 65-5 vol% of phase A and 35-95 vol% of phase B; 125-130min, 5 vol% of phase A and 95 vol% of phase B; column temperature 35 ℃, flow rate: 0.8ml/min, wavelength 260 nm.
The chromatogram of the sample solution obtained by high performance liquid chromatography is shown in FIG. 1, and the chromatogram of the control solution is shown in FIG. 2.
3. Methodology investigation
Precision: taking the sample solution, continuously injecting sample for 6 times according to the chromatographic conditions, and recording the chromatogram. And (3) calculating the RSD of the relative retention time and the relative peak area of the common peak by taking the No. 12 chromatographic peak (ammonium glycyrrhizinate) as a reference peak, wherein the RSD is lower than 5.0 percent, and the instrument precision is good.
Repeatability: taking 6 parts of the same test sample solution, determining according to the chromatographic conditions, recording a chromatogram, taking a No. 12 chromatographic peak (ammonium glycyrrhizinate) as a reference peak, and calculating the relative retention time of the common peak and the RSD of the relative peak area to be lower than 5.0 percent, thereby indicating that the method has good repeatability.
Stability: taking 1 part of the test solution, respectively measuring 0, 2, 4, 8, 12 and 24 hours after preparation according to the chromatographic conditions, recording a chromatogram, taking a No. 12 chromatographic peak (ammonium glycyrrhizinate) as a reference peak, calculating the relative retention time of the common peak and the RSD of the relative peak area to be lower than 5.0 percent, and indicating that the substance standard test solution has good stability within 24 hours.
4. Establishment and detection analysis of fingerprint
Establishing a fingerprint spectrum: and (3) respectively obtaining chromatograms by using 17 batches of Jinshuihujun decoction which are randomly combined according to the method, introducing chromatogram data into software of a traditional Chinese medicine chromatogram fingerprint similarity evaluation system (2012 edition), setting a reference spectrum, and marking 12 common peaks to generate a fingerprint, wherein the software is shown in figure 3.
And (3) similarity evaluation: similarity between the fingerprint of the six monarch drugs in 17 batches of Jinshui decoction and the generated comparison fingerprint is more than 0.9, and as shown in Table 3, the preparation process is stable and the difference between material groups is small.
Table 317 batches of fingerprint similarity of Jinshui Liujun decoction
And (3) data analysis:
SPSS analysis: introducing 12 common peak areas of 17 batches of Jinshuihuijun decoction into IBM SPSS staticisics software for cluster analysis among groups, wherein the distance among samples is calculated by adopting an Euclidean distance method to obtain a 17 batches of Jinshuihuijun decoction fingerprint clustering tree-like relation graph (shown in figure 4) and a lithotripsy graph (shown in figure 5), and the cluster analysis of figure 4 shows that 17 batches of samples can be divided into 2 types, wherein WZJZ-1, 2, 3, 4, 5, 10 and 13 can be grouped into one type, and the rest batches of samples can be grouped into one type;
performing principal component factor analysis on 12 labeled peak areas according to the characteristic values and contribution rates of principal components, calculating a correlation coefficient matrix, calculating principal component characteristic values, accumulated contribution rates and calculating a principal component comprehensive score, and evaluating the prepared 17 batches of Jinshuihuijun decoction, wherein the results are shown in table 5, as can be seen from table 4 and fig. 5, the characteristic values of peaks 1, 2 and 3 are large (greater than 1) and steep in connection among the 12 labeled components, the accumulated variance contribution rate is 89.495%, the accumulated variance contribution rate of the factors is more than 85% and is taken as a principal component extraction standard, the first 3 components can integrally reflect more than 89.495% of index information, wherein the characteristic value of the extracted principal component 1 is 8.319, and the contribution rate is 69.324%; the characteristic value of the extracted principal component 2 is 1.418, and the contribution rate is 11.820%; the characteristic value of the extracted principal component 3 was 1.002, and the contribution rate was 8.351%.
TABLE 4 explanation of variation of the total variance of Jinshui, Liujun decoction
SIMCA analysis: the recorded 12 common peak areas of the 17 batches of the Jinshuihuliujun decoction are subjected to main component analysis by using SIMCA 13.0 software to obtain a figure 6, and as can be seen from a PCA diagram of the figure 6, WZJZ-1, 2, 3, 4, 5, 10 and 13 can be grouped into one type, and samples of the other batches can be grouped into one type.
The above analysis results are combined to show that:
the similarity of 12 common peaks marked by the fingerprint of the six monarch drugs of 17 batches of Jinshui decoction is more than 0.9, which indicates that the difference between different batches is not large, and after the areas of the 12 common peaks are analyzed by SPSS and SIMCA, the substance references of different batches decocted by the same method have certain difference, and the substance references of 17 batches can be divided into 2 types.
The marking peaks 1, 2 and 3 are influence factors of main components, each component in the Jinshuijiujun decoction is obtained by collecting prescription medicinal materials of different batches and different production places and randomly combining, different medicinal materials are mixed and decocted, and the dissolving assisting or dissolving inhibiting effect on certain components can generate difference on the content of certain components, so that the similarity of a fingerprint is not enough to decide the advantages and disadvantages of the components during comprehensive evaluation, the quality of a substance reference is evaluated in multiple aspects through main components, factors and clustering analysis, mutual verification and supplement, the quality of the substance reference is evaluated in multiple aspects, the substance reference is important to multi-angle evaluation, the classical famous Jinshuijiujun decoction has no related drug effect screening research at present, the fingerprint method established by the invention is not only beneficial to establishing related specific quality standards for the substance reference sequence of the Jinshuijuijun decoction, but also provides reference for identifying the components by utilizing the technology such as liquid-mass combination and the like in the later stage, thereby laying a foundation for digging the drug effect substances of the six monarch drugs of Jinshui decoction substance standard.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. A method for establishing fingerprint of Jinshuihuijun decoction is characterized in that: the method comprises the following steps:
a. preparation of a test solution: weighing radix rehmanniae Preparata, radix Angelicae sinensis, radix Glycyrrhizae Preparata, Poria, rhizoma Pinelliae and pericarpium Citri Tangerinae according to the mass ratio of each component in the decoction of six principal drugs of Jinshui, soaking in water and rhizoma Zingiberis recens slice, decocting, and filtering to obtain filtrate as sample solution;
b. preparation of control solutions: dissolving hesperidin and ammonium glycyrrhizinate with solvent to obtain mixed solution as reference solution;
c. and (3) high performance liquid chromatography detection: respectively detecting the test solution and the reference solution by using high performance liquid chromatography to obtain the fingerprint of the Jinshuihuliujun decoction, wherein the conditions of the high performance liquid chromatography are as follows:
stationary phase: a C18 chromatography column;
mobile phase: the mobile phase A is acetonitrile, and the phase B is 0.1-0.3 wt% phosphoric acid solution;
the gradient elution conditions were: 0-10min, 5-8 vol% of phase A and 95-92 vol% of phase B; 10-35min, 8-14 vol% of phase A and 92-86 vol% of phase B; 35-50min, 14-16 vol% of phase A and 86-84 vol% of phase B; 50-65min, 16-21 vol% of phase A and 84-79 vol% of phase B; 65-85min, 21-32 vol% of phase A and 79-68 vol% of phase B; 85-95min, 32-40 vol% of phase A and 68-60 vol% of phase B; 95-120min, 40-65 vol% of phase A and 60-35 vol% of phase B; 120-125min, 65-5 vol% of phase A and 35-95 vol% of phase B; 125 ℃ for 130min, 5 vol% of the phase A and 95 vol% of the phase B.
2. The method for establishing Jinshuihuijun decoction fingerprint spectrum of claim 1, which is characterized in that: the adding amount of water in the step a is 7-8 times of the weight of the six monarch drugs of Jinshui, and the soaking time is 20-30 min; the decocting process comprises the following steps: decocting with strong fire for 8-10min, and decocting with slow fire for 20-22 min.
3. The method for establishing Jinshuihuijun decoction fingerprint spectrum of claim 1, which is characterized in that: the solvent in the step b is 80-100 vol% of methanol solution.
4. The method for establishing Jinshuihuijun decoction fingerprint spectrum of claim 1, which is characterized in that: the stationary phase of the high performance liquid chromatography adopts an elette C18 chromatographic column; a mobile phase A of the high performance liquid chromatography is acetonitrile, and a phase B of the high performance liquid chromatography is 0.1 wt% of phosphoric acid solution.
5. The method for establishing Jinshuihuijun decoction fingerprint spectrum of claim 1, which is characterized in that: the flow rate of the mobile phase of the high performance liquid chromatography in the step c is 0.7-0.8ml/min, the column temperature of the chromatographic column is 34-36 ℃, and the detection wavelength is 260-270 nm.
6. The method for establishing Jinshuihuijun decoction fingerprint spectrum of claim 5, which is characterized in that: the flow rate of the mobile phase was 0.8 ml/min.
7. The method for establishing Jinshuihuijun decoction fingerprint spectrum of claim 5, which is characterized in that: the temperature of the chromatographic column is 35 ℃, and the detection wavelength is 260 nm.
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