CN114720604A - Construction method of heat-clearing and phlegm-eliminating traditional Chinese medicine characteristic map and characteristic map thereof - Google Patents
Construction method of heat-clearing and phlegm-eliminating traditional Chinese medicine characteristic map and characteristic map thereof Download PDFInfo
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Abstract
The invention discloses a construction method of a feature map of a traditional Chinese medicine for clearing heat and eliminating phlegm, which relates to the technical field of pharmaceutical analysis, and comprises the following steps: step one, preparation of reference substance solution: preparing a proper amount of 6-methoxyguaiacol reference substance into 0.03mg/mL solution per 1mL with methanol to obtain reference substance solution; step two, preparation of a test solution: precisely measuring 30ml of heat-clearing and phlegm-eliminating traditional Chinese medicine, shaking and extracting with ethyl acetate for 3 times, 30ml each time, combining ethyl acetate solutions, spin-drying at low temperature, dissolving residues with methanol, and fixing the volume to 5 ml; step three-color spectrum condition determination: precisely sucking 1 mul of reference substance solution and sample solution respectively, injecting into a gas chromatograph, heating in a specific manner, and recording 36min chromatogram to obtain GC characteristic spectrum of the heat-clearing and phlegm-eliminating traditional Chinese medicine. The characteristic map can be used for comprehensively and integrally controlling and evaluating the quality of the characteristic map, and the authenticity, integrity and consistency of the characteristic map are guaranteed.
Description
Technical Field
The invention relates to the technical field of pharmaceutical analysis, in particular to a construction method of a characteristic spectrum of a traditional Chinese medicine for clearing heat and eliminating phlegm and a characteristic spectrum thereof.
Background
The traditional Chinese medicine for clearing heat and eliminating phlegm is liquid naturally dripped from fresh stems of a plurality of plants in Phyllostachys of Gramineae after being heated, has the effects of clearing heat, eliminating phlegm, relieving convulsion and promoting resuscitation, is mainly used for treating lung heat cough with excessive phlegm, high fever and polydipsia, infantile phlegm-heat convulsion and the like, and is called as 'saint of phlegm family' in materia medica Yan Yi (the Yan Yi). The database of the national drug administration website inquires that the number of approved single prescriptions and the number of approved compound prescriptions of the traditional Chinese medicine preparation are 43, wherein the number of the single prescriptions is 24, the number of the compound prescriptions is 19, and the method relates to a plurality of production enterprises in China, and Jiangxi is a main production area.
The current quality standard of heat-clearing and phlegm-eliminating traditional Chinese medicines is currently recorded in traditional Chinese medicinal materials (the first volume) of drug standards of Ministry of health of the people's republic of China (1992), and the traditional Chinese medicines are specified as liquid naturally drained from fresh stems of Phyllostachys plants after being heated. The Phyllostachys has more than 50 species, and is also influenced by the factors such as the producing area and the harvesting period, and the specific heating temperature and time parameters are not specified in the processing method. Therefore, under the influence of factors such as the basic source, the producing area, the harvesting period, the processing method and the like, the existing legal quality standard of the traditional Chinese medicine for clearing heat and eliminating phlegm only has characters, thin-layer chromatography identification and pH value, total solid and relative density check items, which are far from enough to comprehensively reflect the quality of the traditional Chinese medicine and are difficult to ensure the quality authenticity, integrity and consistency.
The literature reports that the traditional Chinese medicine mainly contains phenols, lignin, amino acid and other components, the phenol components are the effective components of the traditional Chinese medicine, the quality control technical report of the traditional Chinese medicine at present mainly focuses on the content measurement of single-component phenols, sugar, amino acid and other components, the quality of the traditional Chinese medicine for clearing heat and eliminating phlegm is difficult to control and evaluate comprehensively, and meanwhile, relevant research reports such as a characteristic map of the traditional Chinese medicine for clearing heat and eliminating phlegm are not found at present. The Chinese medicine characteristic map is a comprehensive and quantifiable identification means, is mainly used for evaluating the authenticity, stability, consistency and the like of the quality of Chinese medicinal materials and preparations thereof, can comprehensively reflect the types and the quantity of chemical components of the Chinese medicinal materials by establishing the Chinese medicine characteristic map, and further performs integral control, evaluation and description on the quality of the Chinese medicinal materials.
Disclosure of Invention
The invention aims to provide a construction method of a characteristic spectrum of a traditional Chinese medicine for clearing heat and eliminating phlegm and a characteristic spectrum thereof, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a construction method of a feature map of a traditional Chinese medicine for clearing heat and eliminating phlegm comprises the following steps: step one preparation of reference solution: accurately weighing a proper amount of 6-methoxyguaiacol reference substance, and preparing 0.03mg/mL solution per 1mL by using methanol to obtain a reference substance solution; step two, preparation of a test solution: precisely measuring 30ml of heat-clearing and phlegm-eliminating traditional Chinese medicine, extracting with ethyl acetate for 3 times, each time extracting with 30ml, mixing ethyl acetate solutions, spin-drying at low temperature, dissolving the residue with methanol, and metering to 5ml to obtain a test solution; step three-color spectrum condition determination: precisely sucking 1 mul of reference substance solution and sample solution respectively, injecting into a gas chromatograph at a split ratio of 50:1, heating in a specific manner, and recording 36min chromatogram to obtain GC characteristic maps of the traditional Chinese medicine for clearing heat and eliminating phlegm; step four, constructing a contrast characteristic spectrum of the traditional Chinese medicine for clearing heat and eliminating phlegm: taking thirteen batches of heat-clearing and phlegm-eliminating traditional Chinese medicine samples, respectively preparing the test solution according to the preparation method of the test solution in the first step, determining according to chromatographic conditions in the third step to obtain chromatograms of the thirteen batches of samples, respectively introducing the chromatograms into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, shearing a solvent peak for 0-2min, carrying out multi-point correction on 14 peaks, adopting Mark peak matching, adopting traditional Chinese medicine chromatogram fingerprint similarity evaluation software to compare 13 batches of characteristic spectra, determining common characteristic peaks, and generating a comparison characteristic spectrum consisting of fourteen common peaks.
On the basis of the technical scheme, the invention also provides the following optional technical scheme:
in one alternative: in the third step, DB-WAX is adopted as a chromatographic column, N2 is adopted as carrier gas, the flow rate of the column is 3.5ml/min, and the temperature of a sample inlet is 250 ℃; the FID detector temperature was 280 ℃.
In one alternative: the heating in a specific mode in the third step is as follows: the initial temperature is 75 ℃, the temperature is increased to 150 ℃ at the temperature increasing rate of 5 ℃/min, and the temperature is kept at 150 ℃ for 0.5 min; heating to 210 deg.C at a heating rate of 3 deg.C/min, maintaining the temperature at 210 deg.C for 0.5min, and operating at 260 deg.C for 5 min.
In one alternative: and constructing a control characteristic spectrum of the heat-clearing and phlegm-eliminating traditional Chinese medicine in the step four, and respectively carrying out precision test, stability test and repeatability test on the heat-clearing and phlegm-eliminating traditional Chinese medicine sample.
In one alternative: the precision test comprises the following steps: taking a heat-clearing and phlegm-eliminating traditional Chinese medicine sample, preparing a test solution according to the test solution preparation method in the step two, continuously injecting samples for 6 times, and measuring chromatographic conditions according to the step three; the RSD of the relative retention time of each characteristic peak and the reference peak is calculated by taking the No. 7 peak as the reference peak, and the result shows that the RSD of the relative retention time of 13 common characteristic peaks in 6 measurement characteristics is less than or equal to 0.01 percent.
In one alternative: the stability test procedure was as follows: taking the traditional Chinese medicine sample for clearing heat and eliminating phlegm, preparing the sample solution according to the preparation method of the sample solution in the step two, respectively measuring the sample solution under chromatographic conditions in the step three at 0, 4, 8, 12, 16 and 24 hours, taking the No. 7 peak as a reference peak, calculating the RSD of the relative retention time of each characteristic peak and the reference peak, and the result shows that the RSD of 13 common characteristic peaks in 6 measurement characteristics is less than or equal to 0.02%.
In one alternative: the repeatability test procedure was as follows: taking the same batch of heat-clearing and phlegm-eliminating traditional Chinese medicines, preparing 6 parts of test solution in parallel according to the step two, carrying out chromatographic condition determination in the step three, taking the No. 7 peak as a reference peak, and calculating the RSD of the relative retention time of each characteristic peak and the reference peak, wherein the result shows that the RSD of the relative retention time of 13 common characteristic peaks in 6 determination characteristics is less than or equal to 0.02%.
The feature map of the traditional Chinese medicine for clearing heat and eliminating phlegm is constructed by the construction method of the feature map of the traditional Chinese medicine for clearing heat and eliminating phlegm.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention establishes the characteristic spectrum of the traditional Chinese medicine for clearing heat and eliminating phlegm by a gas chromatograph, and determines the precision, reproducibility and stability of a standard control characteristic spectrum by tests;
2. the invention establishes and discloses a construction method of a characteristic map of a traditional Chinese medicine for clearing heat and eliminating phlegm and the characteristic map, which can be used for comprehensively and integrally controlling and evaluating the quality of the traditional Chinese medicine and ensuring the authenticity, integrity and consistency of the traditional Chinese medicine.
Drawings
FIG. 1 is a GC characteristic spectrum of the heat-clearing and phlegm-resolving traditional Chinese medicine of the present invention.
FIG. 2 is a chromatogram superposition chart of 13 batches of samples in a control characteristic spectrum of the traditional Chinese medicine for clearing heat and eliminating phlegm.
FIG. 3 is a peak chromatogram of a methanol solvent according to the present invention.
FIG. 4 is a control profile of the present invention.
FIG. 5 is a chromatogram of a test solution according to the present invention.
Figure 6 is a chromatogram of a guaiacol control solution of the present invention (peak No. 4).
FIG. 7 is a chromatogram of a 4-methyl guaiacol control solution of the present invention (peak No. 5).
FIG. 8 is a chromatogram of a phenol control solution of the present invention (peak No. 6).
FIG. 9 is a chromatogram of a 6-methoxyguaiacol control solution of the present invention (peak No. 7).
FIG. 10 is a chromatogram of a methylphenol control solution of the present invention (peak No. 8).
FIG. 11 is a chromatogram of an ethylphenol control solution of the present invention (peak 9).
FIG. 12 is an ethyl acetate extraction chromatogram of the present invention.
FIG. 13 is an ether extraction chromatogram of the present invention.
FIG. 14 is a water-saturated n-butanol extraction chromatogram of the present invention.
FIG. 15 shows a chromatogram (HP-5 column) according to the present invention.
FIG. 16 is a chromatogram of the present invention (DB-17 column).
FIG. 17 is a chromatogram (DB-WAX column) of the present invention.
FIG. 18 is a chromatogram of test group 1 of the present invention.
FIG. 19 is a chromatogram of test group 2 of the present invention.
FIG. 20 is a chromatogram of test group 3 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 described in further detail below with reference to the accompanying drawings and embodiments. The examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention. Any obvious modifications or variations can be made to the present invention without departing from the spirit or scope of the present invention.
In one embodiment, a construction method of a heat-clearing and phlegm-eliminating traditional Chinese medicine characteristic spectrum is provided
1. Instrument and reagent
1.1 Instrument and reagents: model 8890B gas chromatograph, equipped with hydrogen Flame Ionization Detector (FID), model 7693 liquid autosampler, Openlab chromatography workstation. Model BT25S one hundred thousand electronic balance, Milli-Q ultrapure water meter. 6-Methoxyguaiacol (Stanford Chemicals, batch No. MA190816-07, 99.08% pure).
2. Method and results
2.1 preparation of reference solutions: weighing appropriate amount of 6-methoxyguaiacol reference substance, precisely weighing, and making into 0.03mg/mL solution per 1mL with methanol.
2.2 preparation of test solution: precisely measuring 30ml of heat-clearing and phlegm-eliminating traditional Chinese medicine, shaking and extracting with ethyl acetate for 3 times, 30ml each time, combining ethyl acetate solutions, spin-drying at low temperature, dissolving the residue with methanol, and metering to 5 ml.
2.3 chromatographic conditions: DB-WAX (30m × 0.32mm × 0.25um) was used as a chromatographic column, N2 (99.999%) was used as a carrier gas, and the column flow rate: 3.5ml/min, injection port temperature: 250 ℃; FID detector temperature 280 ℃. Precisely sucking 1 μ l of each of the reference solution and the sample solution, injecting into a gas chromatograph at a split ratio of 50:1, heating according to the procedure of Table 1 to obtain GC characteristic spectrum of the heat-clearing and phlegm-resolving traditional Chinese medicine, as shown in FIG. 1, and the retention time of the characteristic peak is shown in Table 2. The theoretical plate number calculated by 6-methoxy guaiacol peak should not be lower than 50000.
TABLE 1 temperature programming table
| Initial temperature (. degree. C.) | Rate (. degree. C./min) | Temperature (. degree. C.) | Retention time (min) |
| 75 | 5 | 150 | 0.5 |
| / | 3 | 210 | 0.5 |
TABLE 2 Retention time of characteristic peaks
| Peak | Retention time | |
| 1 | 8.433 | |
| 2 | 9.935 | |
| 3 | 13.160 | |
| 4 | 13.739 | |
| 5 | 15.579 | |
| 6 | 16.694 | |
| 7 | 17.134 (refer to peak) | |
| 8 | 18.356 | |
| 9 | 20.486 | |
| 10 | 20.806 | |
| 11 | 22.522 | |
| 12 | 24.577 | |
| 13 | 25.634 | |
| 14 | 29.409 |
2.4 methodological investigation:
2.4.1 precision test: taking the traditional Chinese medicine sample for clearing heat and eliminating phlegm, preparing the sample solution according to the preparation method of the sample solution under item 2.1, continuously injecting the sample for 6 times, and determining according to the chromatographic condition under item 2.3. The RSD of the relative retention time of each characteristic peak and the reference peak is calculated by taking the No. 7 peak (6-methoxyguaiacol) as the reference peak, and the result shows that the RSD of the relative retention time of 13 common characteristic peaks in 6 measurement characteristics is less than or equal to 0.01 percent, and the RSD is shown in Table 3 and shows that the precision is good.
TABLE 3 results of precision test
2.4.2 stability test: taking the traditional Chinese medicine samples for clearing heat and eliminating phlegm, preparing the sample solution according to the preparation method of the sample solution under item 2.1, and respectively measuring the sample solution under the chromatographic conditions under item 2.3 for 0, 4, 8, 12, 16 and 24 hours. The RSD of the relative retention time of each characteristic peak and the reference peak is calculated by taking the No. 7 peak (6-methoxyguaiacol) as the reference peak, and the result shows that the RSD of the relative retention time of 13 common characteristic peaks in 6 measurement characteristics is less than or equal to 0.02 percent, and the RSD is shown in Table 4 and shows that the test solution is stable within 24 hours.
TABLE 4 stability test results
2.4.3 repeatability tests: taking the same batch of heat-clearing and phlegm-eliminating traditional Chinese medicines, preparing 6 parts of test solution in parallel according to the method under the item 2.1, measuring according to the chromatographic condition under the item 2.3, taking the No. 7 peak (6-methoxyguaiacol) as a reference peak, calculating the RSD of the relative retention time of each characteristic peak and the reference peak, and the result shows that the RSD of 13 common characteristic peaks in 6 measurement characteristics is less than or equal to 0.02 percent, and the method has good repeatability as shown in Table 5.
TABLE 5 repeatability test results
3, constructing a contrast characteristic spectrum of the traditional Chinese medicine for clearing heat and eliminating phlegm: taking 13 batches of heat-clearing and phlegm-eliminating traditional Chinese medicine samples, respectively preparing the test solution according to the preparation method of the test solution under item 2.1, determining according to the chromatographic condition under item 2.3 to obtain chromatograms of the 13 batches of samples, respectively introducing the chromatograms into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, shearing solvent peaks for 0-2min, carrying out multi-point correction on 14 peaks, and adopting Mark peak matching, as shown in figure 2.
Comparing 13 batches of characteristic spectra with Chinese medicinal chromatogram fingerprint spectrum identification degree evaluation software, determining common characteristic peak (excluding 0-2min solvent peak, see figure 3), and generating control characteristic spectrum composed of 14 common peaks, as shown in figure 4, wherein the reference peak is 6-methoxyguaiacol peak (No. 7 peak).
4, confirming characteristic spectrum chromatographic peaks: taking a proper amount of guaiacol, 4-methyl guaiacol, phenol, 4-ethyl guaiacol, methyl phenol, ethyl phenol, 4-vinyl guaiacol and 6-methoxy guaiacol reference substances, measuring according to the chromatographic condition under the item of 2.3, recording a chromatogram, and identifying main chromatographic peaks of a chromatogram of a test solution by retention time as shown in a graph 5-11, wherein the peak 4 is guaiacol, the peak 5 is 4-methyl guaiacol, the peak 6 is phenol, the peak 7 is 6-methoxy guaiacol, the peak 8 is p-methyl phenol, and the peak 9 is p-ethyl phenol.
5, similarity analysis: the similarity between the 13 batches of feature maps and the generated comparison feature map is more than 0.950 by using traditional Chinese medicine chromatography fingerprint map identification degree evaluation software, and the results are shown in Table 6.
TABLE 6 evaluation results of GC characteristic spectrum similarity of heat-clearing and phlegm-eliminating traditional Chinese medicine
6 Condition optimization and discussion
6.1 investigation of extraction solvent: the experimental investigation shows that the chromatographic peak is obviously less than that of ethyl acetate and diethyl ether when the water-saturated n-butanol is extracted, which is not beneficial to the overall condition characterization of the sample, and the chromatographic peaks of ethyl acetate and diethyl ether are equivalent in number, and the ethyl acetate is finally selected as the extraction solvent in the experiment considering the safety and control performance of the diethyl ether reagent, and the chromatogram of the extraction solvent is 12-14.
6.2 investigation of the column: the test comparatively investigates three capillary chromatographic columns with the same specification, namely HP-5, DB-17 and DB-WAX, but with different stationary phases, and as a result, the separation effect of the HP-5 chromatographic column and the DB-17 chromatographic column is poor, so that most chromatographic peaks are concentrated at a retention time section, and the comprehensive characterization of characteristic spectrums is not facilitated. And (4) integrating the resolution, retention time distribution and resolution of each chromatographic peak, so that a DB-WAX chromatographic column is selected, and the chromatogram of the DB-WAX chromatographic column is shown in 15-17.
6.3 inspection of temperature raising program and flow dividing ratio: the temperature programming and the flow splitting ratio of three groups of chromatographic columns are examined in the test (see table 7 below), and the results show that under the condition of the test group 1, the chromatographic peak separation is more than 1.5, the peak shapes are sharp and symmetrical, the retention time distribution of 14 common characteristic peaks is relatively average, the separation degree of the partial peak is less than 1.5 under the condition of the test group 2, all the characteristic peaks have front edges and the separation degree of the partial peak is less than 1.5 under the condition of the test group 3, and the chromatogram is 18-20.
The above description is only for the specific embodiments of the present disclosure, but the scope of the present disclosure is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present disclosure, and all the changes or substitutions should be covered within the scope of the present disclosure. Therefore, the protection scope of the present disclosure shall be subject to the protection scope of the claims.
Claims (8)
1. A construction method of a feature map of a traditional Chinese medicine for clearing heat and eliminating phlegm is characterized by comprising the following steps:
step one preparation of reference solution: accurately weighing a proper amount of 6-methoxyguaiacol reference substance, and preparing 0.03mg/mL solution per 1mL by using methanol to obtain a reference substance solution;
step two, preparation of a test solution: precisely measuring 30ml of heat-clearing and phlegm-eliminating traditional Chinese medicine, extracting with ethyl acetate for 3 times, each time extracting with 30ml, mixing ethyl acetate solutions, spin-drying at low temperature, dissolving the residue with methanol, and metering to 5ml to obtain a test solution;
step three-color spectrum condition determination: precisely sucking 1 mul of reference substance solution and sample solution respectively, injecting into a gas chromatograph at a split ratio of 50:1, heating in a specific manner, and recording 36min chromatogram to obtain GC characteristic maps of the traditional Chinese medicine for clearing heat and eliminating phlegm;
step four, constructing a contrast characteristic spectrum of the traditional Chinese medicine for clearing heat and eliminating phlegm: taking thirteen batches of heat-clearing and phlegm-eliminating traditional Chinese medicine samples, respectively preparing the test solution according to the preparation method of the test solution in the first step, determining according to chromatographic conditions in the third step to obtain chromatograms of the thirteen batches of samples, respectively introducing the chromatograms into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, shearing a solvent peak for 0-2min, carrying out multi-point correction on 14 peaks, adopting Mark peak matching, adopting traditional Chinese medicine chromatogram fingerprint similarity evaluation software to compare 13 batches of characteristic spectra, determining common characteristic peaks, and generating a comparison characteristic spectrum consisting of fourteen common peaks.
2. The method for constructing the feature map of the heat-clearing and phlegm-eliminating traditional Chinese medicine according to claim 1, wherein DB-WAX is adopted as a chromatographic column in the third step, N2 is adopted as a carrier gas, the flow rate of the column is 3.5ml/min, and the temperature of a sample inlet is 250 ℃; the FID detector temperature was 280 ℃.
3. The method for constructing the feature map of the heat-clearing and phlegm-eliminating traditional Chinese medicine according to claim 1, wherein the specific manner of temperature rise in the third step is as follows: the initial temperature is 75 ℃, the temperature is increased to 150 ℃ at the temperature increasing rate of 5 ℃/min, and the temperature is kept at 150 ℃ for 0.5 min; heating to 210 deg.C at a heating rate of 3 deg.C/min, maintaining the temperature at 210 deg.C for 0.5min, and operating at 260 deg.C for 5 min.
4. The method for constructing the characteristic spectrum of the heat-clearing and phlegm-resolving traditional Chinese medicine according to claim 1, wherein the control characteristic spectrum of the heat-clearing and phlegm-resolving traditional Chinese medicine constructed in the step four is further used for performing a precision test, a stability test and a repeatability test on a sample of the heat-clearing and phlegm-resolving traditional Chinese medicine, respectively.
5. The method for constructing the feature map of the heat-clearing and phlegm-eliminating traditional Chinese medicine according to claim 4, wherein the precision test comprises the following steps: taking a heat-clearing and phlegm-eliminating traditional Chinese medicine sample, preparing a test solution according to the test solution preparation method in the step two, continuously injecting samples for 6 times, and measuring chromatographic conditions according to the step three; and calculating the RSD of the relative retention time of each characteristic peak and the reference peak by taking the No. 7 peak as the reference peak.
6. The method for constructing the characteristic spectrum of the heat-clearing and phlegm-eliminating traditional Chinese medicine according to claim 4, wherein the stability test comprises the following steps: taking the traditional Chinese medicine sample for clearing heat and eliminating phlegm, preparing the sample solution according to the preparation method of the sample solution in the step two, performing chromatographic condition determination according to the step three at 0, 4, 8, 12, 16 and 24 hours respectively, and calculating the RSD of the relative retention time of each characteristic peak and the reference peak by taking the No. 7 peak as the reference peak.
7. The method for constructing the characteristic map of the heat-clearing and phlegm-eliminating traditional Chinese medicine and the characteristic map thereof as claimed in claim 4, wherein the steps of the repeatability test are as follows: taking the same batch of heat-clearing and phlegm-eliminating traditional Chinese medicines, preparing 6 parts of test solution in parallel according to the step two, carrying out chromatographic condition determination in the step three, taking the No. 7 peak as a reference peak, and calculating the RSD of the relative retention time of each characteristic peak and the reference peak.
8. A feature map of a heat-clearing and phlegm-resolving traditional Chinese medicine, which is constructed by using the construction method of the feature map of the heat-clearing and phlegm-resolving traditional Chinese medicine according to any one of claims 1 to 7.
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