CN115290805A - Finger print method and content detection method for radix Pteris Multifidae medicinal material - Google Patents
Finger print method and content detection method for radix Pteris Multifidae medicinal material Download PDFInfo
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- 238000001514 detection method Methods 0.000 title claims abstract description 46
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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Abstract
The invention provides a finger print method and a content detection method for a Pteris multifida medicinal material. The invention also establishes the contents of 4 index components of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside, the content detection method has good precision, stability and reproducibility, and can be used in the application links of quality component detection, authenticity identification, quality control of medicinal materials, production place processing of medicinal materials and the like of the aizoon stonecrop herb, thus providing a new quality detection method for the quality stability of the medicinal materials, ensuring the safety and effectiveness of the clinical use of the medicinal materials and the like.
Description
Technical Field
The invention relates to a fingerprint method and a content detection method for a radix pteridis multifidae medicinal material, and belongs to the field of Chinese medicinal material quality detection methods.
Background
The Pteris multifida, also known as Pteris multifida, pteris phoenix, rhodiola sachalinensis and Rhodiola crenulata, is a rooted whole plant of Rhodiola crenulata Rhodiola dumulosa (Franch.) S.H.Fu of Crassulaceae. The Pteris multifida is one of the medicinal materials in the territorial province of Shanxi, is mainly distributed on hillside rocks with the elevation of 1600-4100 m and in stone gaps in Taibai mountain areas of Qinling mountains, is a natural and precious medicinal plant, is called as plateau ginseng and Xueshan Mesona, is also a medicinal plant commonly used in folk, and is called as 'lao-kuan-hao-chu, and can not leave Phoenix phoenix grass'. The Pteris multifida has remarkable effects of resisting oxidation, inhibiting bacteria, resisting fatigue and resisting anoxia, and total flavonoids of Pteris multifida are main active substances for exerting pharmacological effects. The pteris multifida is reported to contain flavonoid compounds, volatile components, polysaccharide, various amino acids and trace elements.
Modern pharmacological studies show that the effect of the rhodiola sachalinensis is similar to that of the rhodiola rosea, but whether the rhodiola sachalinensis can be substituted by the rhodiola rosea needs to further define the overall quality attribute of the rhodiola sachalinensis. However, the existing research is stopped at the determination of the total flavonoids and 4 flavonoid components of the gynura bicolor, no research report about the fingerprint and the determination of more other component contents is found, and the whole quality of the gynura bicolor medicinal material cannot be fully reflected. The traditional Chinese medicine chromatographic fingerprint can comprehensively reflect the overall characteristics of the chemical components of the traditional Chinese medicine, and is an effective method for evaluating the authenticity, quality, consistency and stability of the traditional Chinese medicine. The method combines a multi-index component quantitative method with a fingerprint map, can provide qualitative and quantitative information of the traditional Chinese medicine at the same time, and is an effective quality control method of the traditional Chinese medicine. In addition, the Principal Component Analysis (PCA) technology can effectively reduce the dimension of the multidimensional information of the traditional Chinese medicine fingerprint, so that the quality difference of the traditional Chinese medicine is more real and vividly presented. Aiming at the problems of uneven quality and single quality detection index of the Pteris multifida medicinal material, the inherent quality difference of the medicinal material is large. Therefore, it is necessary to develop a detection method capable of simultaneously detecting a plurality of intrinsic efficacy index components.
Disclosure of Invention
The invention provides a finger print method and a content detection method for a Pteris multifida medicinal material.
The fingerprint detection method of the invention also combines PCA to analyze the difference of the common peak, and screens out 2 main difference components: gallic acid and rutin, which can affect the quality uniformity of the rhizoma paridis. The finger prints of the Pteris multifida medicinal materials are established, and the similarity of the finger prints of 10 batches of Pteris multifida medicinal materials is greater than 0.993. The invention also establishes the content of 4 index components of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside, the content detection method has good precision, stability and reproducibility, can be used for the application links of quality component detection, authenticity identification, quality control of medicinal materials, production place processing of medicinal materials and the like of the aizoon stonecrop herb, provides a new quality detection method for the quality stability of the medicinal materials and the safety and effectiveness of the clinical use of the medicinal materials.
The technical scheme provided by the invention is as follows:
a finger print detection method for a Pteris multifida medicinal material comprises the following steps:
preparing a reference substance solution: weighing a reference substance of the glyphosate, the rutin, the kaempferol-7-O-rhamnoside and the gallic acid, adding methanol for dissolving and fixing the volume to obtain a reference substance stock solution, and diluting each reference substance stock solution by using methanol until the concentration is 20-40 mu g/mL to obtain the composition;
preparing a test solution: weighing the powder of the root of common Pteris, diluting with 60-90% methanol by a dilution factor of 40-80 times, performing ultrasonic treatment, standing at room temperature, shaking up, filtering, and taking a subsequent filtrate to obtain the final product;
the chromatographic conditions are as follows: by C 18 A chromatographic column; gradient elution with methanol (A) and 0.08-0.12% phosphoric acid aqueous solution (B) as mobile phase, elution procedure of 0-15 min, 20-33% A, 15-30 min,33% A, 30-35 min, 33-50% A, 35-60 min, 50-55% A, detection wavelength of 250-280 nm, flow rate of 0.7-1.2 mL/min, column temperature of 25-35 ℃;
fourth, establishing a fingerprint map: the method comprises the steps of mixing control product stock solution, testing sample solution, measuring chromatographic conditions in the third step, carrying out sample injection analysis on multiple batches of the Pteris multifida sample solution, introducing a data file into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, carrying out multi-point correction and Mark peak matching by taking S1 as a reference map, and generating a Pteris multifida medicinal material comparison fingerprint by a median method.
The number represented by the multiple batches is more than or equal to 10 batches.
Preferably, each control product stock solution is diluted to a concentration of 30 μ g/mL in the preparation of the control product solution.
Further preferably, the detection method comprises the step of preparing the test solution, wherein the concentration of the methanol is 75%.
Further preferably, the detection method comprises the following steps of preparing the test solution, wherein the dilution factor of methanol is 60 times.
Preferably, the detection method comprises the steps of preparing a test solution, wherein the ultrasonic treatment time is 10-40 min, the power is 200-400W, and the frequency is 30-50 kHz.
Preferably, the detection method comprises the following steps of preparing a test solution, wherein the ultrasonic treatment time is 30min, the power is 300W, and the frequency is 40 kHz.
Preferably, said C 18 The types of the chromatographic columns are as follows: ultimate LP and Kromasil.
Preferably, the detection method comprises the following steps: the concentration of the phosphoric acid aqueous solution of the mobile phase (B) was 0.1%.
Preferably, the detection method comprises the following steps: the detection wavelength was 274nm, the flow rate was 1.0mL/min, and the column temperature was 30 ℃.
Preferably, the comparison fingerprint generated in the step four of establishing the fingerprint determines 15 total peaks, and the comparison of the comparison products indicates 4 chromatographic peaks, wherein the peak 1 is gallic acid, the peak 8 is rutin, the peak 12 is glyphosate, and the peak 14 is kaempferol-7-O-rhamnoside.
Preferably, the detection method comprises the following steps:
preparing a mixed reference product stock solution: weighing gallic acid, rutin, kaempferol-7-O-rhamnoside reference substances, and making into mixed reference substance stock solution containing gallic acid, rutin, kaempferol-7-O-rhamnoside;
preparing a test solution: the preparation method comprises the steps of claim 1;
the chromatographic detection conditions are as follows: chromatographic conditions under the conditions according to the step of claim 1;
fourthly, measuring the content of the test sample solution: mixing a reference product stock solution, adding a test solution, carrying out sample injection analysis under chromatographic conditions, recording peak areas, and calculating to obtain the contents of gallic acid, rutin, caretin glycoside and kaempferol-7-O-rhamnoside.
Preferably, in the preparation of the mixed control product stock solution, the concentration of gallic acid is 1.97 to 63.00 μ g/mL, the concentration of rutin is 1.96 to 62.75 μ g/mL, the concentration of the glufosinate-glycoside is 8.41 to 269.00 μ g/mL, and the concentration of kaempferol-7-O-rhamnoside is 1.82 to 58.25 μ g/mL.
Preferably, the step three is adopted for detecting the test solution of the radix pteridis multifidae medicinal material under the chromatographic condition, the high performance liquid chromatography peak and the reference fingerprint are generated, and the similarity is calculated to be 0.990-1.000.
In order to embody the innovation of the technical scheme of the invention, the optimized partial experiment processes of the fingerprint spectrum and the content detection chromatogram are organized as follows:
3.1 examination of the preparation method of the test solution
In the experiment, the influence of different extraction solvents (90% methanol, 75% methanol and 60% methanol) and material-liquid ratios (1: 60, 1: 100, 1: 150 and 1: 200 times) on the extraction effect of the sample is examined, and the result shows that the number of chromatographic peaks of the 75% methanol extraction solution is large, and the peak height and the peak area of each chromatographic peak are ideal when the material-liquid ratio is 1: 60. In addition, the influence of different ultrasonic extraction times (30, 45 and 60 min) on the extraction effect is also examined, and as a result, the number of chromatographic peaks and the absorption intensity thereof are not obviously changed along with the increase of the extraction time. Therefore, the ultrasonic extraction is carried out for 30min by taking 75 percent methanol as a solvent and taking the feed-liquid ratio of 1: 60.
3.2 optimization of chromatographic conditions
The experiment focuses on the types and proportions of the mobile phases (methanol-water, methanol-0.1% phosphoric acid, acetonitrile-0.1% phosphoric acid). When the mobile phase is methanol-water, the chromatographic peak is wide and flat and tails; when the mobile phase is acetonitrile-0.1% phosphoric acid, the chromatographic peak is fast, but the separation degree is poor; when the mobile phase is methanol-0.1% phosphoric acid, the baseline is stable, the chromatographic peak shape is better, and the separation degree is better. The target component of gallic acid has strong polarity and fast peak emergence, and the retention time is delayed in order to avoid solvent interference, so that the gallic acid is determined for 0-15 min, and the proportion of a mobile phase is 20-33% of methanol. Since the Pteris multifida contains a large amount of flavonoid compounds with similar polarity, in order to achieve better separation effect of each flavonoid component, the separation time is 35-60 min, and the proportion of a mobile phase is 50-55% of methanol. Finally, after a large amount of experimental groping and proportion adjustment, determining that the mobile phase is methanol-0.1 percent phosphoric acid gradient elution, the optimal elution proportion is 0-15min, and 20-33 percent methanol; 15-30min, 33% methanol; 30-35min, 33-50% of methanol; 35-60min and 50-55% of methanol.
In addition, the invention also provides detection wavelength (274, 327, 346, 360 nm) and chromatographic column [ Ultimate LP-C 18 (250×4.6mm，5μm)、Kromasil C 18 (250×4.6mm，5μm)]The results of investigation revealed that the number of chromatographic peaks at the detection wavelength of 274nm wasMore, better absorption intensity, and better peak shape and resolution of each chromatogram of the Ultimate LP column.
3.3 selection of index Components
The fingerprint contains 4 peaks, such as gallic acid (peak 1), rutin (peak 8), glyphosate (peak 12) and kaempferol-7-O-rhamnoside (peak 14). The PCA result indicates that gallic acid and rutin can be important index components influencing the quality uniformity of different batches of the radix paeoniae alba medicinal material, the kurarinone glycoside is the largest component in the main component, and the kaempferol-7-O-rhamnoside is a stable and controllable flavonoid component with smaller difference among different batches of the medicinal material. Therefore, the 4 ingredients are all brought into the index ingredient for measuring the content of the Chinese brake herb.
The finger print and content detection method for the Pteris multifida medicinal material has the beneficial effects that:
the HPLC fingerprint of 10 batches of medicinal material of the root of Chinese brake herb is established, a large number of experiments are performed by the inventor of the application, the methanol-0.1% phosphoric acid aqueous solution is finally determined as a mobile phase, good separation effect of each characteristic chromatographic peak is obtained, detection and separation are performed at the wavelength of 274nm, 15 common chromatographic peaks are marked, and 4 chromatographic peaks are identified through comparison of reference substances respectively, wherein the peak 1 is gallic acid, the peak 8 is rutin, the peak 12 is glufosinate-glycoside, and the peak 14 is kaempferol-7-O-rhamnoside. The difference of the common peaks is analyzed by combining PCA, and 2 main difference components are screened out: gallic acid and rutin, which affect the quality uniformity of seven batches of phoenix tail. The fingerprint of the phoenix-tail seven medicinal material is established, and the similarity of 10 batches of finger prints of the phoenix-tail seven medicinal material is greater than 0.993. The research result of the invention provides reference for comprehensive quality evaluation and further development and utilization of the Pteris multifida medicinal material.
The invention also establishes the contents of 4 index components of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside, wherein the contents of the gallic acid and the rutin are firstly determined in the research. The content measurement result by methodology shows that: (1) and the precision test result shows that the peak area RSD of the peak areas of the gallic acid, the rutin, the glyphosate and the kaempferol-7-O-rhamnoside is less than or equal to 0.30 percent, which indicates that the precision of the instrument is good. (2) And the standard peak area RSD of the repeatability test result is less than or equal to 2.5 percent, which also indicates that the method has good repeatability. (3) And the stability test result shows that the RSD of each detection index peak area is less than or equal to 1.49 percent, which indicates that the test article is relatively stable when placed at room temperature for 24 hours. (4) The test results of sample application recovery rates show that the average sample application recovery rates of the gallic acid, the rutin, the glyphosate and the kaempferol-7-O-rhamnoside are respectively 99.24%,94.05%,93.50% and 95.15%, and the RSD of the peak area of each detection index is less than or equal to 2.82%, which indicates that the method has good accuracy. The content of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside in 10 batches of the gynura divaricata is respectively 0.2159-0.3901 mg/g, 0.2132-0.3445 mg/g, 3.2214-4.9397 mg/g and 0.3069-0.4458 mg/g. Therefore, the content determination method is stable, accurate and reliable, can be suitable for detecting the quality components of the pteris multifida medicinal material, and has a very wide market application prospect.
According to the invention, 10 batches of the gynura bicolor medicinal material are collected, HPLC is adopted to establish a fingerprint spectrum and a content determination method of the gynura bicolor medicinal material, and PCA is utilized to compare the difference of common components among different samples, so that a reference basis is provided for the systematic evaluation and quality control of the gynura bicolor medicinal material.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Figure 1-10 batch of radix Pteris Multifidae HPLC fingerprint (totally determining 15 total peaks, numbered 1-15 in sequence, wherein peak 1 is gallic acid, peak 8 is rutin, peak 12 is glufosinate-glycoside, and peak 14 is kaempferol-7-O-rhamnoside);
FIG. 2-10 shows the PCA score chart (A) and loading chart (B) of the batch of Pteris multifida medicinal materials;
FIG. 3 is an HPLC chromatogram of the mixed reference substance (A) and the test solution (B) of radix Pteris Multifidae (wherein, in the chromatogram, peak 1-gallic acid, peak 2-rutin, peak 3-glyphosate, and peak 4-kaempferol-7-O-rhamnoside).
Detailed Description
In order to more fully understand the practice of the present invention, an experimental example is set forth below, and the present invention is further illustrated by the following exemplary examples.
Example 1 establishment of finger-print detection method for Pteris multifida medicinal materials
1 Material
1.1 Instrument
Agilent 1260 high performance liquid chromatography system (Agilent corporation); XM-P22H type stepless power-regulating ultrasonic cleaner (Kunshan Xiaomei ultrasonic instruments Co., ltd.); BT25S and BS210S electronic analytical balances (beijing sidoris scientific instruments ltd).
1.2 drugs and reagents
The Pteris multifida is collected from Shanxi Qinling area, meixian county (S1-S5, S9 and S10) and Zhou to Zhou (S6-S8), identified by Yangzhan researchers at Chinese medicine research institute in Shaanxi province, and is rooted whole grass of Rhodiola rosea Rhodiola dumulosa (Franch.) S.H.Fu of Crassulaceae. The control substances of the lignin glycoside (batch number P07D10S 105270), the rutin (batch number A05GB 144263), the kaempferol-7-O-rhamnoside (batch number P18J11S 116104) are purchased from Shanghai leaf Biotech limited, the gallic acid (batch number 110831-200302) is purchased from China pharmaceutical biological product institute, and the purity of all the control substances is more than 98%; acetonitrile was of chromatographic grade (Thermo Fisher Scientific, USA), water was Waaha purified water, and other reagents were analytically pure.
2 methods and results
2.1 finger-print research of Pteris multifida medicinal materials
2.1.1 chromatographic conditions
Using Ultimate LP-C 18 (4.6X 250mm,5 μm) chromatography column; gradient elution with methanol (A) and 0.1% phosphoric acid water solution (B) as mobile phase, 0-15min as elution program, 20-33% by weight A; 15-30min, 33% A; 30-35min, 33% -50% A; 35-60min, 50-55 percent A; the detection wavelength is 274nm; the flow rate is 1.0mL/min; the column temperature is 30 ℃; the sample size was 10. Mu.L.
2.1.2 preparation of control solutions
Precisely weighing appropriate amount of the control substances of the glyphosate, the rutin, the kaempferol-7-O-rhamnoside and the gallic acid, respectively putting the control substances into 10mL measuring bottles, adding methanol for dissolving and fixing the volume to obtain a control substance stock solution; and diluting each control stock solution with methanol to a suitable concentration of about 30 μ g/mL to obtain each control solution.
2.1.3 preparation of test solutions
Precisely weighing 0.5g of Pteris multifida powder, adding 30mL of 75% methanol, performing ultrasonic treatment for 30min (power 300W and frequency 40 kHz), standing at room temperature, shaking up, filtering with 0.45 μm microporous membrane, and collecting the filtrate.
2.1.4 precision test
Taking the same sample solution (S9), continuously injecting samples for 6 times under the chromatographic condition of the item of 2.1.1, taking the glyphosate (peak 12) as a reference peak, and respectively calculating the RSD of the relative retention time of each common peak to be 0.01-0.08 percent and the RSD of the relative peak area to be 0.19-2.09 percent, thereby showing that the precision of the instrument is good.
2.1.5 repeatability test
Taking the same batch of Pteris multifida medicinal material powder (S9), preparing 6 parts of test solution in parallel by the method under the item 2.1.3, respectively injecting samples under the chromatographic condition under the item 2.1.1, respectively taking the pravastatin (No. 12 peak) as a reference peak, respectively calculating the RSD of the relative retention time of each common peak to be 0.01-0.21%, and the RSD of the relative peak area to be 1.08-2.98%, thus indicating that the method has good repeatability.
2.1.6 stability test
Taking the same sample solution (S9), respectively standing for 0,2,4,8, 12 and 24 hours at room temperature according to the chromatographic condition under the item of 2.1.1, and respectively measuring by taking the pravastatin (peak 12) as a reference peak, respectively calculating the RSD of the relative retention time of all the common peaks to be 0.01-0.10% and the RSD of the relative peak area to be 1.13-2.97%, which indicates that the sample is stable when standing for 24 hours at room temperature.
2.1.7 establishment of fingerprint and analysis of similarity
According to the chromatographic conditions under the item of '2.1.1', 10 batches of test solution of the Pteris multifida Lindl are subjected to sample injection analysis, a data file is converted into an 'AIA' format, and the data file is introduced into a 'traditional Chinese medicine chromatographic fingerprint similarity evaluation system (2012 edition)'. Taking S1 as a reference spectrum, setting the width of a time window to be 0.1, performing multi-point correction and Mark peak matching, generating a reference fingerprint by a median method, and showing an HPLC fingerprint superposition graph and a reference graph of 10 batches of the Pteris multifida medicinal materials in figure 1. Calculating the similarity between the S1-S10 sample and the reference fingerprint spectrum to be 0.995, 0.997, 0.998, 1.000,
1.000, 0.994, 0.993, 0.996, 0.999 and 0.999, which indicates that the quality of the pteris multifida medicinal materials of different batches is stable.
2.1.8 assignment of common Peak
The established 10 batches of Pteris multifida fingerprint spectra totally determine 15 peaks (the area ratio is more than 92 percent) and are numbered 1-15 in sequence. Comparing with reference substance, identifying 4 chromatographic peaks respectively, wherein peak 1 is gallic acid, peak 8 is rutin, peak 12 is glyphosate, and peak 14 is kaempferol-7-O-rhamnoside.
2.2 Principal Component Analysis (PCA)
Introducing 15 common peak areas of 10 batches of the Pteris multifida medicinal materials into SIMCA-P14.1 software, and drawing a PCA score chart and a factor load chart. The results are shown in fig. 2A, wherein 10 batches of samples are located in a 95% confidence interval, the variance contribution rates of 2 principal components are 63.8% and 20.5%, respectively, and the cumulative contribution rate is 84.3%, which indicates that the two principal components can better reflect the quality characteristics of the samples. As can be seen from fig. 2B, peak 12 (glyphosate) is the largest component of the sample; the 15 common peaks are greatly deviated on the main component 1; the peak 1, the peak 2, the peak 3, the peak 4, the peak 8, the peak 9 and the peak 10 have a larger dispersion degree on the main component 2, and particularly have a larger contribution due to the difference of the peak 1 (gallic acid), the peak 2 and the peak 8 (rutin), which suggests that the 3 components may be important index components influencing the quality uniformity of the phoenix tail seven medicinal materials in different batches.
Example 2 content determination of 4 index components in the Pteris multifida medicinal material
2.3.1 chromatographic conditions
The chromatographic detection conditions are as in the section "2.1.1" in the examples of the present invention.
2.3.2 preparation of stock solutions of Mixed controls
Precisely sucking appropriate amount of reference substance stock solutions of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside prepared under the item of '2.1.2', placing in an EP tube, vortex and mixing uniformly to obtain mixed reference substance stock solution containing gallic acid 63.00 μ g/mL, rutin 62.75 μ g/mL, glyphosate 269.00 μ g/mL and kaempferol-7-O-rhamnoside 58.25 μ g/mL.
2.3.3 preparation of test solutions
The same procedure was followed as in example 1 under "2.1.3".
2.3.4 Linear relationship
The mixed reference stock solution prepared under item "2.2.2" was diluted stepwise with 75% (v/v) methanol to 6 different appropriate concentrations, analyzed by sample injection under the chromatographic conditions of item "2.1.1", and the chromatogram and the peak areas of each chromatogram were recorded. And respectively taking the mass concentration of the index components as a horizontal coordinate (X) and the peak area as a vertical coordinate (Y), constructing a standard curve, and calculating a regression equation, wherein the linear relation of the 4 index components is shown in table 1.
Table 1 linear regression analysis of 4 components.
2.3.5 precision test
Taking the same mixed reference substance solution, continuously injecting sample for 6 times under the chromatographic condition of the item of 2.1.1, measuring peak areas, and calculating the peak areas RSD of the gallic acid, the rutin, the kaempferol glycoside and the kaempferol-7-O-rhamnoside to be 0.20%, 0.29%, 0.30% and 0.13% respectively, which indicates that the precision of the instrument is good.
2.3.6 repeatability test
Taking the same batch of the gynura divaricata medicinal material powder (S9), preparing 6 parts of test solution in parallel according to the method under the item of 2.1.3, carrying out sample injection analysis under the chromatographic condition under the item of 2.1.1, calculating to obtain the average contents of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside which are respectively 0.2304, 0.3191, 4.6713 and 0.4486mg/g, and RSD which is respectively 2.1%, 2.7%, 1.7% and 2.5%, thereby indicating that the method has good repeatability.
2.3.7 stability test
Taking the same part of test solution (S9), respectively standing at room temperature for 0,2,4,8, 12 and 24 hours according to the chromatographic condition under the term of '2.1.1', and respectively measuring, wherein RSD of peak areas of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside are calculated to be 1.06%, 1.49%, 0.95% and 0.97%, which indicates that the test solution is stable when standing at room temperature for 24 hours.
2.3.8 sample recovery test
Accurately weighing 0.5g (S9) of the pteris multifida medicinal material powder with known content of the component to be detected, adding 6 parts, respectively adding a certain amount of corresponding reference substance solution according to the level of 100%, preparing a sample solution according to the method under the item '2.1.3', carrying out sample injection analysis under the chromatographic condition under the item '2.1.1', recording peak areas, and calculating the average sample injection recovery rates of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside to be 99.24%,94.05%,93.50% and 95.15%, and RSD to be 2.82%,2.45%,2.56% and 2.58%, respectively, thereby indicating that the method has good accuracy. The specific results are shown in Table 2.
TABLE 2 sample recovery of 4 components (n = 6)
2.3.9 sample assay
Taking 0.5g of each of 10 batches of the medicinal material powder of the root of Chinese brake herb, precisely weighing, preparing a sample solution according to the method under the item of 2.1.3, carrying out sample injection analysis under the chromatographic condition under the item of 2.1.1, recording peak areas, calculating to obtain the contents of gallic acid, rutin, glyphosate and kaempferol-7-O-rhamnoside which are respectively 0.2159-0.3901 mg/g, 0.2132-0.3445 mg/g, 3.2214-4.9397 mg/g and 0.3069-0.4458 mg/g, and mixing a reference substance and the sample HPLC chromatogram map shown in the attached figure 3 of the specification, wherein the specific measurement result is shown in the table 3.
TABLE 3 determination of the content of 4 ingredients in 10 batches of Pteris multifida medicinal materials (mg/g, n = 3)
Finally, it should be noted that: the present invention is not intended to be limited to the embodiments shown above, which are intended to be illustrative, instructive, and not restrictive. Those skilled in the art, having the benefit of this disclosure, will appreciate that various modifications, equivalents, and improvements may be made without departing from the spirit and scope of the invention.
Claims (10)
1. A finger print detection method for a Pteris multifida medicinal material is characterized by comprising the following steps:
preparing a reference substance solution: weighing the control substances of the glyphosate, the rutin, the kaempferol-7-O-rhamnoside and the gallic acid, adding methanol for dissolving and fixing the volume to be used as a control substance stock solution, and diluting each control substance stock solution by using methanol until the concentration is 20-40 mu g/mL to obtain the composition;
preparing a test solution: weighing the powder of the root of Chinese brake, diluting by adding 60-90% methanol by a dilution factor of 40-80 times, carrying out ultrasonic treatment, standing at room temperature, shaking up, filtering, and taking the subsequent filtrate to obtain the medicine;
the chromatographic conditions are as follows: by C 18 A chromatographic column; the mobile phase is methanol (A) and 0.08 to 0.12 percent phosphoric acid aqueous solution (B) for gradient elution, the elution program is 0 to 15min,20 to 33 percent A,15 to 30min,33 percent A,30 to 35min,33 to 50 percent A,35 to 60min,50 to 55 percent A, the detection wavelength is 250 to 280nm, the flow rate is 0.7 to 1.2mL/min, and the column temperature is 25 to 35 ℃;
fourthly, establishing a fingerprint map: the method comprises the steps of mixing control product stock solutions, preparing a test solution, measuring chromatographic conditions under the steps of three, carrying out sample injection analysis on multiple batches of test solutions of the pteris multifida, introducing a data file into a traditional Chinese medicine chromatographic fingerprint similarity evaluation system, carrying out multi-point correction and Mark peak matching by taking S1 as a reference map, and generating a pteris multifida control fingerprint by a median method.
2. The assay of claim 1 wherein the concentration of methanol in the preparation of the test solution is 75%.
3. The detection method according to claim 1, characterized in that the detection method comprises the steps of preparing a test solution, wherein the ultrasonic treatment time is 10-40 min, the power is 200-400W, and the frequency is 30-50 kHz.
4. The assay of claim 1, wherein the assay step and the chromatographic assay conditions are: said C is 18 The types of the chromatographic columns are as follows: ultimate LP and Kromasil.
5. The assay of claim 1, wherein the assay comprises the following steps: the concentration of the mobile phase (B) phosphoric acid aqueous solution was 0.1%.
6. The assay of claim 1, wherein the assay comprises the following steps: the detection wavelength was 274nm, the flow rate was 1.0mL/min, and the column temperature was 30 ℃.
7. The detection method as claimed in claim 1, wherein the step four establishes a comparison fingerprint, a total of 15 peaks are determined, and 4 chromatographic peaks are identified through comparison of comparison products, wherein the peak 1 is gallic acid, the peak 8 is rutin, the peak 12 is glyphosate, and the peak 14 is kaempferol-7-O-rhamnoside.
8. A detection method for the content of a Pteris multifida medicinal material is characterized by comprising the following steps:
preparing a hybrid reference substance reserve liquid: weighing reference substance stock solutions of gallic acid, rutin, kaempferol-7-O-rhamnoside, and making into mixed reference substance stock solution containing gallic acid, rutin, kaempferol-7-O-rhamnoside;
preparing a test solution: the preparation method comprises the steps of claim 1;
the chromatographic detection conditions are as follows: according to the step of claim 1;
fourth, measuring the content of the test sample solution: mixing a reference product stock solution, adding a test solution, carrying out sample injection analysis under chromatographic conditions, recording peak areas, and calculating to obtain the contents of gallic acid, rutin, caretin glycoside and kaempferol-7-O-rhamnoside.
9. The content detection method according to claim 8, characterized in that in the preparation of the mixed control product stock solution, the concentration of gallic acid is 1.97 to 63.00 μ g/mL, the concentration of rutin is 1.96 to 62.75 μ g/mL, the concentration of the glufosinate glycoside is 8.41 to 269.00 μ g/mL, and the concentration of kaempferol-7-O-rhamnoside is 1.82 to 58.25 μ g/mL.
10. The detection method of claim 1, wherein the step three is adopted for detecting the test solution of the Pteris multifida medicinal material under the chromatographic condition, a high performance liquid chromatography peak and a reference fingerprint are generated, and the similarity is calculated to be 0.990-1.000.
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