CN116165300A - Fingerprint construction method of Xiangsha Weiling pill and fingerprint thereof - Google Patents
Fingerprint construction method of Xiangsha Weiling pill and fingerprint thereof Download PDFInfo
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- CN116165300A CN116165300A CN202310158430.5A CN202310158430A CN116165300A CN 116165300 A CN116165300 A CN 116165300A CN 202310158430 A CN202310158430 A CN 202310158430A CN 116165300 A CN116165300 A CN 116165300A
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- 239000006187 pill Substances 0.000 title claims abstract description 65
- 238000010276 construction Methods 0.000 title claims abstract description 24
- VVOAZFWZEDHOOU-UHFFFAOYSA-N magnolol Chemical compound OC1=CC=C(CC=C)C=C1C1=CC(CC=C)=CC=C1O VVOAZFWZEDHOOU-UHFFFAOYSA-N 0.000 claims abstract description 45
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- QUQPHWDTPGMPEX-UHFFFAOYSA-N Hesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(COC4C(C(O)C(O)C(C)O4)O)O3)O)=CC(O)=C2C(=O)C1 QUQPHWDTPGMPEX-UHFFFAOYSA-N 0.000 claims abstract description 18
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- ARGKVCXINMKCAZ-UHFFFAOYSA-N neohesperidine Natural products C1=C(O)C(OC)=CC=C1C1OC2=CC(OC3C(C(O)C(O)C(CO)O3)OC3C(C(O)C(O)C(C)O3)O)=CC(O)=C2C(=O)C1 ARGKVCXINMKCAZ-UHFFFAOYSA-N 0.000 claims abstract description 18
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- 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
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- G—PHYSICS
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- 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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- 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
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- 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
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- G01N30/28—Control of physical parameters of the fluid carrier
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- 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
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- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
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Abstract
The invention relates to the field of medicines, in particular to a fingerprint construction method of a Xiangsha Weiling pill and a fingerprint thereof. The invention provides a fingerprint construction method of a Xiangsha Weiling pill and a fingerprint chromatogram thereof, and the method can effectively characterize the quality of the Xiangsha Weiling pill, thereby being beneficial to comprehensively monitoring the stability, consistency and controllability of the quality of products. The invention has the characteristics of convenience, rapidness, stability, high precision and good repeatability, and can evaluate the quality of the Xiangsha Weiling pill more comprehensively, objectively and scientifically, thereby guaranteeing the effectiveness of the Xiangsha Weiling pill in treatment. The fingerprint constructed by the invention has 14 peaks, wherein three components of hesperidin, magnolol and honokiol can be calibrated, and the fingerprint can comprehensively represent the quality of products.
Description
Technical field: the invention relates to a quality control method of a traditional Chinese medicine preparation, in particular to a fingerprint construction method of a Xiangsha Weiling pill and a fingerprint thereof.
Background
The invention relates to a Xiangsha Weiling pill which is prepared from 11 traditional Chinese medicines of costustoot, fructus amomi, rhizoma atractylodis stir-baked with bran, cortex magnoliae officinalis with ginger, rhizoma atractylodis stir-baked with bran, dried orange peel, poria cocos, rhizoma alismatis, polyporus, cinnamon and liquorice, has the effects of dispelling dampness and activating spleen, and promoting qi circulation and regulating stomach, and is used for treating symptoms such as vomiting, diarrhea, edema, dizziness, dysuria and the like caused by internal water-dampness. The XIANGSHAWEILING pill is a unique stomach medicine, has definite therapeutic effect and high market acceptance.
The quality of the traditional Chinese medicine is closely related to clinical curative effect, and it is extremely important to establish a traditional Chinese medicine quality control method and ensure the consistency of the curative effect of the product. The fingerprint spectrum of the traditional Chinese medicine is a comprehensive and quantifiable chromatographic identification means, is established on the basis of the research of the chemical components of the traditional Chinese medicine, and can identify the uniformity and the stability of the quality of the finished product. The traditional Chinese medicine preparation has complex components, and the method for integrally describing and evaluating the traditional Chinese medicine preparation is very suitable and urgently needed by establishing the method for comprehensively reflecting the types and the amounts of chemical components contained in the traditional Chinese medicine preparation.
The current quality standard only comprises 3 content detection indexes of hesperidin, magnolol and honokiol in total. The Xiangsha Weiling pill is composed of 11 traditional Chinese medicines, and has more chemical components and quantity, so that the internal quality of the pill is difficult to control comprehensively, and the whole substance group of the pill is required to be controlled. Therefore, besides microscopic analysis, the method of macroscopic analysis should be used to effectively characterize the quality of the traditional Chinese medicine as a whole. Fingerprint spectrum is used as the quality control method of Chinese herbal medicine and its preparation, and is now common knowledge of industry personnel. Up to now, no fingerprint of the Xiangsha Weiling pill is reported in the literature. The invention adopts an HPLC analysis method to construct a fingerprint detection method and a fingerprint of the Xiangsha Weiling pill, and identifies the determined components to perform more comprehensive quality control.
Disclosure of Invention
In view of the above, the invention aims to provide a fingerprint construction method of a Xiangsha Weiling pill and a fingerprint thereof. The method has high stability, high accuracy and high repeatability, can be used for monitoring the production process of the Xiangsha Weiling pills, provides a certain theoretical basis and support for the construction of a whole process quality control system, and ensures the safety and effectiveness of clinical medication.
The invention provides a fingerprint construction method of a Xiangsha Weiling pill, which comprises the following specific steps:
(1) Preparation of test solution: grinding a sample of the Xiangsha Weiling pill, precisely weighing, placing the sample into a conical bottle with a plug, precisely adding a certain amount of methanol solution respectively, sealing, weighing, performing ultrasonic treatment for a certain time, taking out, cooling, weighing again, supplementing the lost weight with a certain amount of methanol solution, shaking uniformly, filtering, and taking a subsequent filtrate to obtain a sample solution;
(2) Preparation of a control solution: taking a proper amount of hesperidin reference substance, precisely weighing, and adding methanol to prepare a reference substance solution with a certain concentration; taking magnolol reference substance and a proper amount of honokiol reference substance, precisely weighing, and adding methanol to prepare a mixed reference substance solution containing 0.1mg of each 1 ml;
(3) The measuring method comprises the following steps: precisely sucking the reference substance solution and the sample solution, injecting into a high performance liquid chromatograph combined with an ultraviolet detector, measuring, and recording a chromatogram;
(4) And (3) introducing the obtained fingerprint data of the Xiangsha Weiling pills into a traditional Chinese medicine fingerprint similarity evaluation system (2012 edition) for similarity evaluation.
The fingerprint construction method of the xiangsha Weiling pill provided by the invention is characterized in that the preparation of the sample solution in the step (1) comprises the following specific operation processes: grinding a sample of the Xiangsha Weiling pill, precisely weighing 0.5g, placing the sample into a conical bottle with a plug, precisely adding 25mL of methanol, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 60 minutes, taking out, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate to obtain a sample solution.
The fingerprint spectrum construction method of the xiangsha Weiling pill provided by the invention is characterized in that the specific operation process for preparing the reference substance solution in the step (2) is as follows: taking a proper amount of hesperidin reference substance, precisely weighing, and adding methanol to prepare a reference substance solution with a certain concentration; taking magnolol reference substance and appropriate amount of honokiol reference substance, precisely weighing, and adding methanol to obtain mixed reference substance solution containing 0.1mg of honokiol reference substance per 1 mL.
The fingerprint construction method of the xiangsha Weiling pill provided by the invention is characterized in that the specific operation process of the measurement method in the step (3) is as follows: precisely sucking 10 μl of reference solution and sample solution, respectively, and injecting into high performance liquid chromatograph combined with ultraviolet detector for measurement, wherein the time for recording the chromatogram is 70min.
The fingerprint spectrum construction method of the Xiangsha Weiling pill of the invention preferably comprises the following chromatographic conditions in the fingerprint spectrum measurement of the Xiangsha Weiling pill in the step (3): octadecylsilane chemically bonded silica is used as a filler; acetonitrile as mobile phase a,0.1% formic acid as mobile phase B, gradient elution procedure: 0-7 min, 5-10% (A); 7-24 min, 10-20% (A); 24-34 min, 20-35% (A); 34-38 min, 35-43 percent (A); 38-41 min, 43-54.5% (A); 41-43 min, 54.5-60% (A); 43-62 min, 60-70 percent (A); 62-70 min,70% (A); column temperature is 30 ℃; flow rate 1.0mL per minute; the detection wavelength was 280nm.
The fingerprint construction method of the invention is that the specification of the chromatographic column is preferably Shimadzu ODS-C18,5 μm,250mm multiplied by 4.6mm.
The batches for measuring the fingerprint spectrum of the traditional Chinese medicine are generally 10-30 batches.
The relative retention time of 14 characteristic peaks and peak 7 in the fingerprint obtained by the XIANGSHAWEILING pill under the condition of ultraviolet detector wavelength of 280nm is as follows: peak 1:0.228; peak 2:0.293; peak 3:0.500; peak 4:0.617; peak 5:0.743; peak 6:0.961; peak 8:0.1.138; peak 9:1.431; peak 10:1.500; peak 11:1.585; peak 12:1.695; peak 13:1.865; peak 14:2.064; wherein peak 7 is hesperidin, peak 11 is honokiol, and peak 13 is magnolol.
The invention provides a quality detection method of a Xiangsha Weiling pill, which is characterized in that a fingerprint of the Xiangsha Weiling pill is obtained according to the construction method, and similarity evaluation is carried out on the fingerprint of a sample to be detected and the fingerprint of the Xiangsha Weiling pill, wherein the similarity is not lower than 0.90 and is a qualified product.
The invention provides a fingerprint detection method and a fingerprint of a finished product of a Xiangsha Weiling pill, and the quality of the Xiangsha Weiling pill can be comprehensively controlled by the method, so that the quality stability, consistency and controllability of the Xiangsha Weiling pill are better ensured, and the safety and effectiveness of the Xiangsha Weiling pill are ensured.
The fingerprint constructed by the invention has 14 peaks, wherein three components of hesperidin, magnolol and honokiol can be calibrated, and the fingerprint can comprehensively represent the quality of products.
In the technical fingerprint research scheme of the invention, the inventor of the application finds out through a large number of experiments that the preparation step (1) and the detection method step (3) of the sample solution are correspondingly optimized, and a quality detection method with reliable stability and simple and convenient operation is obtained. In order to show the innovation of the technical scheme of the invention, the preferred partial screening scheme in the project research technology is provided as follows.
1 preparation of sample solution
The test is carried out on the preparation of the sample solution of the Xiangsha Weiling pill in the step (1) by ultrasonic treatment for 60 minutes and heat reflux treatment for 60 minutes, wherein the extraction solvents are 30% methanol, 50% methanol, 80% methanol, 100% methanol, 30% ethanol, 50% ethanol, 80% ethanol and 100% ethanol, and the extraction time is 30 minutes and 60 minutes.
The results show that: the total peak area of the ultrasonic extraction and the reflux extraction target peak is not greatly different; when methanol is used as an extraction solvent, the total area of the common peaks is higher, the peak separation effect is better, and the base line is also smoother; when the ultrasonic time is 30 minutes, the total peak area of the target peak is slightly lower.
Therefore, the preparation method of the preferred test sample comprises the following steps: grinding a sample of the Xiangsha Weiling pill, precisely weighing 0.5g, placing the sample into a conical bottle with a plug, precisely adding 25mL of methanol, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 60 minutes, taking out, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate to obtain a sample solution.
2 screening of chromatographic conditions in the fingerprint of the present invention
2.1 Mobile phase chromatography Condition optimization
The experiment of the invention is carried out on the mobile phase in the chromatographic condition of the step (3), acetonitrile-0.1% formic acid and acetonitrile-0.1% phosphoric acid. As a result, the peak area and the peak separation effect of each component are considered, and finally, it is preferable that: acetonitrile-0.1% formic acid for separation research of XIANGSHAWEILING pill.
2.2 Mobile phase gradient investigation
Acetonitrile-0.1% formic acid is taken as a mobile phase system, the chromatographic peak performance, the separation effect and the retention time of each component are considered, and the final preferred gradient elution program is as follows: 0-7 min, 5-10% (A); 7-24 min, 10-20% (A); 24-34 min, 20-35% (A); 34-38 min, 35-43 percent (A); 38-41 min, 43-54.5% (A); 41-43 min, 54.5-60% (A); 43-62 min, 60-70 percent (A); 62-70 min,70% (A).
2.3 selection of detection wavelength
Further, the detection wavelength in the step (3) is optimized, a DAD detector is adopted for detection, a spectrogram is inspected at the wavelength of 190-400 nm, and comparison analysis is carried out, so that the detection wavelength is 280nm, the chromatographic information is rich, the baseline is stable, and the detection wavelength of 280nm is optimized for comprehensive consideration in order to more comprehensively evaluate the quality of the Xiangsha Weiling pill by the chromatographic method.
2.4 investigation of chromatographic columns
Two different manufacturers of C18 columns were examined, namely Shimadzu ODS (250 mm. Times.4.6 mm. 5 μm) and Agilent C18 (4.6 mm. Times.250 mm. 5 μm). The results show that the performance of the chromatographic peak of the Shimadzu ODS chromatographic column is better, and the final preference is that: ODS (250 mm. Times.4.6mm.5 μm) was subjected to separation studies of XIANGSHAWEILING pill.
2.5 investigation of column temperature
Sample injection analysis was examined at 25℃and 30℃and 35℃respectively. As a result, the peak area and the peak separation effect of each component were combined, and detection was carried out by comprehensively considering the preferable column temperature of 30 ℃.
2.6 selection of flow Rate
The flow rate of 0.8mL per minute, 1.0mL per minute, and 1.2mL per minute were examined for sample analysis, respectively. As a result, the peak area, peak separation effect and baseline smoothness of each component were combined, and the final preferable flow rate was 1.0mL per minute.
The beneficial effects of the detection method of the invention are as follows:
(1) According to the invention, through HPLC optimization, an HPLC fingerprint of the Chinese medicinal preparation of the Xiangsha Weiling pill is established, and the fingerprint marks 14 common peaks at 280nm, namely 3 chromatographic peaks.
(2) The preferred HPLC chromatographic method allows simultaneous evaluation of 14 components under the same chromatographic conditions and verification by the method. The result of the precision test shows that the relative retention time and the relative peak area RSD value of each common peak in the chromatogram of the sample solution are less than 3%, which indicates that the instrument precision is good. Stability tests show that the relative retention time and the relative peak area RSD value of each common peak in the measured chromatograms are less than 3%, and the stability of the test sample solution is good within 24 hours. The repeatability test shows that the relative retention time and the relative peak area RSD value of each common peak in the measured chromatogram are less than 3%, which shows that the method has good repeatability. The detection result shows that the fingerprint detection method is stable, reliable, good in repeatability and stable in index component. Can meet the requirements of fingerprint spectrum technology and quality control of preparation. Can provide reference for quality control of XIANGSHAWEILING pill.
(3) According to the high performance liquid phase detection result of 15 batches, S1 is taken as a reference chromatograph, the similarity between 15 batches of samples is over 0.90, and the quality control regulations of the fingerprint are met.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 shows 15 batch fingerprint spectra superimposed at 280nm
FIG. 2 shows a high performance liquid chromatogram of a sample solution of XIANGSHAWEILING pill, wherein peak 7 is hesperidin, peak 11 is honokiol, and peak 13 is magnolol
FIG. 3 shows a control solution chromatogram
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.
Detailed Description
The invention discloses a fingerprint construction method and a fingerprint of a Xiangsha Weiling pill, and a person skilled in the art can refer to the content of the text and properly improve the parameter implementation. It is expressly noted that all such similar substitutions and modifications will be apparent to those skilled in the art, and are deemed to be included in the present invention. While the methods and applications of this invention have been described in terms of preferred embodiments, it will be apparent to those skilled in the relevant art that variations and modifications can be made in the methods and applications described herein, and in the practice and application of the techniques of this invention, without departing from the spirit or scope of the invention.
In order that the invention may be more fully understood, a more particular description of the invention will be rendered by reference to the following examples.
Example 1 method for detecting fingerprint of XIANGSHAWEILING pill
1.1 instruments and reagents
Ultimate3000 high performance liquid chromatograph (Dynam, USA); ME204E electronic balance (Metrele Tolyduo instruments (Shanghai Co.); AB135-S electronic balance (mertrel-tolido instruments (Shanghai); SB-1200D ultrasonic cleaner (Ningbo Xinzhi biotechnology Co., ltd.). Methanol, formic acid (analytically pure) (from beijing chemical plant); chromatographic methanol, chromatographic acetonitrile (Fisher, usa); the water was purified water (baby haha group limited).
1.2 materials
Hesperidin (lot number: 110710-201821), magnolol (lot number: 110729-202015), and honokiol (110730-201915), all purchased from chinese pharmaceutical and food institute; xiangsha Weiling pill 15 batch (lot numbers 180601, 180602, 180603, 180604, 180605, 180606, 180607, 180608, 180609, 180611, 180705, 180714, 180715, 181002, 181107), specification: each 15 grains had a weight of 1g.
1.3 preparation of test solutions: grinding a sample of the Xiangsha Weiling pill, precisely weighing 0.5g, placing the sample into a conical bottle with a plug, precisely adding 25mL of methanol, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 60 minutes, taking out, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate to obtain a sample solution.
1.4 preparation of control solution: precisely weighing a proper amount of hesperidin reference substance, and adding methanol to prepare a reference substance solution containing 0.40mg of hesperidin per 1 mL; taking magnolol reference substance and appropriate amount of honokiol reference substance, precisely weighing, and adding methanol to obtain mixed reference substance solution containing 0.1mg of honokiol reference substance per 1 mL.
1.5 liquid chromatography conditions: octadecylsilane chemically bonded silica is used as a filler; acetonitrile as mobile phase a,0.1% formic acid as mobile phase B, gradient elution procedure: 0-7 min, 5-10% (A); 7-24 min, 10-20% (A); 24-34 min, 20-35% (A); 34-38 min, 35-43 percent (A); 38-41 min, 43-54.5% (A); 41-43 min, 54.5-60% (A); 43-62 min, 60-70 percent (A); 62-70 min,70% (A); column temperature is 30 ℃; flow rate 1.0mL per minute; the detection wavelength was 280nm.
2 methodological verification
2.1 precision
Taking batch 2 (S2) of the Xiangsha Weiling pills, preparing a sample solution according to a method of preparing a 1.3 sample, continuously injecting the sample solution for 6 times under a 1.5 liquid chromatography condition, and calculating the relative retention time and relative peak area RSD value of each common peak in a chromatogram by taking a No. 7 peak (hesperidin) as a reference. The results are shown in tables 1 and 2.
TABLE 1 results of precision experiments relative retention time
TABLE 2 results of precision test relative peak area
As a result, the relative retention time and relative peak area RSD of each common peak were less than 3%, which indicates that the instrument precision was good.
2.2 stability
Taking batch 2 (S2) of the Xiangsha Weiling pills, preparing a sample solution according to a method of preparing a 1.3 sample, sampling for 0, 2, 4, 6, 8, 10, 12 and 24 hours under a 1.5 liquid chromatography condition, and calculating the relative retention time and relative peak area RSD value of each common peak in a chromatogram by taking a No. 7 peak (hesperidin) as a reference. The results are shown in tables 3 and 4.
TABLE 3 stability test relative retention time results
TABLE 4 stability test relative peak area results
As a result, the relative retention time of each common peak and the relative peak area RSD were less than 3%, indicating that the test sample solution had good stability within 24 hours.
2.3 repeatability
Taking batch 3 (S3) of the fragrant sand stomach poria cocos pills, preparing 6 parts of sample solution according to a method of preparing a 1.3 sample, injecting sample under a 1.5 liquid chromatography condition, and calculating relative retention time and relative peak area RSD value of each common peak in a chromatogram by taking a No. 7 peak (hesperidin) as a reference. The results are shown in tables 5 and 6.
TABLE 5 relative retention time results of repeatability tests
TABLE 6 relative peak area results of repeatability test
As a result, the retention time of each common peak and the relative peak area RSD were less than 3%, indicating good reproducibility of the method.
2.4 construction of finger print and identification of chromatographic peaks
According to the preparation method of the 1.3 test product, 15 batches of test product solutions of the XIANGSHAWEILING pill are prepared, sample injection analysis is carried out under the condition of 1.5 liquid chromatography, a traditional Chinese medicine fingerprint similarity evaluation system (2012 edition) is introduced, and automatic matching of different batches of chromatograms is carried out, wherein the results are shown in figures 1 and 2. As can be seen from the drawings of the specification, the fingerprint marks 14 common peaks at 280nm, and 3 chromatographic peaks are identified. Peak 7 is hesperidin, peak 11 is honokiol, and peak 13 is magnolol.
2.5 similarity evaluation
And (3) establishing a common mode for 15 batches of the spectrum of the Xiangsha Weiling pills by using an S1 as a reference chromatograph and adopting a median method, and comparing each fingerprint with a reference fingerprint to obtain the similarity of each fingerprint and the reference fingerprint, wherein the analysis result is shown in Table 7. The similarity of the fingerprints of the 15 batches of the Xiangsha Weiling pills is good and is above 0.90, and the requirements are met.
Table 715 fingerprint similarity results of pill of Sha-Wei-Ling
Claims (8)
1. The fingerprint construction method of the Xiangsha Weiling pill is characterized by comprising the following steps:
(1) Preparation of test solution: grinding a sample of the Xiangsha Weiling pill, precisely weighing, placing the sample into a conical bottle with a plug, precisely adding a certain amount of methanol solution respectively, sealing, weighing, performing ultrasonic treatment for a certain time, taking out, cooling, weighing again, supplementing the lost weight with a certain amount of methanol solution, shaking uniformly, filtering, and taking a subsequent filtrate to obtain a sample solution;
(2) Preparation of a control solution: taking a proper amount of hesperidin reference substance, precisely weighing, and adding methanol to prepare a reference substance solution with a certain concentration; taking magnolol reference substance and a proper amount of honokiol reference substance, precisely weighing, and adding methanol to prepare a mixed reference substance solution with a certain concentration;
(3) The measuring method comprises the following steps: precisely sucking the reference substance solution and the sample solution, injecting into a high performance liquid chromatograph combined with an ultraviolet detector, measuring, and recording a chromatogram;
(4) And (3) introducing the obtained fingerprint data of the Xiangsha Weiling pills into a traditional Chinese medicine fingerprint similarity evaluation system (2012 edition) for similarity evaluation.
2. The fingerprint spectrum construction method as set forth in claim 1, wherein the preparation method of the sample solution is as follows: grinding a sample of the Xiangsha Weiling pill, precisely weighing 0.5g, placing the sample into a conical bottle with a plug, precisely adding 25mL of methanol, sealing, weighing, performing ultrasonic treatment (power 600W, frequency 40 kHz) for 60 minutes, taking out, cooling, weighing again, supplementing the lost weight with methanol, shaking uniformly, filtering, and taking a subsequent filtrate.
3. The fingerprint spectrum construction method as set forth in claim 1, wherein the preparation method of the reference substance solution is as follows: accurately weighing appropriate amount of hesperidin reference substance, and adding methanol to obtain reference substance solution with certain concentration; taking magnolol reference substance and appropriate amount of honokiol reference substance, precisely weighing, and adding methanol to obtain mixed reference substance solution containing 0.1mg of honokiol reference substance per 1 ml.
4. The fingerprint construction method of claim 1, wherein the time for recording the chromatogram in the step (3) is 70min.
5. The fingerprint construction method according to claim 1, wherein chromatographic conditions for fingerprint measurement of the xiangsha weiling pill are: octadecylsilane chemically bonded silica is used as a filler; acetonitrile as mobile phase a,0.1% formic acid as mobile phase B, gradient elution procedure: 0-7 min, 5-10% (A); 7-24 min, 10-20% (A); 24-34 min, 20-35% (A); 34-38 min, 35-43 percent (A); 38-41 min, 43-54.5% (A); 41-43 min, 54.5-60% (A); 43-62 min, 60-70 percent (A); 62-70 min,70% (A); column temperature is 30 ℃; flow rate 1.0mL per minute; the detection wavelength was 280nm.
6. The fingerprint construction method of claim 1, wherein,
(1) Preparation of test solution: grinding the stomach poria cocos pills with the fragrance sand in different batches, precisely weighing, placing the pills in a conical bottle with a plug, precisely adding a certain amount of methanol solution respectively, sealing, weighing, performing ultrasonic treatment (with the power of 600W and the frequency of 40 kHz) for 60 minutes, taking out, cooling, weighing again, supplementing the lost weight with a certain amount of methanol solution, shaking uniformly, filtering, and taking a subsequent filtrate to obtain a sample solution;
(2) Preparation of a control solution: taking a proper amount of hesperidin reference substance, precisely weighing, and adding methanol to prepare a reference substance solution with a certain concentration; taking magnolol reference substance and a proper amount of honokiol reference substance, precisely weighing, and adding methanol to prepare a mixed reference substance solution containing 0.1mg of each 1 ml;
(3) The measuring method comprises the following steps: precisely sucking the reference solution and the sample solution respectively, injecting into high performance liquid chromatograph combined with ultraviolet detector, and measuring for 70min.
(4) The chromatographic conditions of fingerprint measurement of the Xiangsha Weiling pill are as follows: octadecylsilane chemically bonded silica is used as a filler; acetonitrile as mobile phase a,0.1% formic acid as mobile phase B, gradient elution procedure: 0-7 min, 5-10% (A); 7-24 min, 10-20% (A); 24-34 min, 20-35% (A); 34-38 min, 35-43 percent (A); 38-41 min, 43-54.5% (A); 41-43 min, 54.5-60% (A); 43-62 min, 60-70 percent (A); 62-70 min,70% (A); column temperature is 30 ℃; flow rate 1.0mL per minute; the detection wavelength was 280nm. The specification of the chromatographic column is Shimadzu ODS-C18,5 μm,250mm×4.6mm.
7. The fingerprint construction method of a Xiangsha Weiling pill as claimed in claim 6, wherein the relative retention time of 14 characteristic peaks and peak 7 in the fingerprint obtained under the condition of ultraviolet detector wavelength 280nm is as follows: peak 1:0.228; peak 2:0.293; peak 3:0.500; peak 4:0.617; peak 5:0.743; peak 6:0.961; peak 8:0.1.138; peak 9:1.431; peak 10:1.500; peak 11:1.585; peak 12:1.695; peak 13:1.865; peak 14:2.064; wherein peak 7 is hesperidin, peak 11 is honokiol, and peak 13 is magnolol.
8. The method for constructing the fingerprint of the Xiangsha Weiling pill is characterized in that the fingerprint of the Xiangsha Weiling pill is obtained according to the construction method of any one of claims 1 to 7, and the similarity between the fingerprint of a sample to be tested and the fingerprint of the Xiangsha Weiling pill is evaluated, and the similarity is not lower than 0.90 and is a qualified product.
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