CN112444588A - Fingerprint spectrum detection method for quality of Xiaojin capsules, Xiaojin pills or Xiaojin tablets - Google Patents
Fingerprint spectrum detection method for quality of Xiaojin capsules, Xiaojin pills or Xiaojin tablets Download PDFInfo
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- CN112444588A CN112444588A CN201910794336.2A CN201910794336A CN112444588A CN 112444588 A CN112444588 A CN 112444588A CN 201910794336 A CN201910794336 A CN 201910794336A CN 112444588 A CN112444588 A CN 112444588A
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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
- G01N30/8686—Fingerprinting, e.g. without prior knowledge of the sample components
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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
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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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/74—Optical detectors
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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
- G01N30/8624—Detection of slopes or peaks; baseline correction
- G01N30/8631—Peaks
- G01N30/8634—Peak quality criteria
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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
- G01N30/14—Preparation by elimination of some components
- G01N2030/146—Preparation by elimination of some components using membranes
Abstract
The invention relates to an HPLC fingerprint detection method and a standard fingerprint of a Xiaojin capsule/pill/tablet, wherein the detection method comprises the following steps: (1) preparation of a test solution: extracting XIAOJIN Capsule/pill/tablet with organic solvent, and filtering the extractive solution with microporous membrane to obtain test solution; (2) preparation of a reference solution: respectively preparing 11 carbonyl-beta-acetyl boswellic acid reference substance solutions; (3) the determination method comprises the following steps: measuring by high performance liquid chromatography; (4) establishing standard fingerprint spectrum, comparing with single medicinal material, and performing single medicinal material decoction piece source attribution on to Xiaojin capsule/pill/tablet standard fingerprint spectrum to verify the obtained standard fingerprint spectrum. By comparing the similarity degree of the fingerprint spectrum of the sample to be detected and the standard fingerprint spectrum, the method is beneficial to various enterprises to better control the feeding and track the product quality and is also beneficial to quality inspection departments to monitor the quality of the small gold capsules/pills/tablets.
Description
Technical Field
The invention relates to the technical field of detection of traditional Chinese medicine preparations, in particular to a detection method of an HPLC fingerprint of a Xiaojin capsule/pill/tablet, a standard fingerprint thereof and attribution of HPLC standard fingerprint chromatographic peaks of the Xiaojin capsule/pill/tablet in single medicinal materials.
Background
The Xiaojin capsule, the Xiaojin pill and the Xiaojin tablet are prepared from ten medicinal materials of musk or artificial musk, cochinchina momordica seed, prepared kusnezoff monkshood root, resina Liquidambaris, vinegar frankincense, vinegar myrrh, trogopterus dung, wine angelica, earthworm and Chinese ink according to the same proportion. The first part of the "Chinese pharmacopoeia" 2015 edition is: the capsule is prepared by pulverizing semen Momordicae (hulled and deoiled) 50g, radix Aconiti Kusnezoffii Preparata 50g, resina Liquidambaris 50g, Olibanum 25g, Myrrha 25g, Oletum Trogopterori (processed with vinegar) 50g, radix Angelicae sinensis 25g, Pheretima 50g, and Chinese ink 4g into fine powder, sieving, mixing, adding appropriate amount of starch, granulating, adding Moschus or artificial Moschus 10g, mixing, and making into capsule (1000 granules); the Xiaojin pill is prepared by pulverizing semen Momordicae (hulled and deoiled) 150g, radix Aconiti Kusnezoffii Preparata 150g, resina Liquidambaris 150g, Olibanum 75g, Myrrha 75g, Oletum Trogopterori (processed with vinegar) 150g, radix Angelicae sinensis 75g, Lumbricus 150g, and Chinese ink 12g into fine powder, adding Moschus or artificial Moschus 30g, mixing, sieving, adding starch 25g per 100g powder, mixing, adding starch 5g into diluted paste, making pill, and drying at low temperature; the small gold tablet is prepared by pulverizing radix Aconiti Kusnezoffii Preparata 75g, resina Liquidambaris 75g, Olibanum 37.5g, Myrrha 37.5g, radix Angelicae sinensis 37.5g, Pheretima 75g, and fructus Citri Limoniae 6g into fine powder, pulverizing semen Momordicae (hulled and deoiled) 75g into coarse powder, soaking in 70% ethanol as solvent for 48 hr, slowly percolating, recovering ethanol from percolate, and concentrating to obtain extract with relative density of 1.06-1.10(50 deg.C). Decocting Oletum Trogopterori (parched with vinegar) 75g with water for three times, each for 1 hr, filtering, mixing filtrates, and concentrating to obtain extract with relative density of 1.06-1.10(50 deg.C). Mixing the above two extracts, concentrating to obtain extract with relative density of 1.20-1.25(50 deg.C), mixing with the above fine powder, drying at low temperature, pulverizing, sieving, making into paste with appropriate amount of starch, granulating, drying, adding ground Moschus or artificial Moschus 15g, mixing, and making into 1000 tablets.
Xiaojin capsules/pills/tablets have the functions of resolving masses, relieving swelling, removing blood stasis and relieving pain, and are mainly used for treating cold-dampness, phlegm stasis, and obstruction of channels and collaterals, subcutaneous nodule, scrofula, mammary cancer and nodules of breast. Xiaojin capsules/pills/tablets have obvious clinical curative effect, are very popular with ancient and modern doctors, are widely used for treating diseases of mammary glands, thyroid glands and prostate, and are the first-choice Chinese patent medicine for clinically treating hyperplasia of mammary glands at present.
The existing standard is only one of 'Chinese pharmacopoeia' 2015 edition, the quality of kusnezoff monkshood root and musk or artificial musk in the Xiaojin capsules/pills/tablets is controlled by adopting a diester alkaloid limit (TLC method) and a musk ketone content measurement (GC method) in the standard, a plurality of medicinal materials lack effective control indexes, the evaluation method has single index, and the quality of the Xiaojin capsules/pills/tablets cannot be comprehensively and fully evaluated.
At present, the quality of Xiaojin capsules/pills/tablets is controlled by fingerprint spectrum, and no patent publication and literature report is found at home and abroad.
Disclosure of Invention
The invention aims to provide an HPLC fingerprint detection method of Xiaojin capsules/pills/tablets and a standard fingerprint thereof. Wherein the determination method comprises the following steps: (1) preparation of a test solution: extracting XIAOJIN Capsule/pill/tablet with organic solvent, and filtering the extractive solution with microporous membrane to obtain test solution; (2) preparation of a reference solution: respectively preparing 11 carbonyl-beta-acetyl boswellic acid reference substance solutions; (3) the determination method comprises the following steps: measuring by high performance liquid chromatography; (4) establishing a standard fingerprint spectrum: the fingerprint spectra of some batches of samples obtained are fit to a standard fingerprint spectrum by adopting a traditional Chinese medicine chromatogram fingerprint spectrum similarity evaluation system 2004A edition. According to the steps, the standard fingerprint spectrum of the Xiaojin capsule/pill/tablet with 24 common peaks is obtained, and the sources of the 19 common peaks are assigned by comparing with single medicinal materials. By comparing the similarity between the fingerprint of the sample to be detected and the standard fingerprint, the quality of the small gold capsules/pills/tablets can be reflected, which is beneficial for enterprises to better control the feeding and track the product quality and is also beneficial for quality control departments to monitor the quality of the small gold capsules/pills/tablets.
The invention provides a method for establishing HPLC (high performance liquid chromatography) fingerprint spectrums of Xiaojin capsules/pills/tablets, which comprises the following steps of:
(1) chromatographic conditions and applicability test: symmetry C18(250mm × 4.6mm, 5 μm), acetonitrile as mobile phase A, and 0.10% phosphoric acid aqueous solution by volume fraction as mobile phase B; the detection wavelength is 240 nm; the flow rate is 1. mL/min; column temperature: 30 ℃; sample introduction amount: 10 mu L of the solution; the theoretical plate number is more than 4000 according to the peak of 11 carbonyl-beta-acetyl boswellic acid. The elution gradient was:
| time (min) | Mobile phase A (%) | Mobile phase B (%) |
| 0-40 | 12％→98％ | 88％→2％ |
| 40-55 | 98％→98％ | 2％→2％ |
(2) Preparation of a test solution: taking a proper amount of sample, grinding, adding an organic solvent, weighing, carrying out ultrasonic treatment, cooling, weighing again, complementing the weight loss by the organic solvent, shaking up, and filtering by a membrane to obtain a filtrate which is the sample solution.
(3) Preparation of control solutions: precisely weighing 11 carbonyl-beta-acetyl boswellic acid, and adding an organic solvent to prepare a reference substance solution with a certain concentration.
(4) Establishing an HPLC standard fingerprint;
(5) methodological tests were performed, which included the following:
1) attribution of a standard fingerprint chromatogram peak;
2) testing the stability of the tested solution;
3) testing the precision of the instrument;
4) and (5) performing repeatability test.
(6) And (3) sample determination: precisely absorbing 10 mu L of sample solution to be tested according to chromatographic conditions, injecting the sample solution into a liquid chromatograph, recording a chromatogram for 55 minutes, wherein the chromatogram of the test sample is basically consistent with the standard fingerprint, calculating the similarity between the chromatogram of the test sample and the standard fingerprint by utilizing a traditional Chinese medicine chromatogram fingerprint similarity evaluation system 2004A edition, and evaluating the quality of the test sample according to the similarity calculation result.
The invention has the beneficial effects that:
the HPLC standard fingerprint of Xiaojin capsules/pills/tablets is established based on high performance liquid chromatography, the chromatographic method established in the invention has good reproducibility and is simple and convenient to operate, and common peaks in the standard fingerprint are subjected to single medicinal material source attribution. By comparing the similarity degree of the fingerprint obtained by the sample to be detected and the standard fingerprint, the quality of the small gold capsules/pills/tablets can be reflected, which is beneficial to each enterprise to better control the feeding and track the product quality and is also beneficial to quality inspection departments to monitor the quality of the small gold capsules/pills/tablets.
Drawings
FIG. 1 shows the standard fingerprint of Xiaojin capsule/pill/tablet (24 common peaks in 1-24, 11 carbonyl-beta-acetyl boswellic acid in 17);
FIG. 2 is a chromatogram of S7 batches of Xiaojin capsule sample and Moschus, semen Momordicae, radix Aconiti Kusnezoffii, resina Liquidambaris, Olibanum, Myrrha, Oletum Trogopterori, radix Angelicae sinensis, Lumbricus, and XIANGMO medicinal materials from company A;
FIG. 3 is an overlay of HPLC fingerprints of 44 batches of Xiaojin capsules/pills from 8 companies A-G.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples in order to describe the invention in more detail.
Embodiment 1a fingerprint detection method and standard fingerprint establishment for xiaojin capsules/pills/tablets include the following steps:
1 Instrument and reagent
1.1 instruments
Waters Alliance high performance liquid chromatograph (2695 gradient pump, 2998 diode array detector, autosampler, column thermostating system, Empower chromatographic workstation), 1/10 ten thousand electronic analytical balances (model XS105, METTLER), sonicator (model KQ5200 DE).
1.2 reagent
11 carbonyl-beta-acetyl boswellic acid (China institute for drug and biological products, batch No. 786-9001). Acetonitrile and phosphoric acid reagents are pure chromatographies, water is ultrapure water, and other reagents are analytically pure; the small gold capsule sample is provided by A-G company, and the batch number is shown in Table 1;
TABLE 1 Xiaojin Capsule test sample batch number of A-G company
2 methods and results
2.1 chromatographic conditions and System suitability test: symmetry C18(250mm × 4.6mm, 5 μm), acetonitrile as mobile phase A, and 0.10% phosphoric acid aqueous solution by volume fraction as mobile phase B; the detection wavelength is 240 nm; the flow rate is 1.0 mL/min; column temperature: 30 ℃; sample introduction amount: 10 mu L of the solution; the theoretical plate number is more than 4000 according to the peak of 11 carbonyl-beta-acetyl boswellic acid. The elution gradient was:
TABLE 2 gradient elution Table
2.2 preparation of test solution: taking a proper amount of sample, grinding, taking 2g, precisely weighing, placing in a conical flask with a plug, adding 25mL of methanol, weighing, ultrasonically treating (power 300W, frequency 40Hz, and water temperature controlled below 30 ℃) for 35min, cooling, weighing again, supplementing the weight loss with methanol, shaking uniformly, and filtering with a microporous filter membrane (0.45 mu m), wherein the filtrate is the sample solution.
2.3 preparation of control solutions: precisely weighing 11 carbonyl-beta-acetyl boswellic acid, and adding methanol to obtain a reference solution containing 2.01mg11 carbonyl-beta-acetyl boswellic acid per 1mL methanol.
2.4 establishment of HPLC standard fingerprint: at present, the number of Xiaojin capsules which are approved by the State food and drug administration is only A, E, samples of company A are extracted from a large number of batches in the sampling, 15 batches are total, the market share is large, the similarity of the extracted 15 samples is 0.954-0.999, the quality of the samples of the company A is stable, and therefore the standard fingerprint spectrum is generated by fitting the samples of the company A from 15 batches. The establishing process comprises the following steps: measuring HPLC fingerprints of 15 batches of Xiaojin capsules of A company, analyzing and comparing the obtained fingerprints by software of a traditional Chinese medicine chromatogram fingerprint similarity evaluation system 2004A edition, and fitting to generate the HPLC standard fingerprints of the Xiaojin capsules/pills/tablets. The HPLC standard fingerprint of Xiaojin capsules/pills/tablets has 24 common peaks (see figure 1).
2.5 methodological test
2.5.1 Standard fingerprint chromatogram Peak affiliation
Preparing a sample solution from S7 batches of Xiaojin capsules of A company, artificial musk, cochinchina momordica seed, prepared kusnezoff monkshood root, resina liquidambaris, vinegar frankincense, vinegar myrrh, trogopterus dung, wine angelica, earthworm and Chinese ink medicinal materials according to a preparation method of the sample solution of 2.2, analyzing the sample solution according to 2.1 chromatographic conditions, comparing obtained chromatograms, attributing chromatographic peaks by combining spectral data, wherein the chromatograms are shown in figure 2, and the attribution results of the chromatographic peaks are shown in table 3:
TABLE 3 chromatogram peak attribution table of standard fingerprint of small gold capsule
2.5.2 precision test
Taking S7 samples of company A, preparing a sample solution according to a preparation method of the sample solution of 2.2, continuously injecting samples for 6 times, taking a No. 17 peak chromatographic peak corresponding to 11 carbonyl-beta-acetyl boswellic acid as a reference peak, and calculating the relative retention time of the No. 1-24 common peak and the RSD value of the relative peak area to be less than 4.2%. The measured chromatogram data is introduced into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system 2004A edition, and is calculated by software, the average similarity between the sample spectrum and the standard fingerprint measured 6 times is 1.000, the RSD is 0.00% (n is 6), and the test shows that the instrument precision of the method is good in table 4.
TABLE 4 results of precision test
| 1 | 2 | 3 | 4 | 5 | 6 | RSD | |
| Degree of similarity | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 0.00％ |
2.5.3 stability test
Taking S7 samples of company A, preparing a sample solution according to a preparation method of the sample solution of 2.2, injecting samples at time points of 0, 2, 4, 6, 8, 12, 24, 36 and 48h respectively, taking a No. 17 peak chromatographic peak corresponding to 11 carbonyl-beta-acetyl boswellic acid as a reference peak, and calculating the relative retention time of the No. 1-24 common peak and the RSD value of the relative peak area to be less than 6.4%. The measured chromatogram data is introduced into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system 2004A edition, and is calculated by software, the average similarity of the sample chromatogram and the standard fingerprint is 1.000 after 9 times of measurement results, the RSD is 0.00% (n is 9), and the test shows that the stability of the sample solution is good within 48 hours as shown in Table 5.
TABLE 5 stability test results
| 0 | 2 | 4 | 6 | 8 | 12 | 24 | 36 | 48 | RSD | |
| Degree of similarity | 1.000 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 1.000 | 1.000 | 1.000 | 0.00％ |
2.5.4 reproducibility test
Taking S7 samples of company A, weighing 1 part on the first day, 1 part on the second day and 6 parts on the third day, preparing a sample solution according to a preparation method of 2.2 sample solution, injecting samples respectively, and calculating the relative retention time of 1-24 common peaks and the RSD value of the relative peak area to be less than 6.0% by taking the No. 17 peak chromatographic peak corresponding to 11 carbonyl-beta-acetyl boswellic acid as a reference peak. The measured chromatogram data is introduced into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system 2004A edition, and is calculated by software, the average similarity between the chromatogram of the test sample and the standard fingerprint is 0.998, the RSD is 0.00% (n is 8) after 8 times of measurement, and the test shows that the reproducibility of the method is good as shown in Table 6. TABLE 6 stability test results
| 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | RSD | |
| Degree of similarity | 0.983 | 1.000 | 1.000 | 1.000 | 1.000 | 0.999 | 1.000 | 1.000 | 0.00％ |
2.6 sample determination
Precisely absorbing 10 mu L of sample solution to be detected according to chromatographic conditions, injecting the sample solution into a liquid chromatograph, and recording a chromatogram map for 55 minutes. Fingerprint spectrums of 44 batches of Xiaojin capsules/pills/tablets of different batches of numbers of different manufacturers are measured, an overlay image of 44 batches of samples is shown in figure 3, and the similarity between the obtained chromatogram of the test sample and the standard fingerprint is calculated by utilizing a traditional Chinese medicine chromatogram fingerprint similarity evaluation system 2004A edition. The similarity difference of the samples of each manufacturer is large, so the similarity between the fingerprint of the qualified sample and the standard fingerprint is temporarily determined to be not less than 0.70, the calculation results of the similarity between the fingerprint of the 44 batches of samples and the standard fingerprint are summarized, and the qualification rate is shown in table 7.
TABLE 7 summary of similarity between manufacturers
The invention can efficiently detect the characteristic peaks of musk, sweetgum resin, myrrh and trogopterus dung in the Xiaojin capsules/pills/tablets. Comparing with single medicinal material, and performing single medicinal material decoction piece source attribution on to Xiaojin capsule/pill/tablet standard fingerprint to verify the obtained standard fingerprint. By comparing the similarity between the fingerprint of the sample to be detected and the standard fingerprint, the quality of the small gold capsules/pills/tablets can be reflected, which is beneficial for enterprises to better control the feeding and track the product quality and is also beneficial for quality control departments to monitor the quality of the small gold capsules/pills/tablets.
Claims (7)
1. The fingerprint detection method for the quality of Xiaojin capsules, Xiaojin pills or Xiaojin tablets is characterized in that the method and the establishment of the standard fingerprint comprise the following steps:
1) preparation of a test solution: precisely weighing a sample of Xiaojin capsule, Xiaojin pill or Xiaojin tablet, grinding the sample into fine powder, dissolving the fine powder in an organic solvent, weighing, carrying out ultrasonic treatment, cooling, weighing again, complementing the weight loss by the organic solvent, shaking up, filtering by a membrane, and taking the filtrate as a test solution;
2) preparation of control solutions: weighing 11 carbonyl-beta-acetyl boswellic acid, and adding an organic solvent to prepare a reference solution containing 1.0-3.0 mg of 11 carbonyl-beta-acetyl boswellic acid per 1 mL;
3) chromatographic conditions and applicability test: performing gradient elution on a reversed-phase chromatographic column by taking acetonitrile as a mobile phase A and a phosphoric acid aqueous solution as a mobile phase B;
4) establishing an HPLC standard fingerprint: analyzing and comparing more than 2 (preferably more than 5) samples of the same manufacturer in different batches of the Xiaojin capsules, Xiaojin pills or Xiaojin tablets to be tested according to the chromatographic conditions in the step 3), inputting the obtained chromatographic fingerprint into a Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition for analysis, wherein more than 90% of samples of the same manufacturer have the similarity of not less than 0.9, and more than 2 (preferably more than 5) samples of the manufacturer with the similarity of not less than 0.9 are selected to generate the standard fingerprint of the Xiaojin capsules, Xiaojin pills or Xiaojin tablets;
5) and (3) verification of methodology: preparing a sample solution according to the step 1), preparing a reference solution according to the step 2), analyzing the sample solution according to the step 3), verifying the precision of an instrument, the stability and the repeatability of the sample solution, and calculating the relative retention time of other chromatographic peaks and the Relative Standard Deviation (RSD) of the relative peak area by taking the peak corresponding to the 11 carbonyl-beta-acetyl boswellic acid as a reference peak, wherein the RSD is not more than 6.5%;
6) and (3) sample determination: preparing a sample to be tested from a Xiaojin capsule, a Xiaojin pill or a Xiaojin tablet according to the step 1) to prepare a sample solution, analyzing the sample solution according to the step 3), inputting the obtained chromatographic fingerprint and a standard fingerprint into a Chinese medicine chromatographic fingerprint similarity evaluation system 2004A edition for analysis, wherein the similarity between the test sample and the standard fingerprint is not less than (more than or equal to) 0.7, and the sample to be tested is qualified; if the value is less than 0.7, the sample to be tested is determined to be unqualified.
2. The method of claim 1, wherein the organic solvent of the sample solution of step 1) is one or more of methanol, ethanol, acetonitrile, and acetone.
3. The method of claim 1, wherein the organic solvent of the control solution of step 2) is one or more of methanol, ethanol, acetonitrile, and acetone.
4. The method of claim 1, wherein the mobile phase B is 0.01-0.20% phosphoric acid aqueous solution by volume fraction in the method of step 3).
5. The method of claim 1, wherein in step 4), the chromatographic column is one of Symmetry C8/C18, Waters-acchmm tncure C8/C18, symmetryshird RP 1; the column temperature is 20-40 ℃; the flow rate is 1.0-1.5 mL/min; the detection wavelength is 240 nm.
6. The method according to claim 1, 4 or 5, wherein the elution is performed by a gradient elution, preferably by a gradient elution method comprising:
。
7. The application of the HPLC standard fingerprint obtained by the method of claims 1-6 in the detection of Xiaojin capsules, Xiaojin pills or Xiaojin tablets can calibrate the attribution of HPLC standard fingerprint chromatographic peaks in single medicinal materials and can fully and fully evaluate the quality of the Xiaojin capsules, the Xiaojin pills or the Xiaojin tablets.
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