CN107589185B - Fingerprint detection method of Mailuotong granules and fingerprint thereof - Google Patents
Fingerprint detection method of Mailuotong granules and fingerprint thereof Download PDFInfo
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Abstract
The invention discloses a vein relaxing granule fingerprint spectrum detection method, which is established by adopting a high performance liquid chromatography, and the chromatographic conditions comprise that: using octadecylsilane chemically bonded silica as a filler, acetonitrile as a mobile phase A, and 0.3 volume percent formic acid aqueous solution as a mobile phase B, and carrying out gradient elution at a flow rate of 0.5-1.5 ml/min < -1 >, a column temperature of 20-35 ℃, and a detection wavelength of 210-360 nm; the theoretical plate number is not less than 3000 calculated according to rutin peak. Experimental verification shows that the detection method disclosed by the invention is good in stability and repeatability, high in analysis speed and high in analysis efficiency, and avoids the singleness and sidedness of quality control in the prior art, so that the quality of the granules for dredging collaterals can be objectively, comprehensively and accurately evaluated, and the detection method has important significance for controlling the quality of the granules for dredging collaterals and ensuring the clinical curative effect. In another aspect, the invention also provides a choroid through particle fingerprint obtained by the choroid through particle fingerprint detection method.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a fingerprint detection method and a fingerprint of Mailuotong granules.
Background
The Mailuotong granule has the functions of benefiting qi, activating blood circulation, removing blood stasis, relieving pain, dredging collaterals and activating collaterals. Is suitable for treating chest pain, chest distress, short breath, headache, vertigo, coronary heart disease, angina pectoris caused by thoracic obstruction, and numbness and hemiplegia caused by apoplexy.
The prescription of Mailuotong granules is from Mailuotong granules from the ministerial standards of traditional Chinese medicine, and is produced and marketed exclusively in 1987. In the prescription of the Mailuotong granules, codonopsis pilosula and angelica are used as monarch drugs, so that qi and blood are benefited; safflower, salvia miltiorrhiza, ligusticum wallichii and earthworm are used as ministerial drugs and auxiliary monarch drugs to achieve the effects of activating blood and dredging collaterals; the hawthorn is an adjuvant drug, and has the effects of promoting qi and blood circulation, activating blood circulation, removing blood stasis and relieving pain; the horsetail, the kudzuvine root and the sophora flower bud are guiding medicines, and can ascend clear and dredge arthralgia, help the medicines to ascend and directly reach the focus. The monarch, minister, assistant and guide medicines are compatible in the whole formula, benefit qi, activate blood, remove blood stasis and relieve pain, and are suitable for patients with coronary heart disease and angina pectoris caused by qi deficiency, blood stasis and heart vessel obstruction.
The traditional Chinese medicine fingerprint refers to a chromatogram or a spectrogram which can mark chemical characteristics of certain traditional Chinese medicinal materials or traditional Chinese medicine preparations by adopting a certain analysis means after the traditional Chinese medicinal materials or the traditional Chinese medicine preparations are properly processed. The traditional Chinese medicine fingerprint spectrum is a comprehensive and quantifiable identification means, is established on the basis of the systematic research of the chemical components of the traditional Chinese medicine, and is mainly used for evaluating the authenticity, the excellence and the stability of the quality of the semi-finished products of the traditional Chinese medicine and the traditional Chinese medicine preparation. "integrity" and "fuzziness" are its distinguishing features. At the present stage, under the condition that most of the effective components of the traditional Chinese medicine are not clear, the traditional Chinese medicine fingerprint has important significance for effectively controlling the quality of the traditional Chinese medicine or the traditional Chinese medicine. The Japanese Han prescription pharmaceutical main production enterprises adopt high performance liquid phase fingerprint to control the quality in the enterprises in 80 s of the 20 th century. The quality control of ginkgo biloba extract by HPLC has also been carried out in Germany and France, and the quality control method of the mixture group by HPLC has also been established in recent years in the United states. With the progress of research, people find that any component contained in traditional Chinese medicines, especially compound traditional Chinese medicines, as practical products of the theory of traditional Chinese medicine cannot represent the whole curative effect of the traditional Chinese medicines. It is gradually recognized that the quality standards of the existing reference chemical medicine quality control modes cannot properly reflect the inherent quality of the traditional Chinese medicine. The trend has been to move from the current quality control model to a comprehensive, macroscopic, quantifiable identification combined with the determination of the content of major active ingredients.
The Mailuotong granule contains 10 medicinal materials, the content of puerarin as the main component is not enough in the current quality standard, and the whole substance group of the puerarin must be controlled. Therefore, besides the micro analysis, a certain macro analysis method is also used for effectively representing the quality of the traditional Chinese medicine on the whole. Therefore, the establishment of a fingerprint detection method of the Mailuotong granules is imperative.
Disclosure of Invention
The invention develops a fingerprint detection method of the granules for dredging collaterals and a fingerprint thereof, and the method can ensure the quality stability, consistency and controllability of the granules for dredging collaterals, thereby ensuring the safety and effectiveness of the granules for dredging collaterals.
The invention aims to provide a fingerprint spectrum detection method of the choroid dredging granules.
A second object of the present invention is to provide a fingerprint for use in a fingerprint detection method of particles for venation.
In an embodiment of the present invention, the present invention provides a method for detecting choroid pass particles by fingerprint, comprising detecting the choroid pass particles by high performance liquid chromatography, wherein the chromatographic conditions comprise:
using octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, and 0.3 vol% formic acid aqueous solution as mobile phase B, and performing gradient elution at flow rate of 0.5-1.5ml·min-1The column temperature is 20-35 ℃, and the detection wavelength is 210-360 nm; the theoretical plate number is not less than 3000 calculated according to rutin peak.
In a preferred embodiment of the present invention, the present invention provides a method for detecting a choroid pass particle by fingerprint, wherein, during the gradient elution process, the ratio of the mobile phase a is changed to: 0-3 min, 5 vol% acetonitrile; 3-50 min, 5-42 vol% acetonitrile; 50-50.1 min, 42-95% acetonitrile by volume; 50.1-60 min, 95 volume percent acetonitrile; i.e. gradient elution procedure as follows:
in a preferred embodiment of the present invention, the present invention provides a method for detecting a choroid pass particle by fingerprint, wherein the chromatographic column using octadecylsilane chemically bonded silica as a filler is phenomenenx luna (2) C18(4.6 × 250mm, 5 um).
In a preferred embodiment of the present invention, the present invention provides a method for detecting a choroid pass particle fingerprint, further comprising the following steps:
(1) preparation of a test solution: 2.0g of Mailuotong granules are taken, precisely weighed, placed in a 100ml conical flask with a plug, precisely added with 25-75 ml of 70 volume percent ethanol, tightly plugged, weighed, ultrasonically treated (250w, 40KHz) for 10-40 minutes, cooled, supplemented with 70 volume percent ethanol to reduce the weight loss, shaken uniformly and filtered, and a subsequent filtrate is taken, thus obtaining the Chinese medicinal preparation;
(2) preparation of control solutions: taking a proper amount of puerarin, rutin, ferulic acid, lobetyolin, salvianolic acid B, quercetin and kaempferide, and adding 70 vol% ethanol to prepare a mixed reference solution containing 112 mu g of puerarin, 204 mu g of rutin, 44 mu g of ferulic acid, 32 mu g of lobetyolin, 92 mu g of salvianolic acid B, 40 mu g of quercetin and 28 mu g of kaempferide in each 1 ml;
(3) and (3) determination: precisely absorbing 2-10 μ l of each of the reference solution and the sample solution, respectively, injecting into a high performance liquid chromatograph, recording chromatogram within 60 minutes, and processing the chromatogram with version 2004A of evaluation System for similarity of traditional Chinese medicine chromatogram fingerprint to obtain fingerprint of MAILUOTONG granule.
In a more preferred embodiment of the present invention, the present invention provides a method for detecting a fingerprint of a choroid pass particle, comprising the steps of:
(1) preparation of a test solution: precisely weighing 2.0g of Mailuotong granules, placing into a 100ml conical flask with a plug, precisely adding 50ml of 70 volume percent ethanol, sealing the plug, weighing, treating with ultrasound (250w, 40KHz) for 20 minutes, cooling, supplementing the lost weight with 70 volume percent ethanol, shaking up, filtering, and taking the subsequent filtrate to obtain the final product;
(2) preparation of control solutions: taking a proper amount of puerarin, rutin, ferulic acid, lobetyolin, salvianolic acid B, quercetin and kaempferide, and adding 70 vol% ethanol to prepare a mixed reference solution containing 112 mu g of puerarin, 204 mu g of rutin, 44 mu g of ferulic acid, 32 mu g of lobetyolin, 92 mu g of salvianolic acid B, 40 mu g of quercetin and 28 mu g of kaempferide in each 1 ml;
(3) and (3) determination: precisely absorbing 5 μ l of each of the reference solution and the sample solution, injecting into a high performance liquid chromatograph, recording chromatogram within 60min, and processing chromatogram with 2004A edition of evaluation System for similarity of traditional Chinese medicine chromatogram fingerprint to obtain fingerprint of MAILUOTONG granule;
here, the chromatographic conditions of the high performance liquid chromatography measurement are: octadecylsilane chemically bonded silica is used as a filling agent; acetonitrile is used as a mobile phase A; taking 0.3% formic acid water solution as mobile phase B; gradient elution with a flow rate of 1.0 ml/min-1(ii) a The column temperature is 25 ℃; the detection wavelength is 270 nm; the theoretical plate number is not less than 3000 calculated according to rutin A peak.
In another aspect, the invention provides a choroid through particle fingerprint obtained by the above fingerprint detection method of choroid through particles, wherein the fingerprint has 21 common peaks.
In a preferred embodiment of the present invention, the present invention provides a choroid pass particle fingerprint spectrum, wherein the spectrum has 21 common peaks, and the retention time of each common peak is respectively as follows: common peak 1: 13.234 min; common peak 2: 15.952 min; common peak 3: 17.602 min; consensus peak 4: 20.612 min; consensus peak 5: 21.099 min; consensus peak 6: 21.321 min; common peak 7: 24.057 min; common peak 8: 27.190 min; consensus peak 9: 28.845 min; common peak 10: 29.452 min; common peak 11: 29.830 min; common peak 12: 30.206 min; consensus peak 13: 33.715 min; consensus peak 14: 34.979 min; consensus peak 15: 37.136 min; common peak 16: 38.789 min; consensus peak 17: 39.278 min; consensus peak 18: 39.610 min; common peak 19: 41.671 min; common peaks 20: 45.049 min; common peak 21: 48.173 min.
The invention has the beneficial effects that:
(1) the vein and vein clearing granule fingerprint established by the method provided by the invention can effectively characterize the quality of vein and vein clearing granules and is beneficial to comprehensively monitoring the quality of the medicine.
(2) The fingerprint emphasizes the front-back sequence and the mutual relation of all the formed fingerprint characteristic peaks and the overall facial features, thereby not only avoiding the one-sidedness of judging the quality of the granules for dredging collaterals due to the measurement of individual chemical components, but also reducing the possibility of manual treatment for reaching the quality standard.
(3) The method has the advantages of simplicity, convenience, stability, high precision and good reproducibility.
In the embodiments of the present invention, "%" is used to indicate volume percent unless otherwise specified.
Drawings
FIG. 1 is an overlay of 14 choroid pass particle fingerprints measured in accordance with the present invention.
Figure 2 is a control profile of choroid pass particle fingerprint measured by the present invention.
FIG. 3 is a graph of a MAILONG granule control solution profile measured in accordance with the present invention, with time (min) on the abscissa and absorbance (mAU) on the ordinate.
Fig. 4 is a fingerprint of a typical test solution of the mailuotong granules measured by the present invention, wherein the abscissa is time (min) and the ordinate is absorbance (mAU).
Detailed Description
Comparative example
The quality of the medicine is controlled only by puerarin in the current quality standard of the granules for promoting circulation of blood vessels, and the granules have certain one-sidedness; the vein-relaxing granule fingerprint spectrum detection method can comprehensively compare 21 common peaks of the measured fingerprint spectrum and the comparison spectrum through similarity software, and can more comprehensively and accurately represent the quality of the medicine. According to historical data, the puerarin content in the Mailuotong granules is about 4.5mg, and as can be seen from the following table, the similarity of fingerprint spectrums of batch medicines with the puerarin content near 4.5mg is small, and the reason for the similarity is that the difference between a rutin peak in the fingerprint spectrums of 16110281 and 16101141 and a contrast spectrum is large, the difference between a salvianolic acid B peak in the fingerprint spectrum of 16102381 and the contrast spectrum is large, and the difference between a quercetin peak in the fingerprint spectrum of 16101041 and the contrast spectrum is large, so that the similarity of the quercetin peak and the contrast spectrum is not high. The fingerprint similarity of 2 batches of medicines with lower content is higher, and comparison analysis shows that although the puerarin peak is slightly smaller, the rest 20 peaks are close to the contrast map, so the similarity with the contrast map is high. In brief, the choroid through particle fingerprint spectrum reflects the quality of the medicine by comparing 21 peaks, and is more comprehensive and accurate than single-index puerarin control.
TABLE 1 quality control comparison of MAILUOTONG granule
Examples
The method for constructing the mailuotong granule fingerprint spectrum is to determine the mailuotong granules by adopting a liquid chromatography, and comprises the following specific steps:
(1) preparation of control solutions:
taking a proper amount of puerarin, rutin, ferulic acid, lobetyolin, salvianolic acid B, quercetin and kaempferide, and adding 70% ethanol by volume to prepare a mixed reference solution containing 112 mu g of puerarin, 204 mu g of rutin, 44 mu g of ferulic acid, 32 mu g of lobetyolin, 92 mu g of salvianolic acid B, 40 mu g of quercetin and 28 mu g of kaempferide in each 1 ml.
(2) Preparation of a test solution:
precisely weighing 2.0g of Mailuotong granules, placing into a 100ml conical flask with a plug, precisely adding 50ml of 70 volume percent ethanol, sealing the plug, weighing, treating for 20 minutes by ultrasonic waves (250w, 40KHz), cooling, supplementing the lost weight with 70 volume percent ethanol, shaking uniformly, filtering, and taking the subsequent filtrate to obtain the Chinese medicinal preparation.
(3) Chromatographic conditions and System applicability
A chromatographic column: phenomenex luna (2) C18(4.6 x 250mm, 5 um);
mobile phase: and (B) pump A: acetonitrile; b, pump B: 0.3 vol% formic acid;
gradient elution procedure:
| time (min) | A (acetonitrile) volume% | B (0.30 vol.% formic acid)% by volume |
| 0 | 5 | 95 |
| 3 | 5 | 95 |
| 50 | 42 | 58 |
| 50.1 | 95 | 5 |
| 60 | 95 | 5 |
Detection wavelength: 270 nm;
flow rate: 1.0 ml;
column temperature: 25 deg.C
The theoretical plate number is not less than 3000 according to rutin.
(4) And (3) determination: precisely absorbing 5 μ l of each of the reference solution and the sample solution, injecting into high performance liquid chromatograph, recording chromatogram within 60min, and processing chromatogram with 2004A edition of evaluation System for similarity of traditional Chinese medicine chromatogram fingerprint to obtain fingerprint of MAILUOTONG granule. See fig. 1-2.
The liquid chromatograph is an Agilent 1260 Infinity Series high performance liquid chromatograph.
The fingerprint contains 21 common peaks, and the reference solution and the test solution are simultaneously detected to identify that the No. 4 peak is puerarin, the No. 8 peak is rutin, the No. 9 peak is ferulic acid, the No. 13 peak is lobetyolin, the No. 15 peak is salvianolic acid B, the No. 19 peak is quercetin, and the No. 21 peak is kaempferide. In addition, through LC-MS detection, 12 compounds are respectively estimated to be 1-peak codonopsis pilosula acid, 2-peak 6-hydroxykaempferol 3-rutinoside-6-glucoside, 3-peak genistin, 5-peak puerarin xyloside, 6-peak 3/-methoxy puerarin, 7-peak daidzin, 10-peak codonopsis pilosula glycoside I, 11-peak safflor yellow A, 16-peak daidzein, 17-peak salvianolic acid A, 18-peak biochanin A and 20-peak salvianolic acid C. See fig. 3-4.
Examination of test article preparation method
(1) Examination of extraction solvent
10% methanol, 30% methanol, 50% methanol, 70% methanol, 10% ethanol, 30% ethanol, 50% ethanol, 70% ethanol and ethanol are respectively considered, and the extraction effect of the 70% ethanol and the methanol is equivalent, and the 70% ethanol is selected as the extraction solvent of the Mailuotong granules from the aspects of environmental protection and cost saving.
(2) Investigation of different extraction solvent volumes
When three different volumes of 25ml, 50ml and 75ml of extraction solvents are respectively examined (the corresponding sample amount is 2.5ul, 5ul and 7.5ul), the peak area of the sample is generally larger than that of the sample when the extraction solvent is 25ml when the extraction solvent is 50ml, but the 75ml extraction solvent has no advantage compared with 50ml, and 50ml of 70% ethanol is selected as the volume of the extraction solvent of the Mailuotong granules.
(3) Investigation of different extraction modes
The reflux extraction mode and the ultrasonic extraction mode are compared, the result shows that the reflux extraction mode and the ultrasonic extraction mode have no obvious difference, and the ultrasonic extraction mode is selected as the extraction mode of the venation dredging particles.
(4) Investigation of different extraction times
The extraction time of 5min, 10min, 20min, 30min and 40min as the choroid dredging granule samples is respectively considered, the peak areas of the 5min, the 30min and the 40min are not greatly different when the extraction time is 20min, 30min and 40min, but the advantages are obvious compared with the 5min and 10min, and the 20min is selected as the ultrasonic extraction time of the choroid dredging granule.
Examination of chromatography conditions for Mailuotong granule
(1) Examination of elution System
Compared with 4 different types of elution systems of acetonitrile-water, acetonitrile-acid water, methanol-water and methanol-acid water, the elution system has the advantages that the peak is fast when the organic phase is acetonitrile, most substances can be eluted within 50min, when acid is added into the mobile phase, the characteristic peaks of ferulic acid and salvianolic acid B are advanced in time and have good peak patterns, and therefore the elution system of the product is selected from the acetonitrile-acid water.
(2) Investigation of different kinds of acids
Comparing 3 types of acids with commonly used types and concentrations in 3 laboratories of acetonitrile-0.3% formic acid, acetonitrile-0.5% acetic acid and acetonitrile-0.05% phosphoric acid, finding that the separation effect of the acetonitrile-0.3% formic acid and the acetonitrile-0.05% phosphoric acid is better than that of the acetonitrile-0.5% acetic acid, and finally selecting the formic acid as a pH regulator of the venation dredging particle mobile phase in consideration of the fact that the phosphoric acid cannot enter a liquid chromatography-mass spectrometry system.
(3) Investigation of different acid concentrations
Comparing 0.2% formic acid, 0.3% formic acid, 0.4% formic acid, respectively, the result was that 0.3% formic acid separated the best, so acetonitrile-0.3% formic acid was finally selected as the mobile phase of the venation particle.
(4) Investigation of different chromatography columns
The results of comparison of phenomenex luna (2) C18(4.6 × 250mm, 5um), Agilent plus C18(4.6 × 250mm, 5um), waters Atlantis T3C18(4.6 × 250mm, 5um) with 3 different brands of C18 chromatographic columns, respectively, showed that only phenomenex luna (2) C18 chromatographic columns could separate puerarin xyloside and 3/The-methoxy puerarin is separated, and other 2 types of chromatographic columns are not separated at all, so the phenomenenx luna (2) C18(4.6 x 250mm, 5um) is selected as the chromatographic column for analyzing the fingerprint of the Jingluong particles.
(5) Investigation of different column temperatures
Comparing 3 column temperatures of 20 ℃, 25 ℃ and 30 ℃, the separation effect at 25 ℃ is the best, so 25 ℃ is selected as the column temperature for analyzing the vein-relaxing granule fingerprint.
(6) Investigation of different wavelengths
By comparing the chromatogram patterns with the wavelengths of 250nm, 260nm, 270nm, 300nm, 280nm, 290nm, 325nm and 360nm, the peak appearance conditions of the chromatogram with the wavelength of 270nm are relatively balanced, and the maximum absorption wavelength of the lobetyolin is 270 nm. Therefore, 270nm is selected as the detection wavelength for analyzing the fingerprint spectrum of the vein-relaxing granule.
Methodology investigation
(1) Precision survey
Taking 2.0g of the Mailuotong granules with the batch number of 16102381, preparing a test sample solution according to a test sample preparation method, continuously injecting samples for 6 times, recording chromatograms, and comparing the similarity of 6 maps. As a result, the similarity between the spectra was 1.000, indicating that the precision of the instrument is good, as shown in Table 2.
TABLE 2 Mailuotong granule precision experimental results (16102381)
(2) Repeatability survey
6 parts of test solution was prepared from the Mailuotong granules of lot number 16102381 according to the test preparation method. And (4) injecting samples according to the chromatographic conditions, recording chromatograms, and comparing the similarity of 6 maps. The similarity among the result spectra is 1.000, which shows that the method has good repeatability and is shown in Table 3.
TABLE 3 results of repeated experiments on Mailuotong granules (16102381)
(3) Stability survey
Taking 2.0g of the granules with the batch number of 16102381 for Mailuotong, preparing a sample solution according to a sample preparation method, respectively injecting samples at 0h, 2h, 4h, 8h, 12h, 16h, 20h and 24h after sample preparation, recording chromatograms, and carrying out similarity comparison on the total peaks of 8 maps. As a result, the similarity between the maps was 1.000, indicating that the stability of the sample was good, as shown in Table 4.
TABLE 4 Mailuotong granule stability test results (16102381)
Similarity comparison
The HPLC chromatogram of 14 batches of Mailuotong granules are sequentially led into a traditional Chinese medicine chromatogram fingerprint similarity evaluation system in an AIA format, and similarity comparison is carried out with the generated control fingerprint, and the result is shown in a table 5.
TABLE 514 evaluation results of similarity of MAILUOTONG granule samples
The data show that the similarity of 14 batches of the mailuotong granules and a reference fingerprint spectrum is more than 0.9, which indicates that the quality stability of the product is good.
Compared with the prior art, the vein relaxing granule fingerprint spectrum detection method provided by the invention has good stability and repeatability, can objectively, comprehensively and accurately evaluate the quality of the vein relaxing granule, and has important significance for controlling the quality of the vein relaxing granule and ensuring the clinical curative effect.
The foregoing is illustrative of the present invention and it will be appreciated by those skilled in the art that changes and modifications may be made thereto without departing from the principles of the invention and without departing from the scope of the invention.
Claims (4)
1. A fingerprint detection method of Mailuotong granules comprises the steps of detecting the Mailuotong granules by adopting a high performance liquid chromatography, wherein the chromatography conditions comprise:
using octadecylsilane chemically bonded silica as filler, acetonitrile as mobile phase A, and 0.3 vol% formic acid water solution as mobile phase B, and performing gradient elution at flow rate of 0.5-1.5 ml/min-1The column temperature is 20-35 ℃, and the detection wavelength is 210-360 nm; the theoretical plate number is not less than 3000 calculated according to rutin peak;
during the gradient elution, the ratio of mobile phase a changes as: 0-3 min, 5 vol% acetonitrile; 3-50 min, 5-42 vol% acetonitrile; 50-50.1 min, 42-95% acetonitrile by volume; 50.1-60 min, 95 volume percent acetonitrile; i.e. gradient elution procedure as follows:
The detection method also comprises the following steps:
(1) preparation of a test solution: 2.0g of Mailuotong granules are taken, precisely weighed, placed in a 100ml conical flask with a plug, precisely added with 25-75 ml of 70 volume percent ethanol, tightly plugged and weighed, ultrasonically treated for 10-40 minutes under the conditions of 250w and 40KHz, cooled, supplemented with 70 volume percent ethanol to reduce the weight, shaken evenly and filtered, and the subsequent filtrate is taken, thus obtaining the Chinese medicinal preparation;
(2) preparation of control solutions: taking a proper amount of puerarin, rutin, ferulic acid, lobetyolin, salvianolic acid B, quercetin and kaempferide, and adding 70 vol% ethanol to prepare a mixed reference solution containing 112 mu g of puerarin, 204 mu g of rutin, 44 mu g of ferulic acid, 32 mu g of lobetyolin, 92 mu g of salvianolic acid B, 40 mu g of quercetin and 28 mu g of kaempferide in each 1 ml;
(3) and (3) determination: precisely absorbing 2-10 μ l of each of the reference solution and the sample solution, respectively, injecting into a high performance liquid chromatograph, recording chromatogram within 60 minutes, and processing the chromatogram with version 2004A of evaluation System for similarity of traditional Chinese medicine chromatogram fingerprint to obtain fingerprint of MAILUOTONG granule.
2. The detection method according to claim 1, wherein the chromatography column using octadecylsilane bonded silica gel as a filler is phenomenenx luna (2) C18, 4.6 x 250mm, 5 um.
3. Use of a fingerprint of the choroid pass granules obtained by the method for fingerprint detection of the choroid pass granules according to any one of claims 1 to 2 to control the quality of the choroid pass granules, said fingerprint having 21 common peaks.
4. Use according to claim 3, wherein the retention time of each common peak is: common peak 1: 13.234 min; common peak 2: 15.952 min; common peak 3: 17.602 min; consensus peak 4: 20.612 min; consensus peak 5: 21.099 min; consensus peak 6: 21.321 min; common peak 7: 24.057 min; common peak 8: 27.190 min; consensus peak 9: 28.845 min; common peak 10: 29.452 min; common peak 11: 29.830 min; common peak 12: 30.206 min; consensus peak 13: 33.715 min; consensus peak 14: 34.979 min; consensus peak 15: 37.136 min; common peak 16: 38.789 min; consensus peak 17: 39.278 min; consensus peak 18: 39.610 min; common peak 19: 41.671 min; common peaks 20: 45.049 min; common peak 21: 48.173 min.
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| CN109406672A (en) * | 2018-11-20 | 2019-03-01 | 合肥创新医药技术有限公司 | A kind of fingerprint spectrum method using HPLC measurement Chinese medicine yiguan decoction |
| CN113759009B (en) * | 2020-08-26 | 2023-03-17 | 北京康仁堂药业有限公司 | Method for constructing characteristic spectrum of equisetum hiemale and preparation thereof |
| CN112748201B (en) * | 2020-12-28 | 2022-12-27 | 南京海昌中药集团有限公司 | Method for detecting fingerprint of radix puerariae assorted Chinese herbal tea |
| CN113720954B (en) * | 2021-09-18 | 2022-02-11 | 安徽中医药大学第一附属医院(安徽省中医院) | Method for establishing fingerprint spectrum of brain-improving capsule and quality evaluation method |
| CN114166958B (en) * | 2021-10-29 | 2024-03-29 | 合肥创新医药技术有限公司 | Detection method of fingerprint of traditional Chinese medicine compound herba xanthil stomach-calming particles and application thereof |
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