CN113567575B - Fingerprint spectrum determination method of disintegrating masses and harmonizing stomach capsule - Google Patents
Fingerprint spectrum determination method of disintegrating masses and harmonizing stomach capsule Download PDFInfo
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Images
Classifications
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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
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention discloses a High Performance Liquid Chromatography (HPLC) fingerprint determination method of a capsule for dispersing lumps and harmonizing stomach. The fingerprint spectrum of the capsule for relieving oppression and regulating stomach, which is obtained by the invention, has 17 common peaks, and 6 components (salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1) are identified. The method has good stability and reproducibility, and the established fingerprint of the capsule for relieving distension and fullness and harmonizing the stomach can provide reference for the establishment of the comprehensive quality standard.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine quality analysis, and particularly relates to a High Performance Liquid Chromatography (HPLC) fingerprint spectrum determination method of a capsule for relieving distension and fullness and harmonizing stomach.
Background
The capsule for relieving distension and fullness and harmonizing stomach is derived from Miao nationality, is prepared from four traditional Chinese medicines of radix cynanchi wilfordii, roxburgh rose leaf, willow branch and pseudo-ginseng, has the effects of regulating qi and harmonizing stomach, relieving distension and pain and dredging collaterals and activating collaterals, and can be used for treating symptoms such as burning distending pain of stomach, acid regurgitation, fullness and epigastric upset and the like caused by qi stagnation of spleen and stomach. Can also be clinically used for treating gastrointestinal tract diseases such as gastric precancerous lesion, functional dyspepsia and the like. Radix cynanchi wilfordii, also called bunge auriculate root, enters spleen, stomach and kidney channels and has the pharmacological activities of promoting digestion, removing food retention, nourishing yin, tonifying deficiency, resisting aging, enriching blood and raising qi. The main active ingredients in cynanchum wilfordii comprise C21 steroid saponins and acetophenone compounds, and 4-hydroxyacetophenone is a representative compound. Rosa roxburghii leaf, which belongs to spleen, kidney and stomach channels, mainly contains amino acids, phenolic acids and flavonoids, and can be used for treating food retention, fullness, scabies, pain and incised wound. Willow branch, branch of weeping willow of Salicaceae, belonging to stomach and liver meridians, is commonly used for treating chronic inflammation such as fever, dermatosis, infection, etc., and its characteristics of analgesia, antipyresis and anti-inflammation are closely related to salicin and its derivatives as active ingredients; notoginseng radix is dry root of Panax notoginseng (Burk.) F.H.Chen of Araliaceae, and has effects of stopping bleeding, dispelling blood stasis and relieving pain, and Panax notoginsenosides (including notoginsenoside R1, ginsenoside Rg1, ginsenoside Rb1 and ginsenoside Re) are main active ingredients of Notoginseng radix, and its content is up to 12%.
The capsule for relieving stuffiness and harmonizing stomach is currently collected in the national drug standards of the State drug administration, the quality control method mainly adopts the content measurement of a single substance, but the measurement and analysis method aiming at the single drug component cannot reflect the integral quality level of the traditional Chinese medicine compound, and the quality stability is difficult to ensure.
Disclosure of Invention
In order to improve the technical problem, the invention provides a method for constructing or detecting a fingerprint of a capsule for relieving stuffiness and harmonizing stomach, which comprises the steps of relieving a test solution of the capsule for relieving stuffiness and harmonizing stomach and carrying out HPLC detection, wherein the HPLC detection conditions comprise: gradient elution is carried out by using a C18 chromatographic column and using a water phase as a mobile phase A and acetonitrile as a mobile phase B.
According to the invention, the gradient elution procedure is:
preferably, the gradient elution procedure is:
according to the invention, the C18 column may be SymmetryShieldT MRP18 or
C18 chromatography column, in one embodiment of the invention, is
C18 column, exemplified by C18Column [ (1.5-4.6) mm i.d. × (150-]。
According to the invention, the detection wavelength is 200-206 nm, in one embodiment of the invention 203 nm.
According to the invention, the sample volume for detection is 2.0-8.0. mu.L, and in one embodiment of the invention, the sample volume is 5.0. mu.L.
According to the invention, the flow rate of the assay is 0.8-1.3mL/min, in one embodiment of the invention, 1.0 mL-min-1。
According to the invention, the detected column temperature is 20-40 ℃, and in one embodiment of the invention is 30 ℃.
According to the invention, the preparation method of the test solution comprises the steps of taking the contents of the capsule for relieving stuffiness and harmonizing the stomach, and adding a solvent for extraction. The solvent may be a solvent commonly used in the art for natural compound extraction, including but not limited to an alcohol or an aqueous solution of an alcohol. In some embodiments of the invention, the alcohol is selected from methanol, ethanol. In some embodiments of the invention, the extraction solvent is selected, for example, from a 60-85% aqueous methanol solution, illustratively a 75% aqueous methanol solution.
The extraction method may be a natural compound extraction method commonly used in the art, including but not limited to ultrasonic extraction or reflux extraction. In some embodiments of the invention, reflux extraction is employed. For example, the reflux extraction time is 0.5 to 2 hours, and exemplary times are 0.5 hours, 1 hour, and 2 hours.
According to the invention, the ratio of the weight of the capsule content to the volume of the added extraction solvent in the preparation of the test solution is 10-30 mg of the capsule content/mL, and the exemplary weight is 10mg of the capsule content/mL, 20mg of the capsule content/mL and 30mg of the capsule content/mL.
According to the invention, the preparation method of the test solution further comprises the operation of carrying out solid-liquid separation on the extracting solution to obtain the test solution. The solid-liquid separation may be a separation means commonly used in the art, including but not limited to filtration and centrifugation. In one embodiment of the invention, filtration is used, for example, filtration using a 0.45 μm microfiltration membrane.
The fingerprint construction method of the capsule for relieving distension and fullness and harmonizing stomach further comprises the step of detecting the standard solution under the same HPLC condition.
According to the invention, the standard comprises salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb 1.
According to the invention, the standard solution is a solution of a single standard per standard, and/or a solution of a mixture of 6 standards.
According to the invention, the construction method further comprises the step of preparing a standard solution, the preparation method of the standard solution comprises the steps of preparing a solution of each standard, and dissolving salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 respectively with a solvent to obtain the solution of each standard.
According to the present invention, the method for preparing the standard substance solution may further comprise preparing a solution of a standard substance mixture, mixing salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1, and dissolving with a solvent to obtain a solution of a standard substance mixture.
According to the invention, the solvent for preparing the standard solution is selected from methanol and/or ethanol, in one embodiment of the invention methanol.
According to the invention, the concentrations of salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 of each standard solution or standard mixture solution are respectively 20-25 mug/mL, 5-10 mug/mL, 2-10 mug/mL, 110-120 mug/mL, 400-410 mug/mL and 360-380 mug/mL; in one embodiment of the invention, the concentrations of salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 in the standard solution are 21.8 μ g/mL, 8.04 μ g/mL, 6.66 μ g/mL, 114.4 μ g/mL, 408 μ g/mL and 368 μ g/mL, respectively.
According to the invention, different batches of the capsule samples for relieving oppression and regulating stomach are used for fingerprint construction in the construction method, and the different batches are at least 5 batches; more preferably at least 10 batches.
The fingerprint of the capsule for relieving stuffiness and harmonizing the stomach obtained by the liquid chromatography fingerprint construction method provided by the invention has 17 common characteristic peaks, wherein: the 3 peak is salicin, the 6 peak is epicatechin, the 7 peak is 4-hydroxyacetophenone, the 9 peak is notoginsenoside R1, the 10 peak is ginsenoside Rg1 and the 12 peak is ginsenoside Rb 1.
When the chromatographic peak of the ginsenoside Rb1 with the 12 th peak is taken as a reference (S), the relative retention time of 17 common characteristic peaks is as follows:
when the chromatographic peak of the ginsenoside Rb1 with the 12 th peak is taken as a reference (S), the relative peak area of each common characteristic peak is as follows:
according to the invention, the construction method or the detection method of the fingerprint of the capsule for relieving stuffiness and harmonizing stomach comprises the following steps:
(1) taking salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 as reference substances, respectively preparing into solutions of the reference substances, and optionally further preparing solutions of 6 standard substance mixtures;
(2) removing the content of the capsule, adding 75% methanol, refluxing in water bath, filtering with 0.45 μm microporous membrane, and collecting the filtrate as sample solution;
(3) respectively sucking 5 μ L of the above reference solution and sample solution, and injecting into liquid chromatograph under the following chromatographic conditions: by using
C18 column (4.6 mm. times.150 mm, 5 μm); mobile phase a (aqueous phase) and phase B (acetonitrile); the gradient elution flow rate was 1.0 ml/min-1(ii) a The column temperature is 30 ℃; detecting wavelength is 203nm, theoretical plate number is not less than 5000 according to ginsenoside Rb1, and chromatogram of XIAOPI and HEWEI Capsule of different batches, chromatogram of each control product, and chromatogram of 6 kinds of standard product mixture are obtained;
(4) generating a fingerprint spectrum: and identifying chromatographic peaks through the chromatograms of the various reference substances and the optional 6 standard substance mixture chromatograms, and preparing the fingerprint of the Xiaopi Hewei capsule by the chromatograms of the Xiaopi Hewei capsules of different batches.
On the basis of the technical scheme, according to the detection method of the fingerprint of the xiaofu stomach harmonizing capsule, the to-be-detected xiaofu stomach harmonizing capsule is prepared into the to-be-detected sample solution according to the HPLC detection condition and the preparation method of the to-be-detected sample solution, HPLC detection is carried out, the fingerprint of the to-be-detected xiaofu stomach harmonizing capsule is compared with the fingerprint of the to-be-detected xiaofu stomach harmonizing capsule constructed by the invention, the relative retention time is qualified product within +/-5% of a specified value, and similarity evaluation is carried out on the fingerprint, wherein the similarity is more than 0.8, preferably more than 0.90, and the qualified product is obtained.
The invention also provides a fingerprint of the Xiaopi Hewei capsule obtained by the fingerprint construction method. The fingerprint is substantially as shown in B in figure 2.
The invention also provides an application of the fingerprint construction method and/or the detection method of the capsule for relieving stuffiness and harmonizing the stomach in the quality control of the capsule for relieving stuffiness and harmonizing the stomach.
In the present invention, "optional", "optionally" or "optionally present" means that the subsequently described event or circumstance may, but need not, occur, and that the description includes instances where said event or circumstance occurs and instances where it does not.
In the present invention, "comprise" and "comprise" are open-ended expressions, i.e. include what is indicated by the present invention, but do not exclude other aspects. It should be understood that "comprising" and "including" can encompass the inclusive meaning of "consisting of … …".
The invention has the beneficial effects that:
the traditional Chinese medicine fingerprint is mainly used for evaluating the stability and reproducibility of the quality of the traditional Chinese medicine and the preparation thereof. The invention rapidly and intuitively identifies the drug effect substance basis of the capsule for relieving stuffiness and harmonizing the stomach by adopting a chemical fingerprint quality control method, determines 17 common peaks in total, and identifies 6 components (salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1) in the drug effect substance basis, thereby laying a foundation for establishing the comprehensive quality standard of the capsule for relieving stuffiness and harmonizing the stomach.
The invention compares different extraction solvents of methanol, 75% methanol, 50% methanol and water; different extraction times are 30min, 1h and 2 h; ultrasonic extraction and water bath reflux extraction are carried out by different extraction methods, and finally 75% methanol and water bath reflux are determined to be the preferable preparation method of the test solution.
The invention adopts SymmetryShieldTMRP18(4.6mm multiplied by 150mm, 5 mu m), Diamon C18(2) (4.6mm multiplied by 150mm, 5 mu m) and
c18 column (4.6 mm. times.150 mm, 5 μm), as a result of which it was found that
The chromatogram obtained by separating under C18 chromatographic column (4.6mm × 150mm, 5 μm) has good peak shapeBetter resolution. Therefore, the method can be used as a chromatographic column which is preferable in subsequent research.
The invention establishes an HPLC fingerprint spectrum measuring method of the Xiaopi Hewei capsules by analyzing 10 batches of the Xiaopi Hewei capsules, and comprehensively evaluates the quality of the Xiaopi Hewei capsules. The precision, repeatability and stability experiments prove that the method has higher stability and reliability, so that the method can be used as a method for measuring the fingerprint spectrum of the disintegrating masses and harmonizing the stomach capsule.
Drawings
FIG. 1 shows fingerprint of the Xiaopi Hewei capsule obtained under different chromatographic column conditions, wherein A is the fingerprint of the Xiaopi Hewei capsule obtained under the conditions of the SymmetryShieldMRP 18 chromatographic column; b is fingerprint of the Xiaopi Hewei capsule under the chromatographic column condition of Diamon C18 (2); c is
C18 fingerprint of XIAOPI HEWEI JIAO NANG.
In FIG. 2, A is the chromatogram of the mixed control; in fig. 2, B is the fingerprint of the Xiaopi Weiwei capsule; in figure 2C is the HPLC fingerprint overlay of 10 batches of Xiaopi Hewei capsules.
Detailed Description
The technical solution of the present invention will be further described in detail with reference to specific embodiments. It is to be understood that the following examples are only illustrative and explanatory of the present invention and should not be construed as limiting the scope of the present invention. All the technologies realized based on the above-mentioned contents of the present invention are covered in the protection scope of the present invention.
Unless otherwise indicated, the raw materials and reagents used in the following examples are all commercially available products or can be prepared by known methods.
Example 1 establishment of Standard fingerprint of Xiaopi Weiwei Capsule
1. Apparatus and materials
1.1 instruments
High performance liquid chromatograph (model: U3000, Saimer Feishale science and technology Co., Ltd.), electric heating constant temperature water bath (model: HH-S4A, Beijing Kogyi Yongxing instruments Co., Ltd.); an XS105 type electronic balance (sydows scientific instruments (beijing) ltd); Milli-Q ultrapure water purification system (east science and technology, Wuzhou, Beijing).
1.2 materials
Salicin (purity not less than 98%, lot number Y12S6S1, Shanghai-sourced leaf Biotechnology Co., Ltd.), epicatechin (purity not less than 98%, lot number 110878-supple 201703, China food and drug testing institute), 4-hydroxyacetophenone (purity not less than 98%, lot number T21J6C1, Shanghai-sourced leaf Biotechnology Co., Ltd.), notoginsenoside R1 (purity not less than 98%, lot number 110745-supple 201921, China food and drug testing institute), ginsenoside Rg1 (purity not less than 98%, lot number 110703-supple 202034, China food and drug testing institute), ginsenoside Rb1 (purity not less than 98%, lot number 110704-supple 202129, China food and drug testing institute); 10 batches of xiaopai stomach-harmonizing capsules (batch No. S1-S10) with the respective batch nos. 20200702, 20200701, 20190102, 20200104, 20200105, 20200201, 20200601, 20200603, 20200604, 20200602, from guizhou yongle pharmaceutical limited; chromatographically pure acetonitrile; chromatographically pure methanol; ultrapure water.
2. Method and results
2.1 chromatographic conditions
HPLC fingerprint analysis conditions adopt
C18 column (4.6 mm. times.150 mm, 5 μm); mobile phase a (aqueous phase) and phase B (acetonitrile); gradient elution; the flow rate was 1.0 ml/min-1(ii) a The column temperature is 30 ℃; the sample volume was 5. mu.L, and the detection wavelength was 203 nm.
TABLE 1 gradient elution method
2.2 preparation of control solutions
Respectively taking salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 reference substances, precisely weighing, and adding methanol to prepare a mixed reference substance solution containing 21.8 mu g/ml salicin, 8.04 mu g/ml epicatechin, 6.66 mu g/ml 4-hydroxyacetophenone, 1114.4 mu g/ml notoginsenoside R1408 mu g/ml and ginsenoside Rb 1368 mu g/ml ginsenoside Rb.
Simultaneously, salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 reference substances are respectively taken and precisely weighed, and methanol is respectively added to prepare a single solution of the reference substances of 21.8 mu g/mL salicin, 8.04 mu g/mL epicatechin, 6.66 mu g/mL 4-hydroxyacetophenone, 1114.4 mu g/mL notoginsenoside R, 1408 mu g/mL ginsenoside Rg1408 and 1368 mu g/mL ginsenoside Rb.
2.3 preparation of test solutions
Taking the contents of the capsule for relieving stuffiness and harmonizing the stomach, mixing uniformly, precisely weighing 0.5g of fine powder, placing the fine powder in a conical flask with a plug, precisely adding 25ml of 75% methanol, weighing, refluxing in a water bath for 2h, cooling, weighing, supplementing the weight with 75% methanol, shaking uniformly, filtering through a 0.45 mu m microporous filter membrane, and taking the subsequent filtrate to obtain the capsule.
2.4 HPLC fingerprint analysis of Xiaopi Weiwei capsules
2.4.1 precision test
Sampling the same batch of the capsule sample for relieving oppression and regulating stomach (batch number: 20200702) continuously for 6 times, recording the retention time and peak area of each common chromatographic peak, and calculating the relative retention time and relative peak area of each common chromatographic peak by taking the retention time and peak area of the ginsenoside Rb1 of the 12 th peak as reference so as to examine the consistency of the relative retention time and relative peak area ratio of the chromatographic peaks. The results show that: the relative retention time RSD of each common peak is less than 1%, and the RSD of the relative peak area is less than 2.7%, so that the determination method is stable, the system compactness is good, and the method is stable and reliable.
2.4.2 stability test
Sampling and analyzing the same batch (batch number: 20200702) of the capsule for relieving oppression and regulating stomach, recording the retention time and peak area of each common chromatographic peak at different time points (0h, 2h, 4h, 6h, 8h, 12h and 24h), and converting the relative retention time and relative peak area of each common chromatographic peak by taking the retention time and peak area of the ginsenoside Rb1 as a reference so as to examine the consistency of the relative retention time and relative peak area ratio of the chromatographic peaks. The results show that: the relative retention time RSD of each common peak is less than 1 percent, and the RSD of the relative peak area is less than 2.74 percent. Therefore, the capsule sample for relieving distension and fullness and harmonizing stomach has good stability under experimental conditions, and can ensure the reliability of the analysis result within 24 h.
2.4.3 repeatability test
Taking the same batch (batch number: 20200702) of the capsule for relieving oppression and regulating stomach to prepare 6 test solution parts in parallel according to the method under item '2.3', respectively injecting samples for analysis, recording the retention time and peak area of each common chromatographic peak, and converting the relative retention time and relative peak area of each common peak by taking the retention time and peak area of the No. 12 peak ginsenoside Rb1 as reference so as to examine the consistency of the relative retention time and relative peak area ratio of the chromatographic peaks. This indicates that: the relative retention time RSD of all the shared peaks is less than 1%, and the RSD of the relative peak area is less than 3.29%, so that the method is stable and reliable and is beneficial to popularization.
2.4.4 establishment of HPLC fingerprint of Xiaopi Weiwei capsules and similarity evaluation
Taking 10 batches of XIAOPI HEWEI CAPSULE (batch No.: 20200702, 20200701, 20190102, 20200104, 20200105, 20200201, 20200601, 20200603, 20200604 and 20200602), preparing test solution according to the method under item "2.3", injecting sample, analyzing, and recording chromatogram respectively. Selecting a representative spectrum (a capsule for relieving oppression and regulating stomach with a batch number of 20200702) as a comparison fingerprint, adopting a traditional Chinese medicine chromatogram fingerprint similarity evaluation system recommended by pharmacopoeia committee to analyze, taking chromatogram similarity (similarity) as a fingerprint evaluation index, and adopting multipoint correction full-spectrum matching to generate a fingerprint common mode. The similarity between each batch of samples and the reference fingerprint is (0.999, 0.996, 0.999, 0.994, 0.998, 0.999 and 0.993), respectively.
2.4.5 identification of common peaks in finger print, calculation of relative peak area and relative retention time
And (4) processing by using similarity evaluation system software, and detecting 17 peaks in 10 batches of fingerprint spectrums. Comparing with the mixed reference substance, and calibrating 6 chromatographic peaks, wherein: the No. 3 peak is salicin, the No. 6 peak is epicatechin, the No. 7 peak is 4-hydroxyacetophenone, the No. 9 peak is notoginsenoside R1, the No. 10 peak is ginsenoside Rg1 and the No. 12 peak is ginsenoside Rb 1. The retention time is 6.26min, 8.52min, 14.555min, 34.968min, 35.906min and 41.963 min. The peak shape of the 12 th peak is good, no impurity peak interference exists before and after the peak shape, and the separation is complete, so that the 12 th peak is selected as a reference peak and is used for calculating the relative peak area and the relative retention time of other shared peaks, and the results are shown in the following tables 2 and 3.
Relative peak areas of 17 common peaks in batch 210 samples (S1-S10)
TABLE 310 relative retention times of 17 common peaks in sample lots (S1-S10)
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (20)
1. A method for constructing fingerprint of a capsule for relieving stuffiness and harmonizing stomach is characterized in that a test solution of the capsule for relieving stuffiness and harmonizing stomach is subjected to HPLC detection, and the HPLC detection conditions comprise: performing gradient elution by using a C18 chromatographic column and using a water phase as a mobile phase A and acetonitrile as a mobile phase B, wherein the gradient elution procedure is as follows:
the method also further comprises the steps of detecting the standard solution under the same HPLC condition; the standard substance comprises salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb 1; the standard solutions are solutions of a single per standard, and/or solutions of a mixture of 6 standards.
2. The method of claim 1, wherein the C18 column is Symmetry ShieldTM RP18 or
C18 chromatography column.
3. The construction method according to claim 1, wherein the detection wavelength is 200-206 nm.
4. The construction method according to claim 1, wherein the sample size of the detection is 2.0-8.0. mu.L.
5. The construction method according to claim 1, wherein the detected column temperature is 20-40 ℃.
6. The method according to any one of claims 1 to 5, wherein the fingerprint of the Xiaopi Hewei capsule obtained has 17 common characteristic peaks, wherein: the 3 peak is salicin, the 6 peak is epicatechin, the 7 peak is 4-hydroxyacetophenone, the 9 peak is notoginsenoside R1, the 10 peak is ginsenoside Rg1 and the 12 peak is ginsenoside Rb 1;
when the chromatographic peak of the ginsenoside Rb1 with the 12 th peak is taken as a reference S, the relative retention time of 17 common characteristic peaks is as follows:
。
7. The method according to any one of claims 1 to 5, wherein the fingerprint of the Xiaopi Hewei capsule obtained has 17 common characteristic peaks, wherein: the 3 peak is salicin, the 6 peak is epicatechin, the 7 peak is 4-hydroxyacetophenone, the 9 peak is notoginsenoside R1, the 10 peak is ginsenoside Rg1 and the 12 peak is ginsenoside Rb 1; when the chromatographic peak of the ginsenoside Rb1 with the 12 th peak is taken as a reference S, the relative peak area of each common characteristic peak is as follows:
8. the method of any one of claims 1 to 5, wherein the sample solution is prepared by extracting the contents of the Xiaopi Hewei capsule with a solvent.
9. The method of claim 8, wherein the solvent is a 60-85% aqueous solution of methanol.
10. The construction method according to claim 8, wherein reflux extraction is adopted, and the time of reflux extraction is 0.5-2 h.
11. The method of claim 8, wherein the sample solution is prepared such that the ratio of the weight of the capsule content to the volume of the extraction solvent is 10-30 mg/mL.
12. The method of any one of claims 1 to 5, wherein the solvent for preparing the standard solution is methanol.
13. The construction method according to any one of claims 1 to 5, wherein the concentration of salicin, epicatechin, 4-hydroxyacetophenone, notoginsenoside R1, ginsenoside Rg1 and ginsenoside Rb1 in each standard solution or standard mixture solution is 20 to 25 μ g/mL, 5 to 10 μ g/mL, 2 to 10 μ g/mL, 110 to 120 μ g/mL, 400 to 410 μ g/mL, 360 to 380 μ g/mL, respectively.
14. A method for detecting fingerprint of a capsule for relieving stuffiness and harmonizing stomach is characterized in that the capsule for relieving stuffiness and harmonizing stomach is prepared into a test solution for HPLC detection, and the HPLC detection conditions comprise: performing gradient elution by using a C18 chromatographic column and using a water phase as a mobile phase A and acetonitrile as a mobile phase B, wherein the gradient elution procedure is as follows:
15. the method of claim 14, wherein the C18 chromatography column is Symmetry ShieldTMRP18 or
C18 chromatography column.
16. The detection method according to claim 14, wherein the detection wavelength is 200 to 206 nm.
17. The method according to claim 14, wherein the amount of the sample to be detected is 2.0 to 8.0. mu.L.
18. The method according to claim 14, wherein the column temperature is 20 to 40 ℃.
19. The detection method according to any one of claims 14 to 18, wherein the fingerprint obtained by detecting the gastric and gastric distention capsule to be detected is compared with the fingerprint of the gastric and distention capsule constructed by the method according to any one of claims 1 to 13.
20. Use of the method of construction according to any one of claims 1 to 13 or the method of testing according to any one of claims 14 to 19 for the quality control of xiaofu and wei capsules.
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Effective date of registration: 20221026 Address after: No. 68, Dongfeng Avenue, National High tech Industrial Development Zone, Guiyang, Guizhou 550024 Patentee after: GUIYANG YONGLE PHARMACEUTICAL CO.,LTD. Address before: Building A1, Haitong times business center, No. 11, West Third Ring North Road, Haidian District, Beijing 100089 Patentee before: SHORING (BEIJING) PHARMACEUTICAL TECHNOLOGY Co.,Ltd. |