CN113325115A - Method for establishing characteristic spectrum of qi stagnation stomachache granules and application thereof - Google Patents
Method for establishing characteristic spectrum of qi stagnation stomachache granules and application thereof Download PDFInfo
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- 239000008187 granular material Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 30
- 238000001228 spectrum Methods 0.000 title claims abstract description 20
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- AEQDJSLRWYMAQI-KRWDZBQOSA-N tetrahydropalmatine Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3C[C@H]2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-KRWDZBQOSA-N 0.000 claims description 6
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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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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- 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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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
- G01N30/8679—Target compound analysis, i.e. whereby a limited number of peaks is analysed
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- 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
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Abstract
The scheme relates to a method for establishing a characteristic spectrum of qi stagnation stomachache granules and application thereof, and comprises the steps of preparing a test solution; preparing a reference substance solution; measuring by a liquid chromatograph by taking acetonitrile and phosphoric acid solution with mass concentration of 0.1% as mobile phases; the method is verified by means of specificity, precision, repeatability, stability and the like; and (3) obtaining a characteristic spectrum by utilizing a Chinese medicine chromatogram fingerprint similarity evaluation system of the State pharmacopoeia Committee through data import, multipoint correction and data matching. The characteristic spectrum established by the qi stagnation stomachache granules represents most of pharmacological active ingredients of the qi stagnation stomachache granules, can reflect the quality profile of the qi stagnation stomachache granules, and can be used as one of standard indexes for quality detection and quality control of the qi stagnation stomachache granules; the method has high stability and precision and good repeatability, and can effectively ensure the stability and the uniformity of the quality of the granules for treating the stomachache due to qi stagnation, thereby being conductive to improving the effectiveness and the safety of the clinical medication of the medicine.
Description
Technical Field
The invention relates to the field of quality control methods of traditional Chinese medicine preparations, in particular to a method for establishing a characteristic spectrum of qi stagnation stomachache granules and application thereof.
Background
The qi stagnation stomachache granule is elaborately developed by multiple experts such as national academy of engineers, national famous Chinese medicine expert Wangyangyan professor and the like on the basis of an ancient formula of 'Siyisan', is a classic traditional Chinese medicine compound for treating stomachache series diseases, and is mainly prepared from six medicinal materials including bitter orange, vinegar nutgrass galingale rhizome, radix bupleuri, vinegar rhizoma corydalis, white paeony root and honey-fried licorice root. The traditional Chinese medicine composition is applied to thousands of hospitals in more than 20 provinces, direct prefectures and autonomous regions in China for more than 30 years in the market, has the effective rate of more than 85 percent on the treatment of symptoms such as liver depression and qi stagnation, chest fullness and distention, epigastric pain and the like, and becomes a first-line medicine for clinically treating epigastric pain through years of clinical practice.
At present, the granules for treating qi stagnation stomachache are mainly subjected to thin-layer identification of paeoniflorin and tetrahydropalmatine and paeoniflorin content detection in Chinese pharmacopoeia to control the quality of the granules for treating qi stagnation stomachache. However, since the raw materials of the qi-stagnation stomachache granules are many and the types of the chemical components are many, the quality of the qi-stagnation stomachache granules can not be comprehensively reflected on the whole only by detecting and controlling the quality of the qi-stagnation stomachache granules through 1-2 chemical components, which causes the lack of objectivity and accuracy of the quality detection result, and thus the effectiveness and the safety of clinical medication of the qi-stagnation stomachache granules can not be ensured.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a quality method for comprehensively and rapidly detecting the granules for treating qi stagnation and stomachache, and has important significance for comprehensive quality detection and overall quality control.
In order to achieve the purpose, the invention provides the following technical scheme:
a method for establishing a characteristic spectrum of qi stagnation stomachache granules comprises the following steps:
1) preparation of a test solution: collecting granules with effects of qi stagnation and stomachache, grinding, adding water, ultrasonic treating, and filtering;
2) preparation of control solutions: taking a proper amount of reference substance, and preparing a reference substance solution by using methanol;
3) and (3) determination: precisely absorbing a reference solution and a test solution respectively, injecting into a liquid chromatograph, using octadecylsilane chemically bonded silica as a filler, acetonitrile and a phosphoric acid solution with the mass concentration of 0.1% as a mobile phase in a chromatographic column, and collecting detection data of 90min at a detection wavelength of 230nm and a column temperature of 30 ℃;
4) and (3) verification: the specificity, precision, repeatability and stability are verified;
5) and (3) respectively carrying out data import, multipoint correction and data matching on the liquid chromatogram of the test solution and the reference solution by utilizing a Chinese medicine chromatogram fingerprint similarity evaluation system of the State pharmacopoeia Committee to obtain the characteristic spectrum.
Further, the concentration of the test solution is 0.2g/ml, the power of ultrasonic treatment is 500W, and the frequency is 40 kHz.
Further, the reference substance is paeoniflorin, naringin, neohesperidin, liquiritin, ammonium glycyrrhizinate, tetrahydropalmatine, corydaline A, saikosaponin a or saikosaponin d, and the concentration of the reference substance solution is 25 μ g/ml.
Further, the mobile phase gradient elution procedure was as follows: when acetonitrile is represented by A, a phosphoric acid solution with the mass concentration of 0.1% is represented by B, the mobile phase is 10-23% of A and 90-77% of B in volume fraction in 0-45 min, the mobile phase is 23-28% of A and 77-72% of B in volume fraction in 45-46 min, the mobile phase is 28% of A and 72% of B in volume fraction in 46-60 min, the mobile phase is 28-80% of A and 72-20% of B in volume fraction in 60-80 min, and the mobile phase is 80% of A and 20% of B in volume fraction in 80-90 min.
The invention provides application of the establishing method of the qi stagnation stomachache granule characteristic spectrum in quality detection and quality control of the qi stagnation stomachache granule.
The invention has the beneficial effects that: the HPLC characteristic spectrum established by the qi stagnation stomachache granules represents most of pharmacological active ingredients of the qi stagnation stomachache granules, can reflect the quality profile of the qi stagnation stomachache granules, and can be used as one of standard indexes for quality detection and quality control of the qi stagnation stomachache granules; the method disclosed by the invention has the advantages of high stability, high precision, good repeatability and the like, and can effectively ensure the stability and uniformity of the quality of the qi stagnation stomachache granules, thereby being beneficial to improving the effectiveness and safety of clinical medication of the medicine.
Drawings
FIG. 1 is a chromatogram of qi-stagnation stomachache granule at wavelengths of 200nm, 220nm, 230nm, 240nm and 250nm, respectively.
Fig. 2 DAD full scan 3D picture of qi stagnation stomachache granules.
FIG. 3 is a specificity inspection chromatogram.
FIG. 4 is a chromatogram map of chromatogram peak location of qi stagnation stomachache granule. (S1: paeoniflorin, S2: naringin, S3: neohesperidin, S4: liquiritin, S5: ammonium glycyrrhizinate, S6: tetrahydropalmatine, S7: corydaline, S8: saikosaponin a, S9: saikosaponin d, S10: test solution)
Fig. 5 is a characteristic spectrum of qi stagnation stomachache granules established by the scheme.
Detailed Description
The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments, and it should be understood that the described embodiments are some, but not all, embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In addition, the technical features involved in the different embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The instruments and reagents used in this implementation are as follows:
high performance liquid chromatograph: agilent 1260Infinity, column: agilent Eclipse Plus-C18 (4.6X 250mm,5 μm), Agilent ECLIPSE XDB-C18 (4.6X 250mm,5 μm), Agilent ZORBAX SB-C18 (4.6X 250mm,5 μm), electronic analytical balance Mettler XS105 (one hundred thousand), ME204E (one ten thousand), methanol for chromatographic purity, phosphoric acid for analytical purity, Seimer Feishell technology (China) Co., Ltd;
paeoniflorin (95.10%): batch No. 110736-;
naringin (91.70%): lot numbers 110722 and 201815, China institute for food and drug testing;
neohesperidin (99.40%): lot No. 111857-;
glycyrrhizin (95.00%): lot No. 111610-;
ammonium glycyrrhizinate (97.70%): lot numbers 110731-201720, China institute for food and drug testing;
tetrahydropalmatine (99.80%): batch No. 110726-;
corydalis A (98.00%): lot No. 4099, podan de;
saikosaponin a (98.35%): batch number MUST-18120313, Dowman Biotech, Inc.;
saikosaponin d (96.30%): batch No. 110778-.
The invention provides a method for establishing a characteristic spectrum of qi stagnation stomachache granules, which comprises the following specific implementation methods and results:
firstly, preparing a test solution:
1g of qi stagnation stomachache granules are taken, ground, extracted by adding a solvent and filtered for standby; the extraction method can be ultrasonic or reflux, and the ultrasonic is preferably used as the extraction method; the extraction solvent can be water, methanol or ethanol aqueous solution, and water is preferably used as the extraction solvent.
Secondly, measurement:
precisely absorbing a sample solution and injecting the sample solution into a liquid chromatograph, wherein a chromatographic column takes octadecylsilane chemically bonded silica as a filler, mobile phases comprise acetonitrile (mobile phase A) and a phosphoric acid solution (mobile phase B) with the mass concentration of 0.1 percent, the conditions of a mobile phase gradient elution program are shown in table 1, the column temperature is 30 ℃, the detection wavelengths are set to be 5 wavelengths of 200nm, 220nm, 230nm, 240nm and 250nm for simultaneous detection, and the detection data of 90min are collected.
As shown in figure 1, the spectrogram base line under the condition of 230nm is stable, and meanwhile, a DAD detector is adopted to perform full-wavelength scanning, as shown in figure 2, the chromatogram information under the condition is rich, and the chromatogram peak arrangement is uniform, so that 230nm is selected as the optimal absorption wavelength of the test sample.
TABLE 1
| Time (minutes) | Mobile phase A (%) | Mobile phase B (%) |
| 0～45 | 10→23 | 90→77 |
| 45～46 | 23→28 | 77→72 |
| 46～60 | 28 | 72 |
| 60～80 | 28→80 | 72→20 |
| 80～90 | 80 | 20 |
Third, the methodology validation study
1. Specificity
Preparing the granules for treating stomachache due to qi stagnation by the above method; and water is used as a blank solution, and sample injection detection is carried out according to a determined chromatographic condition, as shown in figure 3, the blank solution basically has no interference on the characteristic spectrum of the qi stagnation stomachache granules within 80 minutes, which indicates that the method has good specificity.
2. Precision degree
The granules for treating stomachache caused by qi stagnation are taken, the test solution is prepared according to the method, the parallel operation is carried out on different test equipment, the spectrum is obtained by measurement, and the RSD (mean shift decomposition) is less than 2 percent by comparing the relative retention time of all common peaks, which indicates that the method has good precision.
3. Repeatability of
The granules for treating stomachache due to qi stagnation are taken, the sample solution is prepared according to the method, the sample is continuously injected for 6 times respectively, and the test results show that the method has good repeatability as RSD is less than 2% by comparing the relative retention time of all common peaks.
4. Stability of
And (3) taking the granules for treating qi stagnation and stomachache, preparing a test solution according to the method, placing the prepared test solution for 0, 2, 4, 8, 12 and 24 hours for sample injection measurement, comparing the relative retention time of all common peaks, and determining that the RSD is less than 2 percent, which indicates that the method has good stability.
Fourthly, preparing and measuring a reference substance solution:
respectively taking 1.25g of paeoniflorin, naringin, neohesperidin, liquiritin, ammonium glycyrrhizinate, tetrahydropalmatine, corydaline A, saikoside a, and saikoside d, and preparing into corresponding reference solutions with 50ml of methanol;
measuring according to the above determination method to obtain corresponding spectra, respectively, and comparing with the test solution spectrogram, as shown in FIG. 4, 5 components including paeoniflorin, naringin, neohesperidin, liquiritin, and ammonium glycyrrhizinate can be identified in the test solution spectrogram.
Fifthly, establishing a characteristic map
A Chinese pharmacopoeia committee promulgated traditional Chinese medicine chromatogram fingerprint similarity evaluation software system (2012.130723 version) is adopted, and HPLC chromatogram peaks of at least 5 batches of qi stagnation stomachache granules are automatically matched to establish a characteristic spectrum to obtain a graph 5.
5 peaks can be identified in the characteristic map of the test sample, wherein peak 1 is paeoniflorin, peak 2 is naringin, peak 3 is neohesperidin, peak 4 is liquiritin, and peak 5 is ammonium glycyrrhizinate. The peak 1 is designated as the S peak, and the relative retention time of the remaining characteristic peak to the S peak is calculated, which should be within + -10% of the specified value. The relative retention times are recorded in table 2.
TABLE 2
| Peak(s) | |
|
|
Peak 4 | |
| Relative retention time | 1.00 | 1.43 | 1.91 | 2.16 | 3.70 |
In conclusion, the establishment method of the characteristic map of the qi stagnation stomachache granules and the relative retention time value of the characteristic compound are specified, so that the quality profile of the qi stagnation stomachache granules can be comprehensively reflected, and the effectiveness and the safety of clinical medication of the qi stagnation stomachache granules are effectively ensured.
While embodiments of the invention have been disclosed above, it is not limited to the applications listed in the description and the embodiments, which are fully applicable in all kinds of fields of application of the invention, and further modifications may readily be effected by those skilled in the art, so that the invention is not limited to the specific details without departing from the general concept defined by the claims and the scope of equivalents.
Claims (5)
1. A method for establishing a characteristic spectrum of qi stagnation stomachache granules is characterized by comprising the following steps:
1) preparation of a test solution: collecting granules with effects of qi stagnation and stomachache, grinding, adding water, ultrasonic treating, and filtering;
2) preparation of control solutions: taking a proper amount of reference substance, and preparing a reference substance solution by using methanol;
3) and (3) determination: precisely absorbing a reference solution and a test solution respectively, injecting into a liquid chromatograph, using octadecylsilane chemically bonded silica as a filler, acetonitrile and a phosphoric acid solution with the mass concentration of 0.1% as a mobile phase in a chromatographic column, and collecting detection data of 90min at a detection wavelength of 230nm and a column temperature of 30 ℃;
4) and (3) verification: the specificity, precision, repeatability and stability are verified;
5) and (3) respectively carrying out data import, multipoint correction and data matching on the liquid chromatogram of the test solution and the reference solution by utilizing a Chinese medicine chromatogram fingerprint similarity evaluation system of the State pharmacopoeia Committee to obtain the characteristic spectrum.
2. The method for establishing the characteristic spectrum of qi-stagnation stomachache granules according to claim 1, wherein the concentration of the test solution is 0.2g/ml, the power of ultrasonic treatment is 500W, and the frequency is 40 kHz.
3. The method for establishing the characteristic spectrum of qi-stagnation stomachache granules according to claim 1, wherein the reference substance is paeoniflorin, naringin, neohesperidin, liquiritin, ammonium glycyrrhizinate, tetrahydropalmatine, corydaline A, saikosaponin a or saikosaponin d, and the concentration of the reference substance solution is 25 μ g/ml.
4. The method for establishing the characteristic map of the qi stagnation stomachache granules according to claim 1, wherein the mobile phase gradient elution procedure is as follows: when acetonitrile is represented by A, a phosphoric acid solution with the mass concentration of 0.1% is represented by B, the mobile phase is 10-23% of A and 90-77% of B in volume fraction in 0-45 min, the mobile phase is 23-28% of A and 77-72% of B in volume fraction in 45-46 min, the mobile phase is 28% of A and 72% of B in volume fraction in 46-60 min, the mobile phase is 28-80% of A and 72-20% of B in volume fraction in 60-80 min, and the mobile phase is 80% of A and 20% of B in volume fraction in 80-90 min.
5. Use of the method for establishing the characteristic map of qi-stagnation stomachache granules according to any one of claims 1 to 4 in quality detection and quality control of the qi-stagnation stomachache granules.
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Application publication date: 20210831 |