CN110579539B - Establishing method of fingerprint of Huaganjian tea - Google Patents

Establishing method of fingerprint of Huaganjian tea Download PDF

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CN110579539B
CN110579539B CN201910625255.XA CN201910625255A CN110579539B CN 110579539 B CN110579539 B CN 110579539B CN 201910625255 A CN201910625255 A CN 201910625255A CN 110579539 B CN110579539 B CN 110579539B
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冯育林
吴欢
张武岗
李丹
侯金才
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Jingjinji Lianchuang Drug Research Beijing Co ltd
Shenwei Pharmaceutical Group Co Ltd
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Abstract

The invention relates to the technical field of traditional Chinese medicine extraction, and particularly discloses a method for establishing a fingerprint of Hua gan Jiang, which comprises the following steps: a. preparation of a test solution: weighing pericarpium Citri Reticulatae viride, pericarpium Citri Tangerinae, radix Paeoniae, cortex moutan, fructus Gardeniae preparata, Alismatis rhizoma and Bulbus Fritillariae Thunbergii according to the mass ratio of each component in the decoction, decocting in water, and filtering to obtain filtrate as sample solution; b. preparation of control solutions: dissolving hesperidin, paeoniflorin, paeonol, geniposide and adenosine with solvent to obtain mixed solution as reference solution; c. and (3) high performance liquid chromatography detection: detecting the sample solution and the reference solution by high performance liquid chromatography respectively to obtain fingerprint of HUAGAN decoction. The invention can carry out qualitative analysis on chemical components in the Hua Gao Jiang, provides basis for evaluating the quality of the Hua Gao Jiang, establishes a uniform quality evaluation standard for the Hua Gao Jiang, and lays a foundation for excavating drug effect substances of the Hua Gao Jiang.

Description

Establishing method of fingerprint of Huaganjian tea
Technical Field
The invention relates to the technical field of traditional Chinese medicine detection, in particular to a method for establishing fingerprint of Hua gan Jiang.
Background
The liver-transforming decoction is a classic and famous traditional Chinese medicine prescription, is named in Jingyue quan Shu of Zhangjing in the Ming Dynasty, consists of pericarpium citri reticulatae viride, pericarpium citri reticulatae, radix paeoniae alba, fried fructus gardeniae, cortex moutan, rhizoma alismatis and thunberg fritillary bulb, is mainly used for treating liver injury caused by anger qi, qi reversal and fire stirring, hypochondriac pain and fullness, dysphoria with smothery sensation and blood stirring, and has the biggest characteristics of relieving depression of liver qi, calming qi reversal and dispersing stagnated fire, and pathological changes of liver depression are common clinically, and the liver-transforming decoction has special effects, proper application and addition and subtraction method and.
SDETP, the full name of Standard Decortion Extract by Traditional Preparation, Chinese means Standard Decoction substance, it means the Traditional Chinese medicine substance prepared according to the classic famous prescription Preparation method recorded in ancient medical books, SDETP is the contrast substance linking the Traditional Preparation method of classic famous prescription and modern industrial production process, it is the evaluation Standard bar of the basic consistency between the two, modern science is to demonstrate the ingredient with curative effect in the prescription through the analysis and establishment Standard of SDETP, form the contrast with the analysis test means adopted by chemical drugs. The material standard of the classical famous prescription is guided by the theory of traditional Chinese medicine, clinical application is taken as a basis, the traditional preparation method is followed, the modern scientific technology is combined, the quality of the raw medicinal materials is controlled from the source, and the extract which is uniform, stable and controllable in quality is prepared by the standardized processes of medicinal material pretreatment, decoction piece processing, decoction, concentration, drying and forming and the like, and is the standard for evaluating whether the preparation is consistent with the medicinal materials used in the traditional Chinese medicine clinic.
At present, the quality standards of traditional Chinese medicines are difficult to unify, the main effective components of the same traditional Chinese medicine are different when the same traditional Chinese medicine is used for treating different diseases, and the classical famous prescription requires that the quality of medicinal materials in a prescription is uniform and stable, so that the determination of the primordium of each traditional Chinese medicine before research and development has very important significance in deep examination and confirmation of the clinical medication condition, the source change of the medicinal materials and the revision condition of Chinese pharmacopoeia of the calendar edition. The quality standard of the traditional Chinese medicine is mainly to measure the substance standard and the content of effective parts, but the traditional Chinese medicine components are complex, and the quality of the traditional Chinese medicine is difficult to clarify by a single effective component or effective parts, so that the focus of attention is on how to establish the substance standard of the classical famous formula of liver decoction and whether to establish a relatively recognized evaluation standard.
Disclosure of Invention
Aiming at the problems that the existing material reference quality standard of the Hua-gan Jiang can not be unified, and the accepted evaluation standard is lacked, the invention provides a method for establishing the fingerprint of the Hua-gan Jiang.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a method for establishing a fingerprint of Hua Gan Jian comprises the following steps:
a. preparation of a test solution: weighing pericarpium Citri Reticulatae viride, pericarpium Citri Tangerinae, radix Paeoniae, cortex moutan, fructus Gardeniae preparata, Alismatis rhizoma and Bulbus Fritillariae Thunbergii according to the mass ratio of each component in the decoction, decocting in water, and filtering to obtain filtrate as sample solution;
b. preparation of control solutions: dissolving hesperidin, paeoniflorin, paeonol, geniposide and adenosine with solvent to obtain mixed solution as reference solution;
c. and (3) high performance liquid chromatography detection: respectively detecting the test solution and the reference solution by using high performance liquid chromatography to obtain the fingerprint of the Hua Gao Jiang, wherein the conditions of the high performance liquid chromatography are as follows:
stationary phase: a C18 chromatography column;
mobile phase: the mobile phase B is methanol, and the phase A is 0.1-0.2 wt% of phosphoric acid solution;
the gradient elution conditions were: 0-13min, 5-12 vol% of phase B and 95-88 vol% of phase A; 13-15min, 12-17 vol% of phase B and 88-83% of phase A; 15-35min, 17-20 vol% of phase B and 83-80 vol% of phase A; 35-40min, 20-28 vol% of phase B and 80-72 vol% of phase A; 40-45min, 28-35 vol% of phase B and 72-65 vol% of phase A; 45-55min, 35-52 vol% of phase B and 65-48 vol% of phase A; 55-60min, 52-65 vol% of phase B and 48-35 vol% of phase A; 60-70min, 62-90 vol% of phase B and 38-10 vol% of phase A;
70-75min, 90-95 vol% of phase B and 10-5 vol% of phase A.
Compared with the prior art, the establishing method of the Hua Gao Jiang fingerprint provided by the invention has the advantages that the similarity between the obtained Hua Gao Jiang fingerprint and the comparison fingerprint is more than 0.94, the method has good stability and repeatability, the difference between different groups and batches is small, the uniformity and the stability between the same batch are good, the obtained fingerprint has large information amount and rich spectral peak information, 55 common peaks are calibrated in the fingerprint, most components in the Hua Gao Jiang decoction are effectively separated, the integral medicinal component information of the Hua Gao Jiang can be completely provided, the integral quality attribute of the Hua Gao Jiang can be reflected by the fingerprint, the specific quality standard of the Hua Gao Jiang decoction can be established, and a foundation is laid for the identification of the later-stage Hua decoction components and the excavation of medicinal effect substances.
The stationary phase adopts a C18 chromatographic column, the phase B of the mobile phase is methanol, the phase A is 0.1-0.2 wt% of phosphoric acid solution, the combination of the stationary phase and the mobile phase is matched with specific elution conditions, the separation degree of each active ingredient in the decoction of the Huagan decoction can be increased, the number and the separation degree of the common peaks of the fingerprint spectra can be effectively improved, the information content of the fingerprint spectra of the Huagan decoction is increased, the peak shape and the chromatographic peak response of the common peaks are good, even if water is used as an extraction solvent and the extraction solution is directly subjected to high performance liquid chromatography, the chromatographic effect can be achieved, the addition of an organic extraction solvent, an organic extraction solvent and the like is omitted, and the universality and the effectiveness of fingerprint detection are ensured.
The method for establishing the fingerprint of Huagan Jiang can qualitatively analyze certain chemical components in the material standard, provides important basis for evaluating the quality of the material standard, can establish a unique SDETP standard for the method, and provides a professional reference method for developing the ancient classical formulation, namely Huagan Jiang.
Preferably, the decocting process with water in step a is as follows: adding water 10-12 times the weight of HUAGAN decoction, soaking for 25-30min, boiling with strong fire, and decocting with slow fire for 25-30 min.
The establishing method of the fingerprint of the Hua-gan decoction ensures the ancient decoction process, the original decoction is injected into a liquid phase for analysis, the ancient decoction process is improved, and the specific decoction mode and the decoction time are set, so that the medicine can be decocted to the optimal state, and the extract yield of the medicine can be maximized.
Preferably, the solvent in step b is methanol.
Preferably, the content of hesperidin in the control solution is 0.103mg/ml, the content of paeoniflorin is 0.102mg/ml, the content of paeonol is 0.101mg/ml, the content of geniposide is 0.103mg/ml and the content of adenosine is 0.152 mg/ml.
Preferably, the stationary phase of the high performance liquid chromatography in the step c adopts a Diamonsil c18 chromatographic column; the mobile phase B of the high performance liquid chromatography is methanol, and the phase A is 0.1 wt% phosphoric acid solution.
The liver-clearing decoction has complex and various chemical components in the basis, mainly contains compounds such as flavonoid, glycosides and organic acids, and the like, and when methanol-0.1 percent phosphoric acid water is selected as a mobile phase, the pressure of a chromatograph is moderate, and the chromatographic peak separation degree of a water decoction is higher.
Preferably, the flow rate of the mobile phase of the high performance liquid chromatography in the step c is 1-1.5ml/min, the column temperature is 40-42 ℃, and the detection wavelength is 230-240 nm.
The column temperature and the flow rate of the mobile phase of the chromatographic column can be set to increase the separation degree of corresponding components in the chromatogram.
Preferably, the mobile phase flow rate is 1 ml/min.
The flow rate of 1ml/min just meets the separation speed of the chromatographic column to each component in the decoction of the Hua gan Jiang.
Preferably, the column temperature is 40 ℃ and the detection wavelength is 238 nm.
Under the detection wavelength of 238nm, the chromatogram base line is relatively stable, the number of common peaks is large, the separation degree of the reference peak and each common peak is good, and part of peaks have high response values.
Drawings
FIG. 1 is a high performance liquid chromatogram of a Hua-gan Jiang test solution prepared in an example of the present invention;
FIG. 2 is a high performance liquid chromatogram of a control solution in an example of the invention;
FIG. 3A is a high performance liquid chromatogram of a test solution prepared from an aqueous blank solution according to an example of the present invention;
FIG. 3B is a high performance liquid chromatogram of a test solution prepared from a single green tangerine orange peel sample according to an embodiment of the present invention;
FIG. 3C is a high performance liquid chromatogram of a test solution prepared from a single sample of dried orange peel in an embodiment of the present invention;
FIG. 3D is a high performance liquid chromatogram of a test solution prepared from a single white peony root sample according to an embodiment of the present invention;
FIG. 3E is a high performance liquid chromatogram of a sample solution prepared from a single sample of moutan bark;
FIG. 3F is a high performance liquid chromatogram of a test solution prepared from a single gardenia sample according to an embodiment of the present invention;
FIG. 3G is a high performance liquid chromatogram of a test solution prepared from a single sample of Alismatis rhizoma in an example of the present invention;
FIG. 3H is a high performance liquid chromatogram of a test solution prepared from a single sample of Fritillaria thunbergii in an embodiment of the present invention;
FIG. 4 is a high performance liquid chromatogram of a 15-lot liver decoction test sample solution in an example of the present invention; wherein R is a consensus pattern spectrum;
FIG. 5 is a fingerprint of Hua gan Jiang obtained in accordance with an embodiment of the present invention;
common peaks include 2, adenosine, 30, geniposide, 31, paeoniflorin, 39, hesperidin, 49 and paeonol.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Examples
Establishing method of fingerprint of Huaganjian tea
1. Instrument and reagent
The instrument comprises the following steps: shimadzu HPLC LC-20AT system (equipped with binary solvent pump, autosampler, online vacuum degasser, PDA detector, Labsolution chromatography workstation), AL-104 analytical balance (mettlerlyton shanghai ltd), hufu brand automatic drug decocting pot (ceramic pot 2L);
reagent testing: the green tangerine orange peel, the dried tangerine peel, the white paeony root, the gardenia, the tree peony bark, the oriental waterplantain rhizome and the thunberg fritillary bulb decoction pieces are certified as genuine products by food and drug inspection in Nanchang city, and accord with the standard of 2015 edition of Chinese pharmacopoeia, samples are reserved in 324 houses of national engineering research center of manufacturing technology of traditional Chinese medicine solid preparation of Jiangxi Chinese medicine university, the collected green tangerine orange peel, dried tangerine peel, white paeony root, gardenia, tree peony bark, oriental waterplantain rhizome and thunberg fritillary bulb decoction piece information is shown in table 1, the decoction pieces are randomly combined according to batch numbers to prepare 15 batches of hepatitis decoction samples, and the specific combination information is shown in table 2;
TABLE 1
Figure BDA0002126885920000061
Figure BDA0002126885920000071
Figure BDA0002126885920000081
Figure BDA0002126885920000091
Figure BDA0002126885920000101
TABLE 2 randomly combined 15 batches of liver-decocting formulation
Figure BDA0002126885920000102
Figure BDA0002126885920000111
The reference products hesperidin (batch number: 110721-;
acetonitrile, methanol (Fisher, chromatographic alcohol), phosphoric acid (Guangdong Guanghua science and technology, Inc., analytical purity), and experimental water as Drech distilled water.
2. Method and results
Preparing a test solution: weighing 7.5g of green tangerine orange peel, dried orange peel and white paeony root respectively, 5.63g of moutan bark, gardenia and oriental waterplantain rhizome respectively and 10g of thunberg fritillary bulb, adding 500ml of water to soak for 30 minutes, boiling with strong fire, then decocting with slow fire for 25min, filtering with a 200-mesh nylon filter screen while hot, taking a proper amount of filtrate and filtering with a 0.22-micron microporous filter membrane, and finally obtaining the filtrate which is the sample solution, and freezing and storing the sample solution at the temperature of-40 ℃ for later use;
preparation of a reference solution: accurately weighing hesperidin, paeoniflorin, paeonol, geniposide and adenosine reference substances 10.31mg, 10.23mg, 10.11mg, 10.34mg and 15.21mg, placing in a 100ml volumetric flask, adding pure methanol to constant volume to prepare a mixed reference substance solution containing 0.103mg of hesperidin, 0.102mg of paeoniflorin, 0.101mg of paeonol, 0.103mg of geniposide and 0.152mg of adenosine in 1ml, storing at 2 ℃ for later use, and filtering with a 0.22 mu m microfiltration membrane before measurement;
detection conditions of high performance liquid chromatography: the method adopts Shimadzu LC-20AT high performance liquid chromatograph, the stationary phase is a Diamonsil c18 chromatographic column (4.6X 250mm, 5 μm), and gradient elution is carried out by taking methanol (B) -0.1% phosphoric acid water solution (A) as a mobile phase, and the gradient elution conditions are as follows: 0-13min, 5-12 vol% of phase B and 95-88 vol% of phase A; 13-15min, 12-17 vol% of phase B and 88-83% of phase A; 15-35min, 17-20 vol% of phase B and 83-80 vol% of phase A; 35-40min, 20-28 vol% of phase B and 80-72 vol% of phase A; 40-45min, 28-35 vol% of phase B and 72-65 vol% of phase A; 45-55min, 35-52 vol% of phase B and 65-48 vol% of phase A; 55-60min, 52-65 vol% of phase B and 48-35 vol% of phase A; 60-70min, 62-90 vol% of phase B and 38-10 vol% of phase A; 70-75min, 90-95 vol% of phase B and 10-5 vol% of phase A; column temperature 40 ℃, flow rate: 1ml/min, wavelength 238 nm.
Performing high performance liquid chromatography detection on the prepared test solution and the prepared reference solution respectively to obtain a chromatogram of the test solution as shown in FIG. 1 and a chromatogram of the reference solution as shown in FIG. 2.
3. Methodology investigation
Precision: taking S1 batch liver decoction water decoction sample solution, carrying out sample injection for 6 times continuously according to the detection conditions of the high performance liquid chromatography in the embodiment, recording a spectrogram, taking geniposide as a reference peak, wherein the RSD of each characteristic common peak relative retention time is less than 1%, and the RSD of each relative peak area is less than 3%, which indicates that the used instrument has good precision and meets the technical requirements of fingerprint spectrum.
Repeatability: taking 6 parts of S1 batch liver decoction water decoction sample solution, taking geniposide as a reference peak according to the detection conditions of high performance liquid chromatography in the embodiment, wherein RSD of each characteristic common peak relative retention time is less than 1%, and RSD of each relative peak area is less than 4%, which shows that the method has good repeatability and meets the technical requirements of fingerprint spectrum.
Stability: taking S1 batches of decoction sample solutions of the Huagan decoction placed at room temperature, determining chromatograms at 0, 4, 8, 12, 16, 20 and 24 hours respectively according to the detection conditions of the high performance liquid chromatography in the embodiment, and taking gardenoside as a reference peak, wherein the results show that the RSD of the relative retention time of all characteristic common peaks is less than 1%, and the RSD of the relative peak area is less than 5%, which indicates that the stability of the test solution in 24 hours is good.
And (3) special investigation: according to the sample solution preparation method in this embodiment, single sample solutions of blank aqueous solution, pericarpium Citri Reticulatae viride, pericarpium Citri Tangerinae, radix Paeoniae alba, cortex moutan, fructus Gardeniae, Alismatis rhizoma, and Bulbus Fritillariae Thunbergii are prepared respectively for high performance liquid chromatography detection, with the chromatographic conditions unchanged, sample introduction and chromatogram recording to obtain 8 chromatograms as shown in FIGS. 3A-H.
4. Establishment of fingerprint of Hua gan Jian
Establishing a fingerprint spectrum: according to the method of item 2 in this example, 15 batches of the randomly combined liver decoction test sample solutions are prepared, the high performance liquid chromatography conditions in this example are adopted for measurement, chromatograms are recorded, the high performance liquid chromatograms of the 15 batches of the liver decoction test sample solutions are shown in fig. 4, the chromatogram data are introduced into software 2004A of a traditional Chinese medicine chromatogram fingerprint similarity evaluation system, reference spectra are set, and fingerprints are generated, as shown in fig. 5;
selection of reference peaks: in 15 batches of sample HPLC finger prints, the separation degree of the geniposide chromatographic peak is good, the peak area is large, no negative interference exists, and the retention time is proper, so that the No. 30 geniposide chromatographic peak is selected as a reference peak;
common peak calibration: introducing HPLC chromatogram of 15 batches of decoction of decocted liver into a 2004A version of a Chinese medicinal chromatogram fingerprint similarity evaluation system for performing chromatogram peak matching, calibrating 55 common peaks after treatment, and identifying 5 common peaks which are respectively adenosine, geniposide, paeoniflorin, hesperidin and paeonol;
and (3) similarity evaluation: by utilizing software of 2004A version of a Chinese medicine chromatogram fingerprint similarity evaluation system, RSD of relative retention time of characteristic common peaks in 15 batches of liver decoction test sample chromatograms is less than 2%, RSD of relative peak areas is less than 5%, and chromatogram similarity is more than 0.94, so that the batch-to-batch difference is small, the preparation process is reliable and stable, the method is accurate, and the analysis result is shown in Table 3.
TABLE 315 comparison of similarity of solutions of the samples of the batch liver decoction
Figure BDA0002126885920000131
Figure BDA0002126885920000141
In the decoction for removing the liver, 5 common peaks are identified, wherein hesperidin is a main component of green tangerine orange peel and dried tangerine peel, the content of the hesperidin in the decoction is high, the jasminoidin is a main component of gardenia, is a reference peak of a fingerprint spectrum of the decoction, the peak area is large, the separation degree is good, and the separation effect of paeoniflorin, adenosine and paeonol is not similar to that of hesperidin and geniposide, so that the method selects the hesperidin and the geniposide as index components, and provides reference opinions for establishing standards for developing the decoction for removing the liver by enterprises in the future.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.

Claims (8)

1. A method for establishing a fingerprint of Hua Gan Jian is characterized in that: the method comprises the following steps:
a. preparation of a test solution: weighing pericarpium Citri Reticulatae viride, pericarpium Citri Tangerinae, radix Paeoniae, cortex moutan, fructus Gardeniae preparata, Alismatis rhizoma and Bulbus Fritillariae Thunbergii according to the mass ratio of each component in the decoction, decocting in water, and filtering to obtain filtrate as sample solution;
b. preparation of control solutions: dissolving hesperidin, paeoniflorin, paeonol, geniposide and adenosine with solvent to obtain mixed solution as reference solution;
c. and (3) high performance liquid chromatography detection: respectively detecting the test solution and the reference solution by using high performance liquid chromatography to obtain the fingerprint of the Hua Gao Jiang, wherein the conditions of the high performance liquid chromatography are as follows:
stationary phase: a C18 chromatography column;
mobile phase: the mobile phase B is methanol, and the phase A is 0.1-0.2 wt% of phosphoric acid solution;
the gradient elution conditions were: 0-13min, 5-12 vol% of phase B and 95-88 vol% of phase A; 13-15min, 12-17 vol% of phase B and 88-83% of phase A; 15-35min, 17-20 vol% of phase B and 83-80 vol% of phase A; 35-40min, 20-28 vol% of phase B and 80-72 vol% of phase A; 40-45min, 28-35 vol% of phase B and 72-65 vol% of phase A; 45-55min, 35-52 vol% of phase B and 65-48 vol% of phase A; 55-60min, 52-65 vol% of phase B and 48-35 vol% of phase A; 60-70min, 62-90 vol% of phase B and 38-10 vol% of phase A; 70-75min, 90-95 vol% of phase B and 10-5 vol% of phase A.
2. The method for establishing the fingerprint of Hua gan Jiang according to claim 1, wherein: the water adding and decocting process in the step a comprises the following steps: adding water 10-12 times the weight of HUAGAN decoction, soaking for 25-30min, boiling with strong fire, and decocting with slow fire for 25-30 min.
3. The method for establishing the fingerprint of Hua gan Jiang according to claim 1, wherein: the solvent in the step b is methanol.
4. The method for establishing the fingerprint of Hua gan Jiang according to claim 1, wherein: the content of hesperidin in the control solution is 0.103mg/ml, the content of paeoniflorin is 0.102mg/ml, the content of paeonol is 0.101mg/ml, the content of geniposide is 0.103mg/ml, and the content of adenosine is 0.152 mg/ml.
5. The method for establishing the fingerprint of Hua gan Jiang according to claim 1, wherein: the stationary phase of the high performance liquid chromatography in the step c adopts a Diamonsil c18 chromatographic column; the mobile phase B of the high performance liquid chromatography is methanol, and the phase A is 0.1 wt% phosphoric acid solution.
6. The method for establishing the fingerprint of Hua gan Jiang according to claim 1, wherein: the flow rate of the mobile phase of the high performance liquid chromatography in the step c is 1-1.5ml/min, the column temperature is 40-42 ℃, and the detection wavelength is 230-240 nm.
7. The method for establishing the fingerprint of Hua gan Jiang according to claim 6, wherein: the mobile phase flow rate was 1 ml/min.
8. The method for establishing the fingerprint of Hua gan Jiang according to claim 6, wherein: the column temperature was 40 ℃ and the detection wavelength was 238 nm.
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CN102818861A (en) * 2012-05-10 2012-12-12 丽珠医药集团股份有限公司 Quality control method and application of Qingdu Anshen capsule
CN103961646A (en) * 2014-05-13 2014-08-06 张旭 Traditional Chinese medicinal preparation composition for nourishing qi and yin and activating blood circulation to remove stasis
CN108888686A (en) * 2018-07-06 2018-11-27 海王(湖北)中医药研究总院有限公司 It is a kind of to treat stomachache, hypochondriac pain, gastroenteritic ulcer, the Chinese medical extract of depression and its preparation method and application
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