CN-122005706-A - Qishenpngji granule for treating ventricular premature beat and quality detection method thereof

CN122005706ACN 122005706 ACN122005706 ACN 122005706ACN-122005706-A

Abstract

The invention discloses a Qishen Pingji granule and a quality detection method thereof, the invention screens out the best molding process of Qishen Pingji particles through a large number of experiments. The invention screens out the optimal thin-layer chromatography unfolding condition and performs qualitative identification research on the salvia miltiorrhiza, radix astragali preparata, szechuan lovage rhizome and the astragalus root in the quality detection method of the Qishen palpitation granule. And the optimal chromatographic conditions such as fluidity composition, gradient elution mode and the like are screened out through a large number of experiments, a fingerprint detection method with high precision, good stability and high accuracy is established, and the content of effective components such as calycosin, ferulic acid, dihydroquercetin, ammonium glycyrrhizate, nardostachyn and the like can be measured simultaneously, so that a quality detection method is provided for ensuring the safety and effectiveness of the effective components.

Inventors

LIU CHUNLING
WU LEI
ZHANG LINNING
LI XINQI
Zhao Baihao
Ji Keman
SHAO MENGQI

Assignees

江苏省中医院

Dates

Publication Date: 20260512
Application Date: 20260123
Priority Date: 20251111

Claims (10)

1. The astragalus-ginseng palpitation relieving granule for treating ventricular premature beat is characterized by being prepared by the following method: Adding 6-10 times of water into radix astragali preparata, radix codonopsis pilosulae, radix ophiopogonis, radix asparagi, radix salviae miltiorrhizae, rhizoma ligustici wallichii, poria cocos, rhizoma pinellinae praeparata and rhizoma nardostachyos, soaking, decocting and extracting for 20-120 min, filtering, concentrating the filtrate under reduced pressure, taking a proper amount of dextrin, placing into a fluidized bed, spray-drying and granulating to obtain the Chinese medicinal preparation.
2. The astragalus-ginseng palpitation particles for treating ventricular premature beat according to claim 1, which are prepared by the following method: 15g of roasted astragalus, 10g of codonopsis pilosula, 10g of dwarf lilyturf tuber, 10g of asparagus root, 15g of red sage root, 15g of szechuan lovage rhizome, 15g of poria cocos, 10g of prepared pinellia tuber and 10g of nardostachyos root, adding water twice, adding 10 times of water for the first time, soaking 60 min, decocting 30min, filtering, adding 8 times of water for the second time, decocting 20min, filtering, concentrating the filtrate under reduced pressure to a relative density of 1.15-1.20 at 60 ℃, taking a proper amount of dextrin, placing the dextrin into a fluidized bed, setting the air inlet temperature to be 90-100 ℃, starting to feed liquid when the temperature of the material is increased to 60 ℃, controlling the feed liquid speed to be 80-150 r/min, controlling the atomization pressure to be 0.2 MPa at the outside, 0.15-MPa at the inside, ending the spraying, continuously drying at 60-70 ℃, and granulating.
3. The quality detection method of the astragalus, ginseng and palpitation relieving particles according to claim 2, which is characterized by comprising the steps of thin-layer chromatography qualitative identification, fingerprint spectrum and content measurement; the thin-layer chromatography qualitative identification comprises the thin-layer identification of radix astragali Preparata, and specifically comprises the following steps: (1) Dissolving QISHENPING palpitation granule in water, shaking with water saturated n-butanol solution, mixing n-butanol solutions, washing with ammonia solution, removing ammonia solution, evaporating to dryness, and dissolving the residue with methanol to obtain sample solution; (2) Preparing a particle without radix astragali Preparata by the same method as in claim 2, and preparing radix astragali Preparata negative control solution by the same method as in step (1); (3) Adding methanol into radix astragali Preparata control medicinal material, performing ultrasonic treatment, filtering, evaporating filtrate to dryness, dissolving residue in water, and preparing radix astragali Preparata control medicinal material solution according to the same method of step (1); (4) The three solutions are absorbed and respectively spotted on the same silica gel G thin layer plate, the upper layer solution of n-butyl alcohol-ethyl acetate-dilute ammonia is taken as a developing agent, and the developing agent is developed, taken out, dried and sprayed with 10 percent sulfuric acid ethanol solution, and heated until the spots develop clearly, and then the spots are inspected under an ultraviolet lamp 365 nm; The thin layer identification of the red sage root comprises the following specific steps: (1) Dissolving QISHENPING palpitation granule in water, adjusting pH to acidity with hydrochloric acid, extracting with ethyl acetate, mixing extractive solutions, evaporating in water bath, and dissolving the residue with methanol to obtain sample solution; (2) Preparing a granule without radix Salviae Miltiorrhizae according to the same method as in claim 2, and preparing radix Salviae Miltiorrhizae negative control solution according to the same method as in step (1); (3) Preparing a red sage root reference medicinal material solution by the same method as in the step (1); (4) Sucking the three solutions, respectively spotting on the same silica gel G thin layer plate, developing with dichloromethane-ethyl acetate-formic acid as developing agent, taking out, air drying, spraying 5% vanillin sulfuric acid solution, and heating to clear spots; the thin-layer identification of the ligusticum wallichii comprises the following specific steps: (1) Dissolving QISHENPING palpitation granule in water, extracting with ethyl acetate, mixing the extractive solutions, evaporating in water bath, and dissolving the residue in methanol to obtain sample solution; (2) Preparing particles without Ligusticum wallichii medicinal material according to the same method as in claim 2, and preparing Ligusticum wallichii negative control solution according to the same method as in step (1); (3) Decocting rhizoma Ligustici Chuanxiong reference materials in water, filtering, extracting the filtrate with ethyl acetate, mixing the extractive solutions, evaporating in water bath, and dissolving the residue in methanol to obtain reference medicinal material solution; (4) The two solutions are absorbed and respectively spotted on the same silica gel GF254 thin layer plate, and the mixture is spread, taken out and dried by using n-hexane-ethyl acetate as a developing agent, and then is inspected under an ultraviolet lamp 365 nm, and spots with the same color are displayed on the positions corresponding to the control medicine chromatograph in the sample chromatograph.
4. The quality detection method of astragalus membranaceus, ginseng and palpitation relieving particles according to claim 3, wherein the thin-layer chromatography qualitative identification comprises the following specific steps of: (1) Dissolving QISHENPING granule in water, filtering, collecting filtrate 40mL, extracting with water saturated n-butanol solution under shaking for 4 times (40 mL times each time), mixing n-butanol solutions, washing with ammonia solution for 2 times (40 mL times each time), discarding ammonia solution, evaporating to dryness in evaporating dish, and dissolving residue with 1mL of methanol to obtain sample solution; (2) Preparing a particle without radix astragali Preparata by the same method as in claim 2, and preparing radix astragali Preparata negative control solution by the same method as in step (1); (3) Adding methanol 50 mL into radix astragali Preparata control 3 g, ultrasonic treating 30 min, filtering, evaporating filtrate, adding water 30 mL into residue to dissolve, and preparing radix astragali Preparata control solution according to the same method of step (1); (4) Absorbing 10 mu L of the three solutions, respectively spotting on a same silica gel G thin layer plate, taking an upper layer solution of n-butanol-ethyl acetate-10% diluted ammonia with a volume ratio of 4:1:5 as a developing agent, developing, taking out, airing, spraying 10% sulfuric acid ethanol solution, heating at 105 ℃ until the spots develop clearly, and placing under an ultraviolet lamp 365 nm for detection; The thin layer identification of the red sage root comprises the following specific steps: (1) Dissolving QISHENPING palpitation granule in water, collecting filtrate 40mL, adjusting pH to 2 with 10% hydrochloric acid, extracting with ethyl acetate for 3 times each time of 20 mL, mixing the extractive solutions, evaporating in water bath, and dissolving the residue with 5 mL methanol to obtain sample solution; (2) Preparing a granule without radix Salviae Miltiorrhizae according to the same method as in claim 2, and preparing radix Salviae Miltiorrhizae negative control solution according to the same method as in step (1); (3) Preparing a red sage root reference medicinal material solution by the same method as in the step (1); (4) Absorbing 10 mu L of the three solutions, respectively spotting on the same silica gel G thin layer plate, developing with methylene dichloride-ethyl acetate-formic acid with the volume ratio of 5:4:2 as developing agent, taking out, airing, spraying 5% vanillin sulfuric acid solution, and heating at 105 ℃ until spots are clear; the thin-layer identification of the ligusticum wallichii comprises the following specific steps: (1) Dissolving QISHENPING palpitation granule in water, collecting filtrate 40mL, extracting with ethyl acetate for 2 times (each time 40 mL), mixing extractive solutions, evaporating in water bath, and dissolving the residue with methanol 2mL to obtain test solution; (2) Preparing particles without Ligusticum wallichii medicinal material according to the same method as in claim 2, and preparing Ligusticum wallichii negative control solution according to the same method as in step (1); (3) Adding water 100mL into rhizoma Ligustici Chuanxiong control 2 g, decocting 0.5, h, filtering, extracting with ethyl acetate for 2 times (40 mL each time), mixing the extractive solutions, evaporating in water bath, and dissolving the residue with methanol 2 mL to obtain rhizoma Ligustici Chuanxiong control solution; (4) The three solutions are absorbed and respectively spotted on the same silica gel GF254 thin layer plate, the solution is unfolded, taken out and dried by taking the n-hexane-ethyl acetate with the volume ratio of 3:1 as the developing agent, and then the solution is placed under an ultraviolet lamp 365 nm for inspection, and spots with the same color are displayed on the positions corresponding to the chromatogram of the reference medicinal material in the chromatogram of the sample.
5. The quality detection method of the astragalus, ginseng and palpitation-suppressing granules according to claim 3, wherein the fingerprint and content measurement comprises the following steps: (1) Preparation of test solutions Taking 15 batches of astragalus root, ginseng and palpitation particles, adding water for dissolving, filtering, precisely sucking 1mL, fixing the volume of methanol into a 2mL volumetric flask, shaking and mixing uniformly, and filtering by using a 0.22 mu m microporous filter membrane to obtain 15 batches of sample solutions S1-S15; (2) Preparation of reference substance solution Precisely weighing 5 reference substances including calycosin, ferulic acid, dihydroquercetin, ammonium glycyrrhizate and nardostachyne, placing into a volumetric flask, adding methanol to dissolve and scale to obtain mixed reference substance solution; (3) Establishment of standard curve equation Sequentially injecting the mixed reference substance solutions with the series of concentrations in the step (2) into a high performance liquid chromatograph, recording a chromatogram, and drawing a standard curve equation by taking the abscissa as the concentration and the ordinate as the peak area; (4) Establishment of fingerprint Sequentially injecting 15 batches of sample solutions in the step (1) into a high performance liquid chromatograph, recording chromatograms, and then deriving the fingerprints of the sample solutions and introducing the fingerprints into 2012 edition of a traditional Chinese medicine chromatographic fingerprint similarity evaluation system; selecting chromatographic peaks existing in chromatograms of different batches of sample solutions as common peaks, calculating relative retention time and relative peak area of each common peak by using a control fingerprint generated by an average value calculation method, and marking chemical components of peaks in the control fingerprint according to the retention time of the chromatograms of the mixed reference solution; Content determination And (3) substituting the peak area of the test sample solution into the standard curve equation according to the retention time and calculating the content of each compound in the test sample solution according to the standard curve equation of the step (3).
6. The quality detection method of the Qishen Pingji granule according to claim 5 is characterized in that the preparation of the reference substance solution in the step (2) comprises precisely weighing 5 reference substance amounts of calycosin, ferulic acid, dihydroquercetin, ammonium glycyrrhizate and nardostachyne, placing the reference substance amounts in a 10 mL volumetric flask, adding methanol for dissolution and fixing the volume to a scale, and preparing the reference substance solutions with mass concentrations of 104.75, 197.37, 59.63, 987.65 and 103.48 mug/mL respectively, and diluting the reference substance solutions with methanol to corresponding 5 concentration mixed reference substance solutions.
7. The method for detecting the quality of the Qishen Pingji particles according to claim 5, wherein the chromatographic conditions in the steps (3) and (4) are as follows: The chromatographic column is a Phi Roman Luna C18 column with the specification of 250mm multiplied by 4.6mm and 5 μm, the flow rate is 1.00 mL/min, the sample injection amount is 10 mu L, the column temperature is 30 ℃, the mobile phase is acetonitrile A phase-0.1% phosphoric acid aqueous solution is B phase, the detection wavelength is 260 nm, and the gradient elution is carried out ：0～10min,2%A～12%A;10～15min,12%A～17%A;15～23min,17%A～23%A;23～31min,23%A;31～38min,23%A～32%A;38～48min,32%A～33%A;48～51min,33%A～36%A;51～53min,36%A～40%A;53～58min,40%A～42%A;58～68min,42%A～50%A;68～75min,50%A～62%A;75～85min,62%A～70%A;85～90min,70%A～80%A.
8. The quality detection method of astragalus, ginseng and palpitation particles according to claim 5, wherein the established fingerprint has 20 common peaks, and after comparison with a reference substance, the peak 5 is calycosin, the peak 6 is ferulic acid, the peak 7 is dihydroquercetin, the peak 18 is ammonium glycyrrhizate, and the peak 19 is nardostachyne.
9. The method for detecting the quality of Qishen Pingji particles according to claim 5, wherein the standard curve equation is 。
10. Use of the qi shen ping-pang particles according to claim 1 or 2 for the preparation of a medicament for the treatment of ventricular premature beat.

Description

Qishenpngji granule for treating ventricular premature beat and quality detection method thereof Technical Field The invention relates to the technical field of traditional Chinese medicines, in particular to a quality detection method of Qishen Pingji particles and a quality detection method thereof. Background The QISHENPING PINGJI granule is prepared from radix astragali Preparata, radix Codonopsis, radix Ophiopogonis, radix asparagi, saviae Miltiorrhizae radix, rhizoma Ligustici Chuanxiong, poria, rhizoma Pinelliae Preparata, and rhizoma et radix Valerianae, The early-stage researches report [ Zhang Linning, liu Chunling, and the like ] on clinical researches on treating ventricular premature beat by a method of supplementing qi, nourishing yin, promoting blood circulation and resolving phlegm, namely, the university of Nanjing traditional Chinese medicine, 2019, and collecting 53 cases of ventricular premature beat patients from the department of cardiology and hospitalized patients in the middle-level hospitals of Jiangsu province through a random control experiment, wherein the patients are randomly divided into a test group and a control group, and the two groups have no obvious difference in gender, age, combined diseases and classification of ventricular premature beat Lown's. Based on the treatment of primary diseases, the control group takes the beta receptor blocker, the test group takes the beta receptor blocker, and based on the beta receptor blocker, traditional Chinese medicine decoction (15 g radix codonopsis pilosulae, 10g radix asparagi, 10g radix ophiopogonis, 10g radix salviae miltiorrhizae, 15g rhizoma ligustici chuanxiong, 15g poria cocos, 10g rhizoma pinellinae praeparata and 10g.4 weeks are a treatment course) is added, the total effective integral after treatment is lower than that of the control group, the traditional Chinese medicine single integral after treatment is improved, and the average heart rate after treatment is reduced compared with that before treatment, the test group and the control group improve the frequency and average heart rate of ventricular premature beat, but the overall curative effect of the test group is better than that of the control group, the post-treatment Myerburg classification and heart rate variability are better than that of the control group. The clinical study proves that Liu Chunling is a main conception physician treatment empirical formula for treating ventricular premature beat, which takes 'qi-tonifying yin-nourishing, blood-activating and stasis-removing' as a treatment rule for treating the ventricular premature beat patient with deficiency of both qi and yin, and can obviously improve clinical symptoms of the patient, reduce the integral of Chinese medicine symptoms, reduce the number of premature beats, reduce the ventricular premature beat frequency, reduce Myerburg classification, improve the ventricular premature beat morphology classification and improve the heart rate variability, and the method has good safety and no obvious adverse reaction for treating the ventricular premature beat. The quality detection method of the Qishen Pingji particles is less at present, and the Qishen Pingji particles cannot be comprehensively and objectively detected, the invention combines the thin layer identification, the fingerprint spectrum and the content determination method, the Qishen Pingji granule is subjected to comprehensive quality detection, and has important significance for controlling the clinical curative effect and ensuring the safety. Disclosure of Invention The invention aims to provide astragalus-ginseng palpitation-calming particles and an objective and comprehensive quality detection method thereof. In order to achieve the above purpose, the technical scheme adopted by the invention is as follows: a astragalus-ginseng palpitation-relieving granule for treating ventricular premature beat is prepared by the following method: Adding 6-10 times of water into radix astragali preparata, radix codonopsis pilosulae, radix ophiopogonis, radix asparagi, radix salviae miltiorrhizae, rhizoma ligustici wallichii, poria cocos, rhizoma pinellinae praeparata and rhizoma nardostachyos, soaking, decocting and extracting for 20-120 min, filtering, concentrating the filtrate under reduced pressure, taking a proper amount of dextrin, placing into a fluidized bed, spray-drying and granulating to obtain the Chinese medicinal preparation. As a preferred scheme, the astragalus-ginseng palpitation relieving granule for treating ventricular premature beat is prepared by the following method: 15g of roasted astragalus, 10g of codonopsis pilosula, 10g of dwarf lilyturf tuber, 10g of asparagus root, 15g of red sage root, 15g of szechuan lovage rhizome, 15g of poria cocos, 10g of prepared pinellia tuber and 10g of nardostachyos root, adding water twice, adding 10 times of water for the first time, soaking 60 min, decocting 30min, filtering, adding 8 time