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CN-122005475-A - Preparation method of apricot Dan Ganwan and fingerprint spectrum method thereof

CN122005475ACN 122005475 ACN122005475 ACN 122005475ACN-122005475-A

Abstract

The application relates to the technical field of traditional Chinese medicine pharmacy, in particular to a preparation method of apricot Dan Ganwan and a fingerprint method thereof. The preparation method comprises the steps of carrying out decoction and extraction on bitter almonds for at least two times, combining the obtained extracting solution to be used as a liquid phase component for preparing pills, drying and crushing bitter almonds residues at low temperature to obtain bitter almonds residue powder, mixing the bitter almonds residue powder with the Chinese gall extract to obtain bitter almonds functional powder, weighing ephedra, liquorice and gypsum according to the formula amount, crushing the ephedra, liquorice and gypsum, mixing the crushed bitter almonds with the bitter almonds functional powder to obtain composite powder for preparing pills, separating the bitter almonds extracting solution into a first liquid phase for nucleation and a second liquid phase for growing pills to form primary pill cores, enabling the primary pill cores to grow gradually to form pill bodies, carrying out surface layer shaping on the pill bodies after the pill bodies reach a preset particle size, and drying the pill bodies at 60 ℃ for 3 hours to obtain finished products of the bitter almonds Dan Ganwan. The application realizes the efficient, stable and high-quality preparation of the apricot Dan Ganwan.

Inventors

  • Du Xicui
  • WANG XIAO
  • YAO WEIYU
  • LI ZETING
  • YANG LIJIE
  • WU SHAN
  • YAO LI
  • LIU WANG
  • LI YUNBO
  • SHI WANYU
  • ZHAO XINGHUA
  • HE XIN
  • XU DAN
  • LIU GEGE
  • ZHANG CHEN
  • GENG LU

Assignees

  • 河北锦坤动物药业有限公司

Dates

Publication Date
20260512
Application Date
20260407

Claims (10)

  1. 1. A method for preparing a apricot Dan Ganwan comprising: S101, decocting and extracting the bitter apricot kernel at least twice, mixing the obtained extracting solutions to be used as a liquid phase component for preparing pills, drying and crushing the extracted bitter apricot kernel dregs at low temperature to obtain bitter apricot kernel dregs powder, and mixing the bitter apricot kernel dregs powder with the Chinese gall extract to obtain bitter apricot kernel functional powder; S102, weighing ephedra, liquorice and gypsum according to the formula amount, crushing, and mixing with the bitter almond functional powder to obtain composite powder for pill preparation; S103, dividing the bitter almond extracting solution into a first liquid phase for nucleation and a second liquid phase for pill growth, firstly wetting and nucleating the composite powder with the first liquid to form primary pill cores, and then alternately adding the second liquid phase and the composite powder to enable the primary pill cores to grow gradually to form pill bodies; s104, after the pellet body reaches the preset particle size, carrying out surface layer shaping on the pellet body, and drying for 3 hours at 60 ℃ to obtain a finished product of the apricot Dan Ganwan.
  2. 2. A finger print method of apricot Dan Ganwan for apricot Dan Ganwan according to claim 1, comprising: s201, taking a sample of the apricot Dan Ganwan, and extracting by adopting an aqueous methanol solution to obtain a sample solution; S202, respectively taking ephedrine hydrochloride, pseudoephedrine hydrochloride, amygdalin, glycyrrhizin and ammonium glycyrrhizate reference substances to prepare a mixed reference substance solution; S203, respectively detecting the sample solution and the mixed reference substance solution by adopting a high performance liquid chromatography, wherein polar diethyl ether connected phenyl bonding silica gel is used as a chromatographic filler, acetonitrile-methanol mixed solution is used as a mobile phase A, aqueous solution containing phosphoric acid and triethylamine is used as a mobile phase B, gradient elution is carried out, the flow rate is 1.0mL/min, and the sectional detection is carried out at 210nm and 250nm wavelengths; s204, determining characteristic peaks of ephedrine hydrochloride, pseudoephedrine hydrochloride, amygdalin, glycyrrhizin and ammonium glycyrrhizate according to the mixed reference substance solution, and establishing a high-efficiency liquid-phase fingerprint of the apricot Dan Ganwan based on the relative retention time and the relative peak area of each characteristic peak; And S205, evaluating the quality consistency of the sample of the apricot Dan Ganwan according to the fingerprint.
  3. 3. The method of claim 1, wherein the apricot Dan Ganwan is prepared from the following raw materials, by weight, 20-45 parts of ephedra herb, 20-45 parts of bitter apricot seed, 100-225 parts of gypsum, and 20-45 parts of liquorice.
  4. 4. The method according to claim 1, wherein the amount of water used for the first decoction extraction in step S101 is 3-10 times the amount of semen Armeniacae amarum fed, and the extraction time is 0.5-2.5 hours.
  5. 5. The method according to claim 1, wherein the amount of water used for the second decoction in step S101 is 2-8 times the amount of the bitter almond dregs added, and the extraction time is 0.5-2.5 hours.
  6. 6. The method according to claim 1, wherein the residue in step S101 is dried at low temperature, pulverized into 80-100 mesh fine powder, and mixed uniformly with the extract of gallnut at a weight ratio of 100:0.2-0.5.
  7. 7. The method according to claim 1, wherein the ephedra herb, licorice and gypsum are pulverized into 80-100 mesh fine powder in step S102 and then mixed.
  8. 8. The method of claim 2, wherein the gradient elution procedure comprises: 0-5min, mobile phase A of 5% and mobile phase B of 95%; 5-32min, 5-23% of mobile phase A and 95-77% of mobile phase B; 32-48min, 23% -29% of mobile phase A and 77% -71% of mobile phase B; 48-56min, 29% -40% of mobile phase A and 71% -60% of mobile phase B; 56-64min, 40% -80% of mobile phase A and 60% -20% of mobile phase B; 64-72min, mobile phase A80-5%, mobile phase B20-95%; 72-80min, mobile phase A of 5% and mobile phase B of 95%; The mobile phase A is a mixed solution with the volume ratio of acetonitrile to methanol being 40:60, and the mobile phase B is an aqueous solution containing 0.1% of phosphoric acid and 0.1% of triethylamine.
  9. 9. The method of claim 2, wherein the control solution contains 80 μg of ephedrine hydrochloride, 40 μg of pseudoephedrine hydrochloride, 200 μg of amygdalin, 80 μg of glycyrrhizin, and 80 μg of ammonium glycyrrhizinate per 1 mL.
  10. 10. The method according to claim 2, wherein the method for preparing the sample solution comprises: Taking 2g of a sample of the apricot Dan Ganwan, precisely weighing, placing in a 25mL volumetric flask, adding a proper amount of 50% methanol, performing ultrasonic treatment for 30min, cooling, supplementing the standard with 50% methanol, shaking uniformly, and filtering to obtain a sample solution; In step S203, a detection wavelength of 210nm is used within 0-55min, and a detection wavelength of 250nm is used within 55-72 min.

Description

Preparation method of apricot Dan Ganwan and fingerprint spectrum method thereof Technical Field The application relates to the technical field of traditional Chinese medicine pharmacy, in particular to a preparation method of apricot Dan Ganwan and a fingerprint method thereof. Background The Ma xing shi gan is derived from Ma xing shi gan decoction of Zhang Zhong Jing Shang Han Lun, and has the effects of relieving cough, eliminating phlegm, relieving asthma, resisting inflammation, relieving fever, and the like. Is often applied to the treatment of diseases such as tracheitis, acute bronchitis, upper respiratory tract infection, bronchial asthma and the like. Along with clinical needs, the ephedra, apricot kernel, gypsum and licorice are gradually expanded from single decoction to multiple dosage forms, and are prepared into pills according to the defects of each dosage form in the taking process, the storage condition and the production. Compared with the Ma Xing Shi Gan oral liquid, the Ma Xing Dan Ganwan does not need to waste dregs, reduces the cost of recycling the dregs while keeping the original characteristics to the greatest extent, and compared with the Ma Xing ShiGan powder, the Ma Xing Dan Ganwan is convenient for animals to swallow and has higher utilization rate, and gypsum is easy to sink at the bottom of a trough when the Ma Xing ShiGan powder is mixed and used, so that the animals cannot conveniently eat the feed. Therefore, the research of the apricot Dan Ganwan is of great significance. The common process of water pill preparation has the disadvantages of difficult molding, more pills broken, low efficiency, more destruction of active ingredients and nonuniform quality. Therefore, the novel pill preparation method provided by the invention has the advantages of round appearance, high pill forming rate, complete retention of active ingredients and high content. Disclosure of Invention The application provides a preparation method of apricot Dan Ganwan and a fingerprint method thereof, which aim to solve the problems. In a first aspect, the present application provides a preparation method of apricot Dan Ganwan, the preparation method comprising: S101, decocting and extracting the bitter apricot kernel at least twice, mixing the obtained extracting solutions to be used as a liquid phase component for preparing pills, drying and crushing the extracted bitter apricot kernel dregs at low temperature to obtain bitter apricot kernel dregs powder, and mixing the bitter apricot kernel dregs powder with the Chinese gall extract to obtain bitter apricot kernel functional powder; S102, weighing ephedra, liquorice and gypsum according to the formula amount, crushing, and mixing with the bitter almond functional powder to obtain composite powder for pill preparation; S103, dividing the bitter almond extracting solution into a first liquid phase for nucleation and a second liquid phase for pill growth, firstly wetting and nucleating the composite powder with the first liquid to form primary pill cores, and then alternately adding the second liquid phase and the composite powder to enable the primary pill cores to grow gradually to form pill bodies; s104, after the pellet body reaches the preset particle size, carrying out surface layer shaping on the pellet body, and drying for 3 hours at 60 ℃ to obtain a finished product of the apricot Dan Ganwan. According to the technical scheme, the total dissolution rate of heat-sensitive components such as amygdalin is improved (about 32% compared with single decoction), tannin-mediated convergence and bacteriostasis are provided for drug residue powder, the extraction liquid is divided into nucleation liquid and long pill liquid, and an alternating mode of wetting, powder adding, rewetting and powder adding is adopted, so that the liquid forms controllable capillary permeation and interfacial tension balance on the surface of powder, adhesion or non-nucleation phenomenon caused by local overwetting is obviously inhibited, the problems of difficult pill forming, more pills breaking, low efficiency and nonuniform quality in the traditional water pill making process are solved, the moisture migration rate and the thermal stress distribution are cooperatively controlled by low-temperature drying and 60 ℃ accurate drying, the drying efficiency is ensured, the degradation of ephedrine and amygdalin is reduced (HPLC measurement shows that the ephedrine retention rate is about 27% compared with 80 ℃ drying promotion, and the amygdalin retention rate is about 41%), and finally the high quality apricot batch variation of the appearance circle degree is more than or equal to 92%, the pill forming rate is 95%, and the inter-grain diameter coefficient is Dan Ganwan.3% is obtained. Optionally, the apricot Dan Ganwan is prepared from the following raw materials, by weight, 20-45 parts of ephedra herb, 20-45 parts of bitter apricot seed, 100-225 parts of gypsum and 20-45 part