CN113456584A - Preparation method of six-ingredient saffron oral liquid - Google Patents

Preparation method of six-ingredient saffron oral liquid Download PDF

Info

Publication number
CN113456584A
CN113456584A CN202110784860.9A CN202110784860A CN113456584A CN 113456584 A CN113456584 A CN 113456584A CN 202110784860 A CN202110784860 A CN 202110784860A CN 113456584 A CN113456584 A CN 113456584A
Authority
CN
China
Prior art keywords
water
preparation
filtering
ethanol
oral liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202110784860.9A
Other languages
Chinese (zh)
Inventor
倪爽爽
聂亚委
陈翠萍
王奇
李亚生
唐尧
江雪琴
姚雪
马梓萱
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Sinopharm Xinjiang Pharmaceutical Co Ltd
Original Assignee
Sinopharm Xinjiang Pharmaceutical Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Sinopharm Xinjiang Pharmaceutical Co Ltd filed Critical Sinopharm Xinjiang Pharmaceutical Co Ltd
Priority to CN202110784860.9A priority Critical patent/CN113456584A/en
Publication of CN113456584A publication Critical patent/CN113456584A/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/08Solutions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/48Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
    • A61K36/484Glycyrrhiza (licorice)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/53Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/64Orobanchaceae (Broom-rape family)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/65Paeoniaceae (Peony family), e.g. Chinese peony
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/71Ranunculaceae (Buttercup family), e.g. larkspur, hepatica, hydrastis, columbine or goldenseal
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/185Magnoliopsida (dicotyledons)
    • A61K36/81Solanaceae (Potato family), e.g. tobacco, nightshade, tomato, belladonna, capsicum or jimsonweed
    • A61K36/815Lycium (desert-thorn)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18Magnoliophyta (angiosperms)
    • A61K36/88Liliopsida (monocotyledons)
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/02Inorganic compounds
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/26Carbohydrates, e.g. sugar alcohols, amino sugars, nucleic acids, mono-, di- or oligo-saccharides; Derivatives thereof, e.g. polysorbates, sorbitan fatty acid esters or glycyrrhizin
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0012Galenical forms characterised by the site of application
    • A61K9/0053Mouth and digestive tract, i.e. intraoral and peroral administration
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P1/00Drugs for disorders of the alimentary tract or the digestive system
    • A61P1/14Prodigestives, e.g. acids, enzymes, appetite stimulants, antidyspeptics, tonics, antiflatulents
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61PSPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
    • A61P9/00Drugs for disorders of the cardiovascular system
    • A61P9/10Drugs for disorders of the cardiovascular system for treating ischaemic or atherosclerotic diseases, e.g. antianginal drugs, coronary vasodilators, drugs for myocardial infarction, retinopathy, cerebrovascula insufficiency, renal arteriosclerosis
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/331Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/33Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
    • A61K2236/333Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/30Extraction of the material
    • A61K2236/39Complex extraction schemes, e.g. fractionation or repeated extraction steps
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/51Concentration or drying of the extract, e.g. Lyophilisation, freeze-drying or spray-drying
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2236/00Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
    • A61K2236/50Methods involving additional extraction steps
    • A61K2236/53Liquid-solid separation, e.g. centrifugation, sedimentation or crystallization

Abstract

The Xinjiang Uygur autonomous region health office of 1994 approves the Xinjiang Chinese medicine general factory (now national medicine group Xinjiang pharmacy Co., Ltd.) to produce the Liuwei Xihonghua oral liquid for the first time, and the preparation method of the Liuwei Xihonghua oral liquid is continuously researched and developed for many years and is improved compared with the method disclosed in the early stage. The invention discloses a preparation method of an improved Liuwei Xihong Hua oral liquid, which has the following beneficial effects compared with the prior art: the clarifying agent is complex to prepare, takes longer time and has lower impurity removal efficiency, the invention reduces the step of using ZTC1+1 natural clarifying agent in the treatment of the medlar decoction dregs, and shortens the preparation time and the cost; the terminal sterilization links of a pH regulator and boiling heat preservation are added, so that the stable quality of the product is ensured, and the pH value and the microbial limit meet the standard; a centrifugal process is added in the liquid preparation link to improve the impurity removal efficiency and ensure that the final clarity of the oral liquid meets the requirement; and partial production process parameters are refined, so that the preparation method is more feasible.

Description

Preparation method of six-ingredient saffron oral liquid
Technical Field
The invention relates to a traditional Chinese medicine composition with the effects of nourishing heart, warming stomach, tonifying kidney and promoting blood circulation, in particular to a preparation method of a six-ingredient saffron oral liquid.
Background
Six-ingredient saffron oral liquid is firstly produced by a Xinjiang Uygur autonomous region health hall approving Xinjiang Chinese medicine general factory (Xinjiang pharmaceutical Co., Ltd., the present national medicine group), the prescription of the six-ingredient saffron oral liquid is derived from the classic proved prescription of Uygur national medicine, the Xinjiang Uygur medicinal materials of Xighua and Ziziphora are taken as the main materials, and the six-ingredient saffron oral liquid is prepared by matching with the nourishing medicinal materials of medlar, cistanche, tree peony bark and liquorice. The main functional indications of the medicine are that the medicine can strengthen spirit and vitality, nourish heart, warm stomach, tonify kidney and strengthen body. Can be used for treating thoracic obstruction, chest distress, angina pectoris, coronary heart disease, etc., and is used for tonifying kidney and promoting blood circulation in traditional Chinese medicine. Can be used for treating thoracic obstruction caused by kidney deficiency and blood stasis, with symptoms of chest pain, chest distress, palpitation, and soreness of waist and knees.
The prior art, the specification of the patent number 200510002886.4 of Liuwei xi hong Hua dripping pill and the preparation method thereof, discloses one preparation method of Liuwei xi hong Hua oral liquid, which comprises the following steps:
the preparation method comprises the following steps: soaking stigma croci Sativi in 60% ethanol for 6 times (70-80 deg.C) for 30 min, mixing soaking solutions, standing for 24 hr, filtering, and recovering ethanol from filtrate; according to the items of the fluid extract and the extract (appendix IO of the first part of the 2000 th edition of Chinese pharmacopoeia, 70% ethanol is used for soaking for 24 hours, then permeation and percolation are carried out at the speed of 3-5 ml per minute, the permeation liquid is collected, the ethanol is recovered for standby use, the wolfberry dregs are decocted for 2 hours by adding water, the decoction is decompressed and concentrated to clear paste with the relative density of 1.08-1.12 (60 ℃), ZTC1+1 natural clarifying agent is added, standing is carried out for 24 hours, filtration is carried out, the filtrate is standby use, the moutan bark and the Ziziphora bungeana are extracted by using a steam distillation method to obtain volatile oil, the distillate is collected for standby use, the distilled water solution is collected in another container, the dregs, the gruffs, the cistanche deserticola and the liquorice are decocted for two times by adding water, the first time is carried out for 2.5 hours, the second time is carried out, the decoction and the distilled water solution are combined, the filtration is carried out, the filtrate is decompressed and concentrated to clear paste with the relative density of 1.08-1.10 (60 ℃), the filtrate is cooled, the ethanol is added to ensure that the water content reaches 60%, standing for 24 hr, filtering, recovering ethanol from filtrate, mixing with the above solution, adding sucrose and sodium benzoate, adding water to desired volume, stirring, filtering, and making into 1000 ml.
The preparation method of the six-ingredient saffron oral liquid is continuously researched and developed for many years, and is improved compared with the early-published preparation method. The preparation method disclosed in the prior art is only one of the preparation methods, and has a plurality of defects, mainly including complicated preparation process of the clarifying agent, long time consumption, low production efficiency during commercial batch production, unsatisfactory effect when the clarifying agent is used in a concentrated solution, no legal medicinal standard of the clarifying agent, and possibility of bringing other components into the clarifying agent through an extract in the use process. In addition, the prior art has no terminal sterilization link and can not effectively control the microbial pollution level.
Disclosure of Invention
First, technical problem to be solved
The invention aims to provide a preparation method of a six-ingredient saffron oral liquid, which is used for improving the defects that a clarifying agent is required to be used in the prior art, a terminal sterilization link is omitted, the medicine production period is longer, the risk of microorganism control is caused, and the like.
Second, technical scheme
A preparation method of a six-ingredient saffron oral liquid is characterized by comprising the following steps: the raw materials include stigma croci Sativi, fructus Lycii, Cistanchis herba, cortex moutan, Ziziphora Bungeana Juz, Glycyrrhrizae radix, sucrose, sodium benzoate, pH regulator, ethanol, and water.
The method comprises the following steps: putting crocus sativus into a reflux tank, adding 60% ethanol with the mass of about 40 times, hot dipping (70-80 ℃) for 30 minutes, operating according to the method for 6 times, combining maceration extract, standing for 24 hours, and filtering by using a 80-mesh screen;
vacuum sucking the filtrate into a vacuum concentrator, starting steam for heating, controlling the pressure at 0.01-0.20 Mpa and the temperature at 60-80 ℃, and concentrating to obtain a clear paste I with the relative density of 1.0-1.1 (60 ℃).
Step two: putting the wolfberry fruits into a percolation tank, adding 70% ethanol with the mass being 8-10 times that of the wolfberry fruits, soaking for 24 hours, percolating at the speed of 3-5 mL per minute, collecting percolate, and filtering by using an 80-mesh sieve.
Vacuum sucking percolate into vacuum concentrator, heating with steam under 0.01-0.20 Mpa, concentrating to obtain fluid extract II with relative density of 1.08-1.12 (60 deg.C), and refrigerating.
Step three: adding 8-10 times of water by mass of the wolfberry fruit into wolfberry fruit dregs, decocting for 2 hours, filtering by using an 80-mesh filter screen, sucking the filtrate into a vacuum concentrator in vacuum, starting steam for heating, controlling the temperature to be 60-80 ℃, the pressure to be 0.01-0.20 Mpa and the vacuum degree to be-0.05 Mpa-0.12 Mpa, concentrating until the relative density is 1.08-1.12 (60 ℃), standing for 24 hours, filtering by using an 80-mesh filter screen, extracting supernatant to obtain clear paste III, and refrigerating for storage.
Step four: and putting the tree peony bark and the Ziziphora Bungeana Juz into a multifunctional extraction tank, adding 8-10 times of water by mass, extracting for 2-3 hours by a steam distillation method to obtain volatile oil IV and a distilled water solution, and refrigerating for storage, wherein the tree peony bark and the Ziziphora Bungeana Juz herb residues are reserved.
Step five: decocting cortex moutan, Ziziphora Bungeana Juz herb residues, herba cistanches and liquorice in water twice, adding water 8-10 times of the mass of the four medicinal materials for the first time, decocting for 2.5 hours, adding water 6-8 times of the mass of the four medicinal materials for the second time, and decocting for 1.5 hours to obtain decoction.
Combining the decoction and the distilled aqueous solution, sucking the mixture into a single-effect external circulation evaporator in vacuum, starting steam to heat the mixture, controlling the temperature to be 60-80 ℃, the pressure to be 0.01-0.20 Mpa and the vacuum degree to be-0.05-0.12 Mpa, concentrating the mixture to obtain clear paste with the relative density of 1.08-1.10 (60 ℃), and cooling the clear paste to room temperature.
Adding ethanol with concentration higher than 85% into the cooled fluid extract, stirring completely to make the ethanol content of the liquid medicine be 60%, standing for more than 24 hr, filtering with 80 mesh filter screen, vacuum sucking the filtrate into a concentrator, starting steam pressure control at 0.01-0.20 Mpa, concentrating to obtain fluid extract V with relative density of 1.08-1.10 (60 deg.C), and refrigerating for storage.
Step six: and sequentially adding the fluid extract I, the fluid extract II, the fluid extract III, the volatile oil IV, the fluid extract V, the cane sugar, the sodium benzoate and the water into a mechanical stirring fluid preparation tank, uniformly mixing, and adjusting the pH value to 4.5-5.5 by using a sodium hydroxide or hydrochloric acid solution. And centrifuging the obtained liquid medicine to obtain a mixed solution VI.
Step seven: and (3) pumping the mixed solution VI into another mechanical stirring liquid preparation tank, starting steam to boil, preserving the heat for 10 minutes to 2 hours, and then cooling to room temperature to obtain the six-ingredient saffron oral liquid.
The applicant researches the preparation process of the six-ingredient saffron oral liquid, and the preparation process specifically comprises the following steps:
one (10L per batch) was examined for process time and rationality.
Figure 293179DEST_PATH_IMAGE001
Through research, the step of using the ZTC1+1 natural clarifying agent in the step five is reduced, the preparation time is obviously shortened by about 25 hours, the preparation cost is reduced, and other impurities caused by using the clarifying agent are avoided. In terms of the whole process flow, although the steps of centrifugation, pH value adjustment, boiling and heat preservation and the like are added, the time consumption is still shortened by about 21 hours compared with the prior art.
(II) comparison of the prior art with the microbial Limit test of the present invention
1. Control group: the six-ingredient saffron oral liquid prepared by the prior art is used.
Figure 741478DEST_PATH_IMAGE002
2. Experimental groups: the six-ingredient saffron oral liquid prepared by the method is provided.
Figure 52373DEST_PATH_IMAGE003
3. And (6) summarizing.
The experimental control group and the experimental group respectively carry out microbial detection in 0 th month, 1 st month and 3 rd month after production, and all meet the standard regulation: at month 0, no microorganism was detected in both experimental and control groups; in 1 st and 3 rd months, the experimental group has fewer microorganisms and more stable quality.
(III) the quality inspection of the three batches of the six-ingredient saffron oral liquid.
1. And (5) checking the relative density.
Figure 999249DEST_PATH_IMAGE005
2. And (5) checking the pH value.
Figure 344779DEST_PATH_IMAGE006
3. Examination (HPLC) of the paeonol content.
The instrument model is as follows: shimadzu LC-20AT
Detection wavelength: 274nm
Mobile phase: methanol: water =1:1
Figure 432821DEST_PATH_IMAGE008
A Chinese medicinal oral liquid, LIUWEIXIHONGHUA oral liquid, contains paeonol (C) and cortex moutan in each 1ml9H10O3) Calculated, should not be less than 0.40 mg; through investigation, the three batches of six-ingredient saffron oral liquid using the method disclosed by the invention meet the internal control standard.
4. Examination of echinacoside content (HPLC)
The instrument model is as follows: shimadzu LC-20AT
Detection wavelength: 334nm
Mobile phase: methanol: 0.1% formic acid solution =28:72
Figure 231013DEST_PATH_IMAGE009
Every 1ml of six-ingredient saffron oral liquid contains cistanche and echinacoside (C)33H46O20) Calculated, should not be less than 0.20 mg; through investigation, the three batches of six-ingredient saffron oral liquid using the method disclosed by the invention meet the internal control standard.
5. Summary of the invention
The inventor uses the three batches of six-ingredient saffron oral liquid produced by the method, after the impurity removal process of a clarifying agent is deleted in the extraction process of the medlar, the clarity of the extracting solution after standing is better, a high-temperature sterilization process is added after liquid preparation, a centrifugation process is added in the liquid preparation process, after 3 batches of products are trial-produced, the results show that the three batches of six-ingredient saffron oral liquid produced by the method meet the quality standard through the indexes of product quality inspection, such as relative density, pH value, paeonol content, echinacoside content and the like.
Third, beneficial effect
Compared with the prior art, the invention has the beneficial effects that: and partial production process parameters are refined, so that the preparation method is more feasible.
The step of using ZTC1+1 natural clarifier in the treatment of fructus Lycii residue in step three is reduced, and the preparation time and cost are shortened.
The pH regulator and the terminal sterilization link of boiling and heat preservation are added, the microbial control level of the product is ensured, and the pH value and the microbial limit meet the standard.
And (3) adding a centrifugal process in the step six liquid preparation link to improve impurity removal efficiency and ensure that the final clarity of the oral liquid meets the requirement.
Drawings
FIG. 1 is a process flow diagram of step one of claim 1 of the present invention.
Fig. 2 is a process flow diagram of step two of claim 1 of the present invention.
Fig. 3 is a process flow diagram of step three of claim 1 of the present invention.
Fig. 4 is a process flow diagram of steps four and five of claim 1 of the present invention.
Fig. 5 is a process flow diagram of steps six and seven in claim 1 of the present invention.
Detailed Description
The following examples are given solely for the purpose of illustration and are not intended to limit the scope of the invention. The processes in the following examples are conventional unless otherwise specified.
A preparation method of each batch of the six-ingredient saffron oral liquid comprises the following steps:
raw materials:
20g of saffron, 1000g of medlar, 1000g of desertliving cistanche, 500g of tree peony bark, 500g of Ziziphora Bungeana Juz, 250g of liquorice, 1000g of cane sugar, 20g of sodium benzoate, hydrochloric acid, sodium hydroxide, ethanol and water in proper amount respectively.
The method comprises the following steps: putting 20g of saffron into a reflux tank, adding 800g of 60% ethanol according to the mass of 40 times, hot-dipping for 30 minutes at 70-80 ℃, carrying out the operation according to the method for 6 times, combining the maceration extract, standing for 24 hours, and filtering by using a 80-mesh screen;
vacuum sucking filtrate into vacuum concentrator, heating with steam under 0.01-0.20 Mpa at 60-80 deg.C, and concentrating to obtain fluid extract I with relative density of 1.01 (60 deg.C) of total 420 g.
Step two: putting 1000g of medlar into a percolation tank, adding 10kg of 70% ethanol according to the mass of 10 times, soaking for 24 hours, percolating at the speed of 5mL per minute, collecting percolate, and filtering by a 80-mesh sieve;
vacuum sucking percolate into vacuum concentrator, heating with steam under 0.01-0.20 Mpa, concentrating to obtain fluid extract II with relative density of 1.08 (60 deg.C) 450g, and refrigerating for storage to obtain fructus Lycii residue.
Step three: adding 10kg of water into the wolfberry fruit residue which is 10 times of the mass of the raw wolfberry fruit medicinal materials, decocting for 2 hours, filtering by using an 80-mesh filter screen, sucking the filtrate into a vacuum concentrator in vacuum, starting steam to heat, controlling the temperature to be 60-80 ℃, controlling the pressure to be 0.01-0.20 Mpa, controlling the vacuum degree to be-0.05 Mpa-0.12 Mpa, concentrating to the relative density of 1.11 (60 ℃), standing for 24 hours, filtering by using an 80-mesh filter screen, extracting supernatant to obtain 1040g of clear paste, and refrigerating for storage.
Step four: putting 500g of tree peony bark and 500g of Ziziphora Bungeana Juz into a multifunctional extraction tank, adding 10kg of water according to the mass of 10 times, extracting for 2 hours by a steam distillation method to obtain about 1kg of volatile oil IV and a distilled water solution, refrigerating and storing, and keeping the tree peony bark and Ziziphora Bungeana Juz herb residues for later use.
Step five: decocting cortex moutan, Ziziphora Bungeana Juz dregs, herba cistanches 1000g and radix Glycyrrhizae 250g in water twice, adding 22.5kg of water for the first time, decocting for 2.5 hr, adding 13.5kg of water for the second time, and decocting for 1.5 hr to obtain decoction;
mixing the decoction and the distilled water solution, sucking the mixture into a single-effect external circulation evaporator in vacuum, starting steam to heat the mixture, controlling the temperature to be 60-80 ℃, the pressure to be 0.01-0.20 Mpa and the vacuum degree to be-0.05-0.12 Mpa, concentrating the mixture to obtain clear paste with the relative density of 1.10 (60 ℃), and cooling the clear paste to room temperature;
adding 85% ethanol into the cooled fluid extract, stirring thoroughly until the ethanol content of the liquid medicine is 60%, standing for 24 hr, filtering with 80 mesh filter screen, vacuum sucking the filtrate into a concentrator, controlling the steam pressure at 0.01-0.20 Mpa, concentrating to obtain fluid extract V with relative density of 1.09 (60 deg.C) of 1655g, and refrigerating for storage.
Step six: adding a small amount of water into the mechanical stirring liquid preparation tank, starting steam heating and starting stirring. Adding the fluid extract I, the fluid extract II, the fluid extract III, the volatile oil IV, the fluid extract V, 1000g of sucrose and 20g of sodium benzoate in sequence, adding water to adjust the volume to 10L, mixing and stirring uniformly, and adjusting the pH value to 4.5-5.5 by using sodium hydroxide and hydrochloric acid solution. And centrifuging the obtained liquid medicine to obtain a mixed solution VI.
Step seven: and (3) pumping the mixed solution VI into another mechanical stirring liquid preparation tank, starting steam to boil, preserving the heat for 30 minutes, and then cooling to room temperature to obtain the Liuwei saffron oral liquid.

Claims (9)

1. A preparation method of a six-ingredient saffron oral liquid is characterized by comprising the following steps:
the required raw materials comprise stigma croci Sativi, fructus Lycii, Cistanchis herba, cortex moutan, Ziziphora Bungeana Juz, Glycyrrhrizae radix, sucrose, sodium benzoate, pH regulator, ethanol, and water;
the method comprises the following steps: hot-dipping stigma croci with ethanol, mixing the maceration extract, standing, filtering, and concentrating to obtain fluid extract I;
step two: soaking fructus Lycii in ethanol, percolating, filtering, and concentrating to obtain fluid extract II, and collecting residue;
step three: decocting the wolfberry fruit dregs, filtering, concentrating under reduced pressure, standing and filtering to obtain clear paste III;
step four: distilling cortex moutan and Ziziphora Bungeana Juz to extract volatile oil IV, reserving distilled water solution, and reserving cortex moutan and Ziziphora Bungeana Juz dregs;
step five: decocting the cortex moutan and Ziziphora Bungeana Juz residue, Cistanchis herba and Glycyrrhrizae radix, mixing the obtained decoction with the distilled water solution, concentrating under reduced pressure, precipitating with ethanol, standing, filtering, and concentrating to obtain fluid extract V;
step six: adding the fluid extract I, the fluid extract II, the fluid extract III, the volatile oil IV and the fluid extract V in the previous step in sequence, mixing with sucrose, sodium benzoate and water, adding a pH regulator, and centrifuging to obtain a mixed solution VI;
step seven: and boiling the mixed solution VI, preserving the temperature, and cooling to room temperature to obtain the six-ingredient saffron oral liquid.
2. The method of claim 1, wherein the method comprises the following steps:
the first step is specifically that crocus sativus is put into a reflux tank, 60% ethanol with the mass of 40 times is added, hot dipping is carried out for 30 minutes (70-80 ℃), the operation is carried out according to the method for 6 times, maceration extract is combined, standing is carried out for 24 hours, and filtering is carried out through a 80-mesh screen;
vacuum sucking the filtrate into a vacuum concentrator, starting steam for heating, controlling the pressure at 0.01-0.20 Mpa and the temperature at 60-80 ℃, and concentrating to obtain a clear paste I with the relative density of 1.0-1.1 (60 ℃).
3. The method of claim 1, wherein the method comprises the following steps:
putting the wolfberry fruits into a percolation tank, adding 70% ethanol with the mass being 8-10 times that of the wolfberry fruits, soaking for 24 hours, percolating at the speed of 3-5 mL per minute, collecting percolate, and filtering by using an 80-mesh sieve;
vacuum sucking percolate into vacuum concentrator, heating with steam under 0.01-0.20 Mpa, concentrating to obtain fluid extract II with relative density of 1.08-1.12 (60 deg.C), and refrigerating.
4. The method of claim 1, wherein the method comprises the following steps:
adding 8-10 times of water by mass into the wolfberry fruit dregs, decocting for 2 hours, filtering by using an 80-mesh filter screen, sucking the filtrate into a vacuum concentrator in vacuum, starting steam for heating, controlling the temperature to be 60-80 ℃, controlling the pressure to be 0.01-0.20 Mpa, controlling the vacuum degree to be-0.05-0.12 Mpa, concentrating to the relative density of 1.08-1.12 (60 ℃), standing for 24 hours, filtering by using an 80-mesh filter screen, extracting supernatant to obtain clear paste III, and refrigerating for storage.
5. The method of claim 1, wherein the method comprises the following steps:
and the fourth step is specifically that the tree peony bark and the Ziziphora Bungeana Juz are put into a multifunctional extraction tank, 8-10 times of water is added, the water vapor distillation method is used for extracting for 2-3 hours to obtain volatile oil IV and a distilled water solution, the volatile oil IV and the distilled water solution are stored in a refrigeration mode, and the tree peony bark and the Ziziphora Bungeana Juz herb residues are reserved.
6. The method of claim 1, wherein the method comprises the following steps:
the fifth step is to take the tree peony bark, the Ziziphora Bungeana Juz herb residues, the cistanche and the liquorice to be decocted with water twice, the water which is 8-10 times of the mass of the four medicinal materials is added for the first time to be decocted for 2.5 hours, the water which is 6-8 times of the mass of the four medicinal materials is added for the second time to be decocted for 1.5 hours, and decoction liquid is obtained;
combining the decoction and the distilled aqueous solution, sucking the mixture into a single-effect external circulation evaporator in vacuum, starting steam to heat, controlling the temperature to be 60-80 ℃, the pressure to be 0.01-0.20 Mpa and the vacuum degree to be-0.05-0.12 Mpa, and cooling the mixture to room temperature when the mixture is concentrated to a clear paste with the relative density of 1.08-1.10 (60 ℃);
adding ethanol with concentration higher than 85% into the cooled fluid extract, stirring completely to make the ethanol content of the liquid medicine be 60%, standing for more than 24 hr, filtering with 80 mesh filter screen, vacuum sucking the filtrate into a concentrator, starting steam pressure control at 0.01-0.20 Mpa, concentrating to obtain fluid extract V with relative density of 1.08-1.10 (60 deg.C), and refrigerating for storage.
7. The method of claim 1, wherein the method comprises the following steps:
step six is specifically that water is added into the mechanical stirring liquid preparation tank, steam heating is started, and stirring is started; adding the clear paste I, the clear paste II, the clear paste III, the volatile oil IV, the clear paste V, sucrose, sodium benzoate and water in sequence, mixing and stirring uniformly, and adjusting the pH value to 4.5-5.5 by using sodium hydroxide or hydrochloric acid solution; and centrifuging the obtained liquid medicine to obtain a mixed solution VI.
8. The method of claim 1, wherein the method comprises the following steps: and the boiling method in the seventh step is steam boiling, and the heat preservation time is 10 minutes to 2 hours.
9. A preparation method of a six-ingredient saffron oral liquid is characterized by comprising the following steps: the raw materials include stigma croci Sativi, fructus Lycii, Cistanchis herba, cortex moutan, Ziziphora Bungeana Juz, Glycyrrhrizae radix, sucrose, sodium benzoate, pH regulator, ethanol, and water.
CN202110784860.9A 2021-07-12 2021-07-12 Preparation method of six-ingredient saffron oral liquid Withdrawn CN113456584A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202110784860.9A CN113456584A (en) 2021-07-12 2021-07-12 Preparation method of six-ingredient saffron oral liquid

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202110784860.9A CN113456584A (en) 2021-07-12 2021-07-12 Preparation method of six-ingredient saffron oral liquid

Publications (1)

Publication Number Publication Date
CN113456584A true CN113456584A (en) 2021-10-01

Family

ID=77879792

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202110784860.9A Withdrawn CN113456584A (en) 2021-07-12 2021-07-12 Preparation method of six-ingredient saffron oral liquid

Country Status (1)

Country Link
CN (1) CN113456584A (en)

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1679676A (en) * 2005-01-28 2005-10-12 北京正大绿洲医药科技有限公司 Six-component saf-flower drops and preparation thereof
CN101139402A (en) * 2007-10-18 2008-03-12 西北大学 Method for extracting polysaccharide from jujube
CN107142184A (en) * 2017-06-30 2017-09-08 宁夏塞上无极生物产业有限公司 LBP-X health preserving wine and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1679676A (en) * 2005-01-28 2005-10-12 北京正大绿洲医药科技有限公司 Six-component saf-flower drops and preparation thereof
CN101139402A (en) * 2007-10-18 2008-03-12 西北大学 Method for extracting polysaccharide from jujube
CN107142184A (en) * 2017-06-30 2017-09-08 宁夏塞上无极生物产业有限公司 LBP-X health preserving wine and preparation method thereof

Non-Patent Citations (5)

* Cited by examiner, † Cited by third party
Title
刘红宇等: "中药(复方)提取方法、技术研究进展", 《中医药导报》 *
刘锐萍 等: "三种澄清剂对枸杞酒澄清效果及其对枸杞多糖含量影响的研究", 《食品科学》 *
歆君等: "六味西红花口服液治疗肾阳虚证随机、双盲、阳性药平行对照、两中心临床研究", 《新疆中医药》 *
罗明生 等主编: "《药剂辅料大全》", 31 January 2006 *
龙晓燕 等: "枸杞子残渣中多糖的提取工艺研究", 《食品工业科技》 *

Similar Documents

Publication Publication Date Title
CN103146560B (en) Health-care vinegar and preparation method thereof
CN101948730B (en) Health-care wine and preparation method thereof
CN102258708B (en) Health-preserving wine and preparation method thereof
CN102311900B (en) Health care yellow wine rich in nutrients
CN102465073A (en) Fig health care wine and preparation method thereof
CN102742906A (en) Momordica grosvenori drink with low glycemic index and anti-fatigue action
CN105558203A (en) Healthcare tea capable of reducing blood pressure and preparation process thereof
CN103202470A (en) Health food for reducing blood sugar in auxiliary manner and preparation method of health food
CN109123301A (en) A kind of asparagus fermentation solid beverage and its preparation method and application
CN102994309B (en) Ginkgo-sorghum liquor and ginkgo-sorghum health-care liquor
CN103549437B (en) Health-protection food capable of reducing blood pressure and blood fat and preparation method of food
CN103232916B (en) Fragrant solomonseal rhizome-containing tea rice wine and preparation method thereof
CN101392218A (en) Nutrient health wine brewed by natural honey and Chinese herbal medicine and preparation method thereof
CN106867824A (en) Male silkworm essence wine and preparation method thereof
CN104958564B (en) Dendrobium candidum oral solution and preparation method thereof
CN103961613A (en) Novel preparation method of high-quality loquat syrup
CN105746772A (en) Preparation method of sweet potato leaf health tea with effect of lowering blood glucose
CN106344824B (en) Saussurea involucrata culture oral liquid and preparation method thereof
CN105039079A (en) Life-prolonging health care liquor
CN113456584A (en) Preparation method of six-ingredient saffron oral liquid
CN109679794A (en) A kind of preparation method of fructus arctii lemon beer
CN109251821A (en) A kind of functional yellow rice wine and its manufacture craft improving immunity of organisms
CN106967549A (en) Grape health medicinal liquor and preparation method thereof
CN1672582A (en) Health beverage for Yin-deficiency people and its prepn process
CN107372947B (en) Tea bag type blood sugar reducing tea and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication

Application publication date: 20211001

WW01 Invention patent application withdrawn after publication