CN112263609A - Preparation method of classical famous prescription poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extracting solution - Google Patents

Preparation method of classical famous prescription poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extracting solution Download PDF

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CN112263609A
CN112263609A CN202011314965.XA CN202011314965A CN112263609A CN 112263609 A CN112263609 A CN 112263609A CN 202011314965 A CN202011314965 A CN 202011314965A CN 112263609 A CN112263609 A CN 112263609A
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廖正根
周玉春
蔣且英
康兴东
袁其里
李小锋
梁新丽
陈梁
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JIANGXI PUZHENG PHARMACEUTICAL CO Ltd
Jiangxi University of Traditional Chinese Medicine
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    • 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
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    • A61K36/07Basidiomycota, e.g. Cryptococcus
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    • A61K36/28Asteraceae or Compositae (Aster or Sunflower family), e.g. chamomile, feverfew, yarrow or echinacea
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    • A61K2236/30Extraction of the material
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    • 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 or decoction

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Abstract

The invention belongs to the field of pharmaceutical preparations, and relates to a preparation method of a classical famous formula poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extracting solution. The preparation method of the classical famous prescription Ling Gui Zhu gan Tang extract is that the classical famous prescription Ling Gui Zhu gan Tang is firstly extracted with volatile oil before being decocted according to the traditional process and then is prepared with extract according to the traditional process, or the classical famous prescription Ling Gui Zhu gan Tang is decocted according to the traditional process, and then the decoction is firstly extracted and separated with volatile oil and enters the concentration link and simultaneously collects the concentrated solution, or the preparation method of the extract is that the volatile oil and the concentrated solution are collected simultaneously during concentration. The preparation method of the classic famous prescription Ling Gui shu gan Tang extract can reduce the volatile oil loss caused by direct concentration and drying of the decoction in the traditional process of the classic famous prescription, and ensure that the substance standard of the decoction is consistent with that of the decoction in the traditional process. The preparation method is simple in preparation process, easy to industrialize and good in application prospect.

Description

Preparation method of classical famous prescription poria cocos, cassia twig, rhizoma atractylodis macrocephalae and licorice decoction extracting solution
Technical Field
The invention relates to the technical field of traditional Chinese medicine preparations, and relates to a preparation method of a classical famous formula poria cocos, cassia twig, rhizoma atractylodis and licorice decoction extracting solution.
Background
The classical famous prescription is still widely applied at present because of the exact curative effect. In order to support the development of classical famous prescriptions, the national drug administration (drug administration) issues a ' declaration data requirement (request for comments) of the material standard of traditional Chinese medicine compound preparations of ancient classical famous prescriptions in 2019, 3 months, and the core idea of the method is to ensure that the medicinal materials used in clinic are basically consistent with the medicinal materials of traditional decoctions, so how to realize ' basic consistency ' becomes the key and core of the research on the production process of classical famous prescriptions.
The traditional decoction has short storage time, so the clear decoction in the ancient Chinese medicinal compound preparation with famous prescriptions can be prepared into granules, the existing preparation method of the solid substance with the famous prescriptions is generally to prepare the decoction according to the traditional process of the famous prescriptions, the decoction is further prepared by spray drying or freeze drying the decoction, and the process links such as concentration drying and the like can not avoid the loss of volatile components, but the volatile components are the important components for the traditional Chinese medicinal preparation to exert the curative effect, so the consistency of the famous prescriptions solid preparation and the traditional decoction substance is difficult to ensure.
The invention relates to a preparation method of a classical famous prescription Lingguizhan decoction extract which simultaneously reserves volatile components and non-volatile components, namely a preparation method of extracting volatile oil firstly and storing the volatile oil and then preparing the extract according to the traditional process, or extracting the volatile oil firstly and separating the decoction, then entering a concentration link and simultaneously collecting the concentrated solution after the decoction is decocted according to the traditional process, or simultaneously collecting the volatile oil and the concentrated solution during concentration.
Disclosure of Invention
The invention aims to provide a preparation method of a classical famous formula poria cocos, cassia twig, rhizoma atractylodis and licorice decoction extracting solution. The preparation method can reduce the volatile oil loss caused by direct concentration and drying of the decoction in the traditional process of the classical name prescription, and ensure that the substance standard of the decoction of the preparation and the traditional process is consistent.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of a classic famous prescription Ling Gui Zhu gan Tang extract, which comprises the following steps:
(1) soaking Poria, ramulus Cinnamomi, Atractylodis rhizoma and Glycyrrhrizae radix in water, and decocting.
(2) Extracting volatile oil from the decoction by a volatile oil extractor, and filtering to obtain an extracting solution.
Furthermore, in the step (1), 55-56g of poria cocos, 41-42g of cassia twig, 41-42g of bighead atractylodes rhizome and 27-28g of liquorice are taken, and 1000-2000mL of water is added for soaking for 1-3h and decocting for 1-3 h.
Further, the time for extracting the volatile oil in the step (2) is 2-6 h.
Alternatively, the preparation method of the invention comprises the following steps:
(1) soaking ramulus Cinnamomi, Atractylodis rhizoma, Poria, and Glycyrrhrizae radix in water, decocting, and filtering to obtain filtrate.
(2) Extracting volatile oil from the filtrate with volatile oil extractor, and collecting volatile oil to obtain extractive solution and volatile oil.
Further, 41-42g of cassia twig, 41-42g of bighead atractylodes rhizome, 55-56g of poria cocos and 27-28g of liquorice are taken in the step (1), 1000 mL of 1500mL of water is added, the soaking time is 0.5-1.5h, and the decoction is carried out for 1-3 h.
Preferably, in the step (1), 41.4g of cassia twig, 41.4g of bighead atractylodes rhizome, 55.2g of poria cocos and 27.6g of liquorice are added with 1200mL of water, soaked for 1 hour and decocted for 2 hours.
Further, the time for extracting the volatile oil in the step (2) is 2-6 h.
Preferably, the time for extracting the volatile oil in the step (2) is 4 hours.
Alternatively, the preparation method of the invention comprises the following steps:
(1) soaking ramulus Cinnamomi and Atractylodis rhizoma in water, extracting volatile oil with volatile oil extractor, and collecting volatile oil to obtain volatile oil and decoction of ramulus Cinnamomi and Atractylodis rhizoma.
(2) Adding Poria and Glycyrrhrizae radix into the decoction of ramulus Cinnamomi and Atractylodis rhizoma, soaking in water, decocting, and filtering to obtain extractive solution.
Further, 41-42g of cassia twig and 41-42g of bighead atractylodes rhizome are taken in the step (1), 200mL of water is added, the soaking is carried out for 0.5-1.5h, and the volatile oil is extracted by a volatile oil extractor for 3-5 h.
Preferably, 41.4g of cassia twig and 41.4g of bighead atractylodes rhizome are taken in the step (1), 250mL of water is added for soaking for 1h, and a volatile oil extractor is used for extracting volatile oil for 4 h.
Further, 55-56g of poria cocos and 27-28g of liquorice are added in the step (2), water is supplemented until the volume is 1500mL of 1000-.
Preferably, 55.2g of poria cocos and 27.6g of liquorice are added in the step (1), water is added to 1200ml, and the mixture is soaked for 1 hour and decocted for 2 hours.
The technical effects obtained by the invention are as follows:
1. compared with the modern secondary reflux extraction process, the preparation method of the classical famous formula Ling Gui Zhu gan Tang extract can more effectively ensure that the substance standard of the decoction of the subsequent preparation is consistent with that of the decoction of the traditional process.
2. The preparation method is simple in preparation process, easy to industrialize and good in application prospect.
Drawings
FIG. 14 is a comparison of the characteristic spectra of the extracts prepared by the processes.
Absolute peak area comparison of 21 common peaks for the 24 processes: (
Figure BDA0002791072590000031
n=3)。
Detailed Description
The invention is further illustrated, but not limited, by the following specific examples.
Example 1
(1) Taking 41.4g of cassia twig, 41.4g of bighead atractylodes rhizome, 55.2g of poria cocos and 27.6g of liquorice, adding 1200mL of water, soaking for 1h, decocting for 2h, and filtering to obtain filtrate.
(2) Extracting volatile oil for 4 hr, and collecting volatile oil to obtain extractive solution and volatile oil.
Example 2
(1) Taking 41.4g of cassia twig and 41.4g of bighead atractylodes rhizome, adding 250mL of water, soaking for 1h, extracting volatile oil for 4h by a volatile oil extractor, and collecting the volatile oil to obtain volatile oil and a decoction of the cassia twig and the bighead atractylodes rhizome.
(2) Adding Poria and Glycyrrhrizae radix into the decoction of ramulus Cinnamomi and Atractylodis rhizoma, adding water to 1200ml, soaking for 1 hr, decocting for 2 hr, and filtering to obtain extractive solution.
Example 3
(1) Taking 55.2g of poria cocos, 41.4g of cassia twig, 41.4g of bighead atractylodes rhizome and 27.6g of liquorice, adding 1500mL of water, soaking for 2h, and decocting for 2 h.
(2) Extracting volatile oil from the decoction for 4 hr, and filtering to obtain extractive solution.
Screening of extraction Process
The following 4 extraction processes were designed:
process-traditional process for preparing extracting solution
Taking 55.2g of poria cocos, 41.4g of cassia twig, 41.4g of bighead atractylodes rhizome and 27.6g of liquorice, adding 1200mL of water for soaking for 1h, decocting for 2h, and filtering to obtain 600mL of extracting solution (named as S1).
Distilling the extractive solution to separate volatile oil, mixing volatile oil and the residual solution
Preparing 55.2g of poria cocos, 41.4g of cassia twig, 41.4g of bighead atractylodes rhizome and 27.6g of liquorice according to the first process, extracting volatile oil for 4 hours by using a volatile oil extractor, and combining the volatile oil and residual liquid obtained after the volatile oil is extracted (named as S2).
Preparation of extracting solution by using technological three modern secondary reflux extraction processes
Soaking Poria 55.2g, ramulus Cinnamomi 41.4g, Atractylodis rhizoma 41.4g, and Glycyrrhrizae radix 27.6g in water for 1 hr, reflux extracting for 2 times, each time extracting 1200ml water for 2 hr, and collecting volatile oil with volatile oil extractor. Mixing the two decoctions, concentrating with rotary evaporator, mixing the decoctions and volatile oil, and adjusting with water to 600mL (named S3).
Extracting volatile oil, decocting, mixing extractive solutions and volatile oil
Soaking ramulus Cinnamomi 41.4g, Atractylodis rhizoma 41.4g and 250ml water for 1 hr, and reflux-extracting volatile oil to obtain ramulus Cinnamomi Atractylodis rhizoma decoction and volatile oil. And adding 55.2g of poria cocos and 27.6g of liquorice into the decoction of the cassia twig and the bighead atractylodes rhizome, adding water to 1200ml, soaking for 1h, preparing an extracting solution according to the first process, and combining the volatile oil (named as S4).
4 comparing the characteristic spectrums of the extracting solution of the preparation process
Each process was carried out in parallel with 3 parts of extract. The fingerprint obtained by each extraction process in parallel for three times is used to generate a control map, and the characteristic map of the extract obtained by the 4 preparation processes is shown in figure 1. The similarity evaluation of the characteristic spectrum of the poria, cassia twig and rhizoma glycyrrhizae decoction of the S2, S3 and S43 processes and the characteristic spectrum of S1 is carried out by taking the process-one extracting solution S1 as a reference spectrum, applying a Chinese pharmacopoeia committee '2012 version of a traditional Chinese medicine chromatography fingerprint similarity evaluation system' and adopting a median method with the time window width of 0.1. The similarities of S2, S3, S4 and S1 are 0.997, 0.91 and 0.978, respectively (see table 1). The absolute peak areas of the peaks of the 4 processes are shown in fig. 2, and the analysis of the one-way variance of GraphPad Prism6 software shows: (ii) a decrease in peak area of peak No. 4 of S2 as compared to the absolute peak area of S1; the areas of the peaks 1, 4-8, 10, 12-15, 17 and 21 of S3 increased, and the areas of the peaks 4 and 18 of S4 decreased.
TABLE 14 comparison of characteristic spectra of extractive solutions of technical Linggui-Zhu-gan decoction
Figure BDA0002791072590000041
*: p <0.05 compared to S1
Comparison of index component content and extract yield of each formula of 4 process extract solutions
The contents of each prescription and the amount of extract of 4 technical extracts of Linggui shu gan Tang are shown in Table 2. the t test result shows that compared with S1, the contents and the paste yield of 4 components in S2 and S4 are not statistically different; except cinnamaldehyde, the content and the paste output of the other 3 components of S3 are obviously higher than S1.
Table 24 recipe of process extracts with the contents of the index components and the amount of the extracts: (
Figure BDA0002791072590000051
n=3)
Figure BDA0002791072590000052
*: p <0.05 compared to S1
Comparison of the ratio of process three to process one
Table 3 shows that the amount of cream discharged from process three is significantly higher than that of process one, and that there is a swelling phenomenon in process three, and in order to show whether the proportions of swelling of the respective components are consistent, the relative peak areas of the remaining peaks were calculated by using stable cinnamaldehyde with large peak areas of S1 and S3 as reference peaks, respectively, and the results are shown in table 3. the t test shows that the relative peak areas of the peaks 6-8, 10, 14, 17 and 21 of the S3 are obviously higher than those of the peaks S1, while the relative peak areas of the other peaks are unchanged, and shows that the swelling ratios of different components are inconsistent.
Relative peak area and significant difference of 321 common peaks in table: (
Figure BDA0002791072590000053
n=3)
Figure BDA0002791072590000054
Figure BDA0002791072590000061
*: p <0.05 compared to S1
Experiments prove that the preparation method of the extracting solution, which is prepared by firstly extracting the volatile oil and preserving the volatile oil in another container and then preparing the extracting solution according to the traditional process, or decocting the volatile oil according to the traditional process, and then extracting and separating the volatile oil from the decoction, enters a concentration link and simultaneously collects the concentrated solution, or simultaneously collects the volatile oil and the concentrated solution during concentration, can ensure that the substance standard of the classical famous formula Lingguizhu Ganshen decoction extracting solution is consistent with the substance standard of the traditional decoction. Therefore, the optimal preparation method of the extracting solution comprises the following steps: soaking ramulus Cinnamomi, Atractylodis rhizoma, Poria and Glycyrrhrizae radix in water, decocting, filtering, extracting volatile oil from the filtrate with volatile oil extractor, and collecting volatile oil to obtain extractive solution and volatile oil. Or soaking ramulus Cinnamomi and Atractylodis rhizoma in water, extracting volatile oil with volatile oil extractor, and collecting volatile oil to obtain volatile oil and decoction of ramulus Cinnamomi and Atractylodis rhizoma. The cassia twig and the largehead atractylodes rhizome are added with the prescription medicinal materials of tuckahoe and liquorice, and water is added for soaking, decocting and filtering. Finally obtaining the extracting solution and the volatile oil.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.

Claims (10)

1. A preparation method of a classic and famous formula Ling Gui Zhu gan Tang extract is characterized by comprising the following steps: the method comprises the following steps:
(1) soaking Poria, ramulus Cinnamomi, Atractylodis rhizoma and Glycyrrhrizae radix in water, and decocting.
(2) Extracting volatile oil from the decoction by a volatile oil extractor, and filtering to obtain an extracting solution.
2. The method for preparing the classic and famous extracting solution of linggui zhu gan tang as claimed in claim 1, wherein: in the step (1), 55-56g of poria cocos, 41-42g of cassia twig, 41-42g of bighead atractylodes rhizome and 27-28g of liquorice are taken, and are soaked in 2000mL of water for 1-3h and decocted for 1-3 h.
3. The method for preparing the classic and famous extracting solution of linggui zhu gan tang as claimed in claim 1, wherein: the time for extracting the volatile oil in the step (2) is 2-6 h.
4. A preparation method of a classic and famous formula Ling Gui Zhu gan Tang extract is characterized by comprising the following steps: the method comprises the following steps:
(1) soaking ramulus Cinnamomi, Atractylodis rhizoma, Poria, and Glycyrrhrizae radix in water, decocting, and filtering to obtain filtrate.
(2) Extracting volatile oil from the filtrate with volatile oil extractor, and collecting volatile oil to obtain extractive solution and volatile oil.
5. The method for preparing the classic and famous extracting solution of linggui zhu gan tang as claimed in claim 4, wherein: in the step (1), 41-42g of cassia twig, 41-42g of bighead atractylodes rhizome, 55-56g of tuckahoe and 27-28g of liquorice are taken, and 1000 mL of 1500mL of water is added.
6. The method for preparing the classic and famous extracting solution of linggui zhu gan tang as claimed in claim 4, wherein: in the step (1), the soaking time is 0.5-1.5h, and the decoction time is 1-3 h.
7. The method for preparing the classic and famous extracting solution of linggui zhu gan tang as claimed in claim 4, wherein: the time for extracting the volatile oil in the step (2) is 2-6 h.
8. A preparation method of a classic and famous formula Ling Gui Zhu gan Tang extract is characterized by comprising the following steps: the method comprises the following steps:
(1) soaking ramulus Cinnamomi and Atractylodis rhizoma in water, extracting volatile oil with volatile oil extractor, and collecting volatile oil to obtain volatile oil and decoction of ramulus Cinnamomi and Atractylodis rhizoma.
(2) Adding Poria and Glycyrrhrizae radix into the decoction of ramulus Cinnamomi and Atractylodis rhizoma, soaking in water, decocting, and filtering to obtain extractive solution.
9. The method for preparing the classic and famous extracting solution of linggui zhu gan tang as claimed in claim 8, wherein: in the step (1), 41-42g of cassia twig and 41-42g of bighead atractylodes rhizome are taken, 200mL of water is added, the mixture is soaked for 0.5-1.5h, and the volatile oil is extracted for 3-5h by a volatile oil extractor.
10. The method for preparing the classic and famous extracting solution of linggui zhu gan tang as claimed in claim 8, wherein: in the step (2), 55-56g of tuckahoe and 27-28g of liquorice are taken, water is added to 1000 and 1500mL, the tuckahoe and the liquorice are soaked for 0.5-1.5h and decocted for 1-3 h.
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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113390985A (en) * 2021-05-31 2021-09-14 盛实百草药业有限公司 Ephedra decoction substance standard, preparation method and quality detection method thereof
CN114561248A (en) * 2022-03-02 2022-05-31 华润三九(雅安)药业有限公司 Preparation method and device of volatile oil, inclusion compound and preparation method of pharmaceutical composition
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CN114924008A (en) * 2022-05-31 2022-08-19 江西普正制药股份有限公司 Decision method for extracting technological parameters of classical famous prescription Ling Gui shu gan Tang
WO2024141120A1 (en) * 2022-12-29 2024-07-04 江中药业股份有限公司 Poria, cinnamomi ramulus, atractylodis macrocephalae rhizoma and glycyrrhizae radix et rhizoma decoction extract and preparation method therefor
CN115957254A (en) * 2023-01-17 2023-04-14 嘉实(湖南)医药科技有限公司 Preparation method of poria cocos, cassia twig, rhizoma atractylodis and rhizoma glycyrrhizae decoction granules

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