CN114689714A

CN114689714A - Meridian warming soup reference extract and preparation method thereof

Info

Publication number: CN114689714A
Application number: CN202011604918.9A
Authority: CN
Inventors: 周巧敏; 胡昌江; 张强; 陈玉梅; 钟磊; 刘珂; 姚丽琴; 周维; 叶志萍
Original assignee: Sichuan New Green Pharmaceutical Technology Development Co ltd
Current assignee: Sichuan New Green Pharmaceutical Technology Development Co ltd
Priority date: 2020-12-30
Filing date: 2020-12-30
Publication date: 2022-07-01
Anticipated expiration: 2040-12-30
Also published as: CN114689714B

Abstract

The invention discloses a channel warming decoction control extract and a preparation method thereof, relates to the technical field of Chinese patent medicine production, and obtains channel warming decoction control extract freeze-dried powder with stable quality by controlling the process parameters of pretreatment, decoction, concentration, freeze drying and the like of medicinal materials of a channel warming decoction formula.

Description

Meridian warming soup reference extract and preparation method thereof

Technical Field

The invention relates to the technical field of Chinese patent medicine production, in particular to a channel warming decoction reference extract and a preparation method thereof.

Background

The channel warming decoction is originally found in the ' women's complete prescription ' in Song Dynasty and old self-explanatory, the whole formula consists of nine medicines, and the decoction is a traditional Chinese medicine decoction which is commonly used in clinic, and is mainly used for treating gynecological diseases, such as irregular menstruation, dysmenorrheal, infertility and the like. The decoction method is that the Chinese angelica, the Szechuan lovage rhizome, the paeony root, the cassia bark, the tree peony bark and the zedoary are respectively half two, and the ginseng, the liquoric root and the twotooth achyranthes root are respectively one or two. Right side

Chew for five money each time. Decocting with water for one and a half, removing residues, and taking warm.

According to examination certificates such as dosage and preparation method of poria and cassia twig decoction in the requirements of declaration data of material basis of traditional Chinese medicine compound preparations of ancient classic famous prescriptions (examination of comments and drafts) and key information table of ancient classic famous prescriptions (7 formulas), the modern decoction method of the warming channel decoction can be known as follows according to the results of the examination certificates: 20.6g of angelica, ligusticum wallichii, white paeony root, cinnamon, moutan bark and curcuma zedoary respectively, and 41.3g of ginseng, achyranthes and liquorice (liquorice) respectively. Pulverizing into coarse powder, taking 20g per dose, adding 450 ml water, decocting to 360 ml, removing residues, and taking warm.

The classical famous prescription is a compound composed of a plurality of medicines, and due to the complexity of the ingredients and the diversity of influencing factors, how to objectively evaluate the quality control in the classical famous prescription is always a difficult problem on the modernization road of the traditional Chinese medicine. And the chemical reference substances are difficult to develop, the separation difficulty is high, the monomers are unstable, the corresponding production cost and technical requirements are high, the detection cost is expensive, the supply quantity of the chemical reference substances which are difficult to obtain is more limited, the chemical reference substances have a plurality of limitations in practical application and are difficult to popularize, and the traditional Chinese food and drug verification research institute does not have the reference extracts of classical famous prescriptions.

The traditional Chinese medicine contrast extract is a new concept proposed in the industry in recent years, the traditional Chinese medicine contrast extract is a non-monomer component contrast, the contrast extract is easy to prepare in a single contrast product, low in price, good in stability and relatively simple in preparation operation, and the use of the monomer contrast product can be greatly reduced as a standard substance, so that the rare resources of the traditional Chinese medicine are saved, and the inspection cost is reduced; by using the qualitative action of the control extract, different primordial factors of the traditional Chinese medicinal materials of the classical name prescription can be identified, and the authenticity of the medicinal materials can be evaluated. Thereby objectively evaluating the quality control of the medicine in the classical famous prescription.

The traditional Chinese medicine contrast extract becomes a trend of the development of the traditional Chinese medicine contrast in our country, and the research on the contrast extract becomes necessary and urgent. At present, the channel warming decoction control extract needs to be researched urgently, and key parameters such as water adding amount, decoction time, water adding times, a freeze-drying process and the like influence the preparation process of the channel warming decoction control extract.

Disclosure of Invention

The invention aims to provide a comparison extract of the channel warming decoction and a preparation process study, wherein the comparison extract is used for making a comparison reference for the study of the characteristic spectrum of the channel warming decoction in the later period, and is used as a qualitative function to effectively control the quality of traditional Chinese medicinal materials and provide technical support for the quality control of a channel warming decoction compound preparation.

The invention is realized by the following technical scheme:

a preparation method of a channel warming soup contrast extract comprises the following steps:

A. pretreatment of medicinal materials: taking medicinal angelica, ligusticum wallichii, white peony root, tree peony bark, zedoary, ginseng, achyranthes root, liquorice and cinnamon, removing silt, impurities and non-medicinal parts, moistening, cutting, drying, and then processing the angelica, the zedoary and the liquorice to obtain fried angelica, ligusticum wallichii, the white peony root, the tree peony bark, vinegar curcuma zedoary, ginseng, the achyranthes root, the fried liquorice and cinnamon decoction pieces;

B. decocting: weighing each decoction piece in the step A according to the formula of the channel warming decoction, adding 6-8 times of water, soaking for 20-40min, decocting for 20-30min, decocting for 2-3 times, mixing the liquid medicines, filtering, and collecting the filtrate;

C. concentration: concentrating the filtrate obtained in step B at 50 + -2 deg.C under vacuum degree of 0.080Mpa to relative density of 1.02-1.06 to obtain concentrated solution;

D. and (3) freeze drying: and D, pre-freezing the concentrated solution in the step C under normal pressure, carrying out sublimation drying under the pressure of 0.0pa, carrying out resolution drying, collecting powder at the temperature of 10-26 ℃ and the relative humidity of 40-60%, weighing, subpackaging in brown penicillin bottles, and sealing to obtain the channel warming decoction control extract freeze-dried powder.

Further, in the step a, the pretreatment method of the medicinal materials comprises the following steps:

removing silt and non-medicinal parts of medicinal angelica, ligusticum wallichii, white paeony root, tree peony bark, rhizoma zedoariae, ginseng, achyranthes and liquorice, taking medicinal cinnamon, and removing impurities and crude bark; spraying clear water on radix Angelicae sinensis, rhizoma Ligustici Chuanxiong, radix Paeoniae alba, Ginseng radix, Achyranthis radix, and Glycyrrhrizae radix for 2-3 times, moistening for 1-2 hr, cleaning cortex moutan rapidly, soaking Curcumae rhizoma slightly, and cleaning with clear water; cutting radix Angelicae sinensis, radix Paeoniae alba, cortex moutan, and Ginseng radix into 1-2mm slices, cutting rhizoma Ligustici Chuanxiong, Curcumae rhizoma, and Glycyrrhrizae radix into 2-4mm thick slices, mashing cortex Cinnamomi, and cutting Achyranthis radix into 5-10mm short segments; drying radix Angelicae sinensis and cortex moutan at 50 + -5 deg.C, drying rhizoma Ligustici Chuanxiong, radix Paeoniae alba, Ginseng radix, Achyranthis radix and Glycyrrhrizae radix at 75 + -5 deg.C to meet water content requirement, and processing radix Angelicae sinensis, Curcumae rhizoma and Glycyrrhrizae radix into parched radix Angelicae sinensis, vinegar Curcumae rhizoma and parched Glycyrrhrizae radix for use.

Further, in the step D, the conditions of sublimation drying are as follows:

maintaining the temperature at-40 ℃ for 1 h;

maintaining the temperature at-30 ℃ for 1 h;

maintaining the temperature at-20 ℃ for 2 h;

maintaining the temperature at-10 ℃ for 3 h;

the temperature was maintained at 0 ℃ for 3 h.

In step D, the conditions for the desorption drying are as follows:

the temperature is 10 ℃, the temperature is maintained for 3 hours, and the pressure is 0.0 pa;

the temperature is 20 ℃, the pressure is maintained for 2h, and the pressure is 0.0 pa;

the temperature is 30 ℃, the temperature is maintained for 2 hours, and the pressure is 0.0 pa;

the temperature was 45 ℃ and the pressure was maintained for 22h at 0.0 pa.

Further, in the step A, the step B,

the stir-frying method of the fried angelica comprises the following steps: parching cleaned radix Angelicae sinensis slices with slow fire to yellow in a parching container, taking out, and spreading for cooling;

the preparation method of the vinegar curcuma zedoary comprises the following steps: adding vinegar into clean Curcumae rhizoma at a ratio of 20kg of rice vinegar per 100kg of Curcumae rhizoma, stirring, decocting until it is thoroughly transparent, taking out, cooling, cutting into 2-4mm thick pieces, and drying;

the processing method of the fried liquorice comprises the following steps: taking the clean liquorice tablets, putting the clean liquorice tablets into a frying container, frying the clean liquorice tablets to be yellow by slow fire, taking out the fried liquorice tablets, and spreading the fried liquorice tablets for cooling.

Further, in the step B, weighing each decoction piece in the step A according to the formula of the channel warming decoction, decocting for one time, adding 8 times of water, soaking for 30min, and decocting for 30 min; adding 6 times of water into the second decoction, decocting for 20min, mixing the decoctions, filtering, and collecting the filtrate.

Further, in the step B, the filtering condition is that a filter with 200-mesh filtration is adopted for filtering, and then the filtrate is collected.

Further, the formula of the channel warming soup comprises the following components in parts by weight: 20.6 parts of angelica, szechuan lovage rhizome, white paeony root, cinnamon, tree peony bark and zedoary each, and 41.3 parts of ginseng, twotooth achyranthes root and liquoric root each.

A warming channel soup control extract prepared according to the preparation method of the warming channel soup control extract is characterized in that the water content of freeze-dried powder of the warming channel soup control extract is 5.2% -6.8%, the extract is yellow to brown yellow powder, slight in smell, bitter in taste first and then sweet.

Compared with the prior art, the invention has the following advantages and beneficial effects:

(1) in the invention, on the basis of the classical famous prescription of the traditional Chinese medicine, namely the channel warming decoction, on the basis of the traditional decoction method, after the extraction of a solvent, the decoction times, the decoction time and the water addition amount are investigated, the corresponding channel warming decoction control extract is prepared, and the characteristic map research is carried out on the channel warming decoction control extract, so that the channel warming decoction can be used for qualitative identification of the corresponding decoction.

(2) In the invention, the preparation of the control extract has important significance: firstly, technical support is provided for quality control of a contrast extract and a compound preparation reported by China food and drug testing research institute, and the method has strong creativity; and secondly, the method responds to the call of the multi-index overall quality control of the traditional Chinese medicine, avoids the repeated occurrence of the procedures such as pretreatment, prescription, extraction, component identification and the like, makes the experimental operation more simple and convenient and reduces the consumption of resources. Can provide guarantee for the quality control of the traditional Chinese medicine classical famous prescription decoction and lay a certain foundation for the international popularization thereof.

(3) In the invention, the quality control is carried out by using the warm channel soup as the control extract and using the integral control substance as the control, so that the integral quality control in the real sense is realized, the detectable range and the detectable quantity are infinite, the detection cost is hardly increased, and the repeatability of the detection method is obviously improved.

(4) In the invention, the meridian warming decoction control extract represents the integral internal quality of the preparation, and can provide reference basis for the related preparation of the subsequent classical famous meridian warming decoction.

Drawings

FIG. 1 is a water absorption curve of the warming meridian soup in example 4.

FIG. 2 is a control profile of Wen Jing Tang in example 9.

FIG. 3 is the characteristic spectrum of 10 batches of the extract of the warming channel decoction in example 10.

Detailed Description

The present invention provides a meridian warming decoction control extract and a preparation method thereof, and the present invention is further described in detail below in order to make the objects, technical schemes and effects of the present invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.

The experimental instruments and materials involved in the examples are as follows:

an electronic balance: JY series one hundredth balance of Shanghai Fangrui instruments Co., Ltd;

a medicine decocting pot: 4 liters of a delicious family full-automatic split type ceramic medicine decocting pot;

screening: a nine-peak screen mesh is 200 meshes;

a vacuum freeze dryer: LGJ-100F, a Beijing Song Huaxing science and technology development Co., Ltd;

penicillin bottle capping machine: SZ 20A;

a plurality of 2000ml stainless steel measuring cups; penicillin bottles: 10ml, 30ml and more than 50 ml;

high performance liquid chromatograph: waters 2695-2996 high performance liquid chromatograph, Agilent 1260-type high performance liquid chromatograph and Shimadzu 20-AD high performance liquid chromatograph;

an ultrasonic cleaner: model KQ5200DB (600W, 40 KHz; ultrasonic instruments, Inc. of Kunshan);

an electronic balance: JY series hundredth balance, ME204E/02, MS205DU, Shanghai Fangrui instruments, Inc,

XP26 (mettler-toledo instruments ltd);

an ultra-pure water machine: cell type 1810A (Shanghai Mohler scientific instruments, Inc.);

a chromatographic column: agilent ZORBAX SB-C18250X 4.6mm, Kromasil C185 μm 4.6X 250mm,

Phenomenex Luna 5um C18(2)100A 4.6×250mm。

Reagent: acetonitrile is chromatographically pure, water is ultrapure water, and other reagents are analytically pure;

reagent testing: gallic acid, paeoniflorin, and glycyrrhizic acid reference substance;

radix Angelicae sinensis, rhizoma Ligustici Chuanxiong, radix Paeoniae alba, cortex Cinnamomi, cortex moutan, Curcumae rhizoma, Achyranthis radix, and Glycyrrhrizae radix (provided by Sichuan New Green pharmaceutical science and technology development Co., Ltd.);

wen Jing Tang control extract (prepared by Sichuan New Green pharmaceutical science and technology development Co., Ltd.: WJT200901, WJT200902, WJT200903, WJT200904, WJT200905, WJT200906, WJT200907, WJT200908, WJT200909, WJT 200910).

Example 1

The embodiment relates to a specific preparation method of a channel warming soup control extract, which comprises the following steps:

D. and (3) freeze drying: and D, pre-freezing the concentrated solution in the step C under normal pressure, then sublimating and drying under the pressure of 0.0pa, then performing resolution drying, collecting powder at the temperature of 10-26 ℃ and the relative humidity of 40-60%, weighing, subpackaging in brown penicillin bottles, and sealing to obtain the channel warming decoction control extract freeze-dried powder.

Example 2

In this embodiment, the further optimization is performed in embodiment 1, and in step a, after the medicinal herbs including angelica sinensis, ligusticum wallichii, radix paeoniae alba, cortex moutan, curcuma zedoary, ginseng, achyranthes bidentata, liquorice and cinnamon are taken, the specific pretreatment method is as follows:

chinese angelica: removing impurities, cleaning, moistening, cutting into 1-2mm slices, and drying at low temperature. Parching cleaned radix Angelicae sinensis with slow fire to yellow in a parching container, taking out, and spreading for cooling.

Ligusticum wallichii: removing impurities, separating, cleaning, moistening, cutting into 2-4mm thick pieces, and drying.

White peony root: cleaning, moistening, cutting into 1-2mm slices, and drying.

Moutan bark: quickly cleaning, moistening, cutting into 1-2mm slices, and drying in the sun.

Zedoary turmeric: removing impurities, soaking, cleaning, adding vinegar (20 kg of rice vinegar per 100kg of Curcumae rhizoma), stirring, decocting, taking out, cooling, cutting into 2-4mm thick pieces, and drying.

Ginseng: moistening, cutting into 1-2mm slices, and drying.

Achyranthes root: removing impurities, cleaning, moistening, removing residual rhizoma Phragmitis, cutting into 5-10mm short segments, and drying.

Licorice (licorice): removing impurities, cleaning, moistening, cutting into 2-4mm thick pieces, and drying. Taking the clean liquorice tablets, putting the clean liquorice tablets into a frying container, frying the clean liquorice tablets to be yellow by slow fire, taking out the fried liquorice tablets, and spreading the fried liquorice tablets for cooling.

Cinnamon: removing impurities and coarse skin. Pounding into pieces for use.

When the decoction pieces are moistened, the decoction pieces are generally moistened by a hand-held method until the inner core is moistened; checking the length of the cut decoction pieces, wherein the special-shaped pieces are not more than 10%. And then the qualified decoction pieces are sent into a decoction pot for the next decoction step.

Example 3

This example is a study of the properties of the warm meridian decoction control extract.

The warm channel soup contrast extract is processed to obtain a solid powder. The properties and water contents of 10 batches of the warming channel decoction control extract are shown in tables 1 and 2 respectively.

Table 1: 10 batches of channel warming decoction contrast extract character

Table 2: moisture examination of 10 batches of warming decoction control extract

According to the detection results of multiple batches of warming channel soup control extracts, the warming channel soup control extract is yellow to brown yellow powder, has light smell, tastes bitter first and then is sweet; the water content of the warm channel soup control extract is within the range of 5.2% -6.8%, and the average value is 5.9%.

Example 4

In the technical field of traditional Chinese medicine pharmacy, different decoction pieces have different water absorption rates, so the water absorption rate of the channel warming decoction needs to be considered, and further the water adding amount is used as a reference. This example mainly examined the change in water absorption when the warming channel soup control extract was prepared.

Weighing 100g of decoction pieces in the prescription amount (calculated according to the proportion of 20.6 parts of each of Chinese angelica, ligusticum wallichii, white paeony root, cinnamon, tree peony bark and curcuma zedoary and 41.3 parts of each of ginseng, achyranthes bidentata and liquorice), adding 8 times of water in two parts respectively, soaking for 10min, 20min, 30min, 50min, 1h, 1.5h, 2h, 4h, 6h, 8h, 16h and 24h respectively, measuring and calculating the water absorption rate, wherein the result is shown in a table 3, and the water absorption curve is shown in a table 1.

Table 3: water absorption data of channel warming decoction

As can be seen from Table 3 and FIG. 1, the decoction pieces of Warm meridian decoction rapidly absorbed water in the first 1.5h, gradually decreased after 2h, and absorbed water nearly saturated in 12h, with an average water absorption of 268.8%. The water absorption was about 2.5 times.

Referring to the opinion of ' water adding amount ' part of ' technical requirements for quality control and standard formulation of traditional Chinese medicine formula granules (solicited opinion draft): because the quality and the water absorption rate of the traditional Chinese medicine decoction pieces are greatly different, the water adding amount is determined according to different decoction pieces. The water addition amount is preferably 2-5 cm higher than the medicine surface, the water can be added into flower and grass decoction pieces or decoction pieces which are decocted for a longer time, and the water addition amount in the first time in the step of preparing the warming channel decoction is 8 times of that in the second time in the previous experiment.

Example 5

On the basis of example 4, by considering the water addition amount and the extraction times of the meridian warming soup, the water addition amount of the first decoction can be adjusted to 8 times, and the water addition amount of the second decoction can be adjusted to 6 times, and the extraction can be carried out for 2 times by referring to the water absorption rate; or adjusting the water adding times of the first decoction to 7 times, setting the water adding times of the second decoction to 6 times, extracting for 2 times, finding that the difference of the final results is not large when the water adding amount of each time is controlled to be 6-8 times, but when the water adding amount is adjusted to 9 times, the time length of the subsequent concentration process is obviously prolonged, so setting that the water adding times of the first decoction to 8 times, the water adding times of the second decoction to 6 times, extracting for 2 times and having higher efficiency.

Example 6

This example is a study of the soaking time in the preparation process of the decoction for warming meridians control extract.

Taking 100g of decoction pieces prepared according to the prescription of the decoction piece for warming channels, adding 8 times of water into the decoction pieces, and observing the soaking condition of the decoction pieces every 10min until the decoction pieces are soaked until the inner cores are wet.

The results show that: taking decoction pieces of the warm channel soup formula, adding 8 times of water, and observing the soaking condition of the decoction pieces every 10min until the decoction pieces are soaked until the inner core is wet. Soaking for 10min until most decoction pieces are not soaked thoroughly; soaking for 20min until the inner core of the decoction pieces is wet, and the inner core of the decoction pieces is not wet; soaking for 30min until the inner cores of all decoction pieces are wet, and determining the soaking time to be 30 min.

Example 7

This example is a study of the freezing process in the preparation process of the decoction for warming meridians as a control extract.

According to the requirements of the declaration data of the material standard of the ancient classical famous prescription traditional Chinese medicine compound preparation (the request for comments), the freeze-drying method is preferably adopted in the drying process of the extract, so that the quality stability and the storage easiness of the extract can be ensured. The examination of the freeze-drying process parameters lists the control conditions of two freeze-drying processes, which are shown in tables 4-1 and 4-2.

Table 4-1: freeze-drying process of meridian warming decoction contrast extract

Tables 4-2: freeze-drying process (II) of meridian warming soup contrast extract

And two kinds of freeze-dried powder are obtained by matching the freeze-drying process with the control parameters in the table. Detection shows that the freeze-dried powder obtained by the process parameters shown in the table 4-1 is looser and drier and is more beneficial to storage. So the process conditions corresponding to the control parameters of table 4-1 are finally selected.

And then, rapidly collecting the freeze-dried powder obtained by the process at the temperature of 10-26 ℃ and the relative humidity of 40-60%, weighing, subpackaging in brown penicillin bottles, sealing and labeling.

Example 8

In this example, the decoction of the warm channel decoction control extract was verified, and according to the investigation of the preparation process of the warm channel decoction control extract in the foregoing implementation, the finally determined preferred process is as follows: decocting decoction pieces of the warm channel decoction formula twice with water, adding 8 times of water for one decoction, soaking for 30min, boiling, keeping boiling for 30min, filtering with 200 mesh screen, and immediately cooling to room temperature; adding 6 times of water into the second decoction, boiling, keeping slightly boiling, decocting for 20 minutes, filtering with a 200-mesh screen, and immediately cooling to room temperature; mixing the decoctions, freeze drying, and packaging.

By adopting the preparation process, 10 batches of decoction of the warm channel soup reference extract are decocted, and the results are shown in table 5.

Table 5: summary of 10 batches of decoction for warming meridians control extract data

As shown in Table 5, the powder yield of the control extract of 10 batches of the warming channel decoction was 27.37% on the average. SD is 1.17. The range of 70% -130% of the average value is 19.16% -35.58%. The average value plus or minus 3 times SD range is 23.86% -30.88%. The data are within normal range and can be used as reference for production process.

Example 9

The embodiment is a characteristic map construction method for applying the freeze-dried powder of the warming channel decoction control extract obtained in the technical scheme to the warming channel decoction control extract, and then applying the obtained map to qualitative detection of the warming channel decoction compound preparation.

a. Preparation of control solutions: adding 70% methanol into gallic acid, penoniflorin and glycyrrhizic acid reference substances respectively to obtain mixed solution containing 40 μ g of each 1 ml.

b. Preparation of a test solution: weighing about 0.5g of the powder, precisely weighing, placing in a conical flask with a plug, precisely adding 25ml of 70% methanol, sealing the plug, weighing, ultrasonically treating (power 300W, frequency 25kHz) for 30 minutes, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking up, filtering, and taking the subsequent filtrate.

c. And (3) detection: and c, injecting the reference substance solution and the test solution obtained in the steps a and b into a high performance liquid chromatograph for detection, selecting common peaks from the characteristic spectrum of the test solution by taking the characteristic spectrum of the reference substance solution as a reference spectrum, and constructing the characteristic spectrum of the channel warming soup reference extract.

The detection conditions of the high performance liquid chromatography meet the following conditions:

a chromatographic column: octadecylsilane chemically bonded silica is used as a filler (the column length is 250mm, the inner diameter is 4.6mm, and the particle size is 5 μm);

column temperature: 30 ℃;

flow rate: 1.0 ml/min;

sample introduction amount: 10 mu l of the mixture;

detection wavelength: 254 nm;

the mobile phase A is acetonitrile, the mobile phase B is 0.1 percent phosphoric acid water solution, and gradient elution is carried out.

The gradient elution process is as follows:

0-3 min, 2 percent of mobile phase A, 98 percent of mobile phase B,

3-35 min, 2-28% of mobile phase A, 98-72% of mobile phase B,

35-45 min, 28-40% of mobile phase A, 72-60% of mobile phase B,

45-60 min, the mobile phase A is 40-60%, the mobile phase B is 60-40%,

60-75 min, 60-95% of mobile phase A, 40-5% of mobile phase B,

75-80 min, 95% of mobile phase A and 5% of mobile phase B.

d. And c, taking the characteristic map of the reference substance solution in the step c as a reference map, selecting common peaks from the characteristic maps of the test substance solution, and constructing the characteristic map of the channel warming soup reference extract.

The test sample characteristic map should present 16 characteristic peaks, wherein peak 1, peak 6, and peak 13 should respectively correspond to the retention time of reference substance peak of gallic acid, paeoniflorin, and glycyrrhizic acid reference substance. The peak corresponding to the paeoniflorin reference peak was taken as the S1 peak, and the relative retention times of peaks 2-10 and S1 were calculated, which should be within. + -. 8% of the specified values. The values were defined as 0.577 (peak 2), 0.602 (peak 3), 0.890 (peak 4), 0.959 (peak 5), 1.233 (peak 7), 1.254 (peak 8), 1.278 (peak 9), and 1.419 (peak 10). The peak corresponding to the glycyrrhizic acid reference substance peak was taken as the S2 peak, and the relative retention times of peaks 11 to 16 and the S2 peak were calculated to be within ± 8% of the specified values. The predetermined values were 0.862 (peak 11), 0.961 (peak 12), 1.148 (peak 14), 1.178 (peak 15), and 1.229 (peak 16). As shown in fig. 2. Wherein, peak 1: gallic acid, peak 2: l-tryptophan, peak 3: protocatechuic acid, peak 4: chlorogenic acid, peak 5: albiflorin, peak 6 (S1): paeoniflorin, peak 8: liquiritin; peak 13 (S2): glycyrrhizic acid.

Example 10

Verification of characteristic spectrum of warm channel decoction control extract

The characteristic spectrum of 10 batches of the wenjing soup control extracts (S1-S10: WJT200901, WJT200902, WJT200903, WJT200904, WJT200905, WJT200906, WJT200907, WJT200908, WJT200909 and WJT200910) is verified according to the characteristic spectrum detection method of the wenjing soup control extract, and the result is shown in figure 3.

By adopting the characteristic map, the quality control of the warm channel soup reference extract can be integrally carried out so as to ensure the quality uniformity and stability; the result shows that the quality of the 10 batches of the channel warming soup reference extract is uniform and stable.

The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and all simple modifications and equivalent variations of the above embodiments according to the technical spirit of the present invention are included in the scope of the present invention.

Claims

1. A preparation method of a channel warming decoction control extract is characterized by comprising the following steps:

2. The method for preparing a warming channel soup control extract as claimed in claim 1, wherein in the step A, the pretreatment method of medicinal materials comprises:

3. The method for preparing a warming channel soup control extract as claimed in claim 2, wherein in the step D, the conditions of sublimation drying are as follows:

maintaining the temperature at-40 ℃ for 1 h;

maintaining the temperature at-30 ℃ for 1 h;

maintaining the temperature at-20 ℃ for 2 h;

maintaining the temperature at-10 ℃ for 3 h;

the temperature was maintained at 0 ℃ for 3 h.

4. The method for preparing a warming channel soup control extract as claimed in claim 3, wherein in the step D, the analysis and drying conditions are as follows:

the temperature is 30 ℃, the pressure is maintained for 2 hours, and the pressure is 0.0 pa;

the temperature was 45 ℃ and the pressure was maintained for 22h at 0.0 pa.

5. The method for preparing a warming channel soup control extract as claimed in claim 4, wherein in the step A,

6. The method for preparing a warming channel decoction control extract as claimed in claim 5, wherein in the step B, each decoction piece in the step A is weighed according to the formula of the warming channel decoction, decocted for one time, added with 8 times of water, soaked for 30min and decocted for 30 min; adding 6 times of water into the second decoction, decocting for 20min, mixing the decoctions, filtering, and collecting the filtrate.

7. The method for preparing a warming channel soup control extract as claimed in claim 6, wherein in the step B, the filtering condition is filtering with a 200 mesh filter, and then collecting the filtrate.

8. The preparation method of the warming channel soup control extract as claimed in any one of claims 1 to 7, wherein the formula of the warming channel soup is as follows, calculated by weight: chinese angelica root, Ligusticum wallichii, root of herbaceous peony, Cinnamomum cassia, bark of peony root, zedoary each 20.6 parts, ginseng, achyranthes and licorice root each 41.3 parts.

9. A meridian warming soup contrast extract is characterized in that: the method for preparing the warming channel soup reference extract according to claim 8, wherein the obtained warming channel soup reference extract freeze-dried powder has a water content of 5.2% -6.8%, and is yellow to brown yellow powder, light in smell, bitter in taste first and then sweet.