CN114689714B - Channel warming soup control extract and preparation method thereof - Google Patents
Channel warming soup control extract and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a reference extract of Wenzhen decoction and a preparation method thereof, which relate to the technical field of Chinese patent medicine production.
Description
Technical Field
The invention relates to the technical field of Chinese patent medicine production, in particular to a channel warming soup control extract and a preparation method thereof.
Background
The decoction for warming meridians is found in Song DaichenThe medicine is a clinically common traditional Chinese medicine decoction, which is mainly used for treating gynecological diseases, and is mostly seen in irregular menstruation, dysmenorrhea, infertility and other diseases. The decoction method is that Chinese angelica, szechuan lovage rhizome, chinese herbaceous peony, cassia bark, tree peony bark, zedoary and ginseng, liquorice and twofold achyranthes root are respectively used. Right side
The mouth is used for taking five pieces per time. Decocting one and half of the water to eight minutes, removing dregs and taking warm.
According to examination papers such as the requirements of reporting materials (solicited opinion manuscripts) and the dosage and preparation method of Ling Gui Zhu Gan Tang in the key information Table (7 prescriptions) of the ancient classical prescription, the modern decoction method of the Wenzhen Tang is known from the results of examination papers: 20.6g of angelica, ligusticum wallichii, root of herbaceous peony, cinnamon bark, zedoary, and 41.3g of ginseng, achyranthes and licorice root. Pulverizing into coarse powder, adding 450 ml of water, decocting to 360 ml, and removing residues.
The classical prescription is a compound prescription composed of a plurality of medicines, and how to objectively evaluate the quality control in the classical prescription is always a difficult problem on the modern road of traditional Chinese medicines due to the complexity of the components and the diversity of influencing factors. And the chemical reference substance is difficult to develop, the separation difficulty is high, the monomer is unstable, the corresponding production cost and technical requirements are high, the detection cost is high, the supply quantity of the chemical reference substance which is not easy to obtain is limited, a plurality of limitations are provided in the practical application, the popularization is difficult, and the current Chinese food and drug verification institute does not have a control extract with a classical name.
The traditional Chinese medicine control extract is a new concept proposed in the industry in recent years, is a non-monomer component control, is easy to prepare in a single control, has low price and good stability, is relatively simple to prepare and operate, and can greatly reduce the use of a monomer control as a standard substance, thereby saving rare resources of traditional Chinese medicines and reducing the inspection cost; by using the qualitative effect of the control extract, different origins of the traditional Chinese medicinal materials in the classical prescription can be identified, and the authenticity of the medicinal materials can be evaluated. Thereby objectively evaluating the quality control of the traditional Chinese medicine in the classical prescription.
The traditional Chinese medicine reference extract has become a trend of the development of the traditional Chinese medicine reference in our country, and the research on the reference extract has become a necessity and urgent. At present, research on the temperature-menstruation-decoction control extract is urgently needed, and key parameters such as water addition amount, decoction time, water addition multiple, freeze-drying process and the like influence the preparation process of the temperature-menstruation-decoction control extract.
Disclosure of Invention
The invention is based on the problems, and aims to provide a control extract of the Wenying decoction and a preparation process research, wherein the control extract is used for making a control reference for the research of the characteristic spectrum of the Wenying decoction in the later period, and is used as a qualitative effect to effectively control the quality of Chinese medicinal materials and provide technical support for the quality control of the Wenying decoction compound preparation.
The invention is realized by the following technical scheme:
a preparation method of a reference extract of a Wenjing decoction comprises the following steps:
A. pretreatment of medicinal materials: taking Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, zedoary, ginseng, twotooth achyranthes root, liquoric root and cassia bark, removing sediment and impurities from non-medicinal parts, moistening, cutting, drying, and then stir-baking the Chinese angelica, the zedoary and the liquoric root to obtain stir-baked Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, vinegar zedoary, ginseng, twotooth achyranthes root, stir-baked liquoric root and cassia bark decoction pieces;
B. decocting: weighing each decoction piece in the step A according to the formula of the decoction for warming channels, adding 6-8 times of water, soaking for 20-40min, decocting for 20-30min, decocting for 2-3 times, mixing the medicinal liquids, filtering, and collecting filtrate;
C. concentrating: concentrating the filtrate in the step B to a relative density of 1.02-1.06 at 50+ -2deg.C and under vacuum degree of 0.080Mpa to obtain concentrated solution;
D. and (3) freeze drying: c, pre-freezing the concentrated solution in the step C, sublimating and drying under the condition of the pressure of 0.0pa, resolving and drying, collecting powder at the temperature of 10-26 ℃ and the relative humidity of 40-60%, weighing, split charging into brown penicillin bottles, and sealing to obtain the freeze-dried powder of the extract of the Wenzhen soup.
Further, in the step a, the pretreatment method of the medicinal materials comprises the following steps:
taking Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, zedoary, ginseng, twotooth achyranthes root and liquoric root, removing sediment and non-medicinal parts, taking Chinese cinnamon, and removing impurities and crude skin; spraying clear water for 2-3 times, moistening for 1-2 hours, rapidly cleaning cortex moutan, slightly soaking Curcumae rhizoma, 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 sections; drying radix Angelicae sinensis and cortex moutan at 50+ -5deg.C, drying rhizoma Ligustici Chuanxiong, radix Paeoniae alba, ginseng radix, achyranthis radix, glycyrrhrizae radix at 75+ -5deg.C to meet water requirement, and parching radix Angelicae sinensis, curcumae rhizoma, and Glycyrrhrizae radix to obtain parched radix Angelicae sinensis, vinegar Curcumae rhizoma, and parched Glycyrrhrizae radix.
Further, in the step D, the conditions of sublimation drying are:
maintaining the temperature at-40 ℃ for 1h;
maintaining the temperature at-30 ℃ for 1h;
maintaining the temperature at-20 ℃ for 2 hours;
maintaining the temperature at-10deg.C for 3 hr;
the temperature was maintained at 0℃for 3 hours.
Further, in the step D, the conditions for analytical drying are:
maintaining the temperature at 10 ℃ for 3 hours and the pressure at 0.0pa;
maintaining the temperature at 20 ℃ for 2 hours and the pressure at 0.0pa;
maintaining the temperature at 30 ℃ for 2 hours and the pressure at 0.0pa;
the temperature was 45℃and the pressure was 0.0pa for 22 hours.
Further, in the step a,
the stir-fried angelica sinensis stir-frying method comprises the following steps: parching radix Angelicae sinensis slice with slow fire to yellow, taking out, and spreading to cool;
the stir-frying method of the vinegar curcuma zedoary comprises the following steps: adding vinegar into Curcumae rhizoma according to the ratio of 20kg rice vinegar per 100kg Curcumae rhizoma, stirring, decocting to penetrate heart, taking out, cooling, slicing into 2-4mm thick slices, and drying;
the stir-fried licorice root stir-frying method comprises the following steps: parching Glycyrrhrizae radix tablet with slow fire to yellow, taking out, and spreading to cool.
Further, in the step B, each decoction piece in the step A is weighed according to the formula of the decoction for warming channels, and is decocted for 30min after 8 times of water is added for soaking for 30min; decocting with 6 times of water for 20min, mixing decoctions, filtering, and collecting filtrate.
Further, in the step B, the condition of filtration is that filtration is performed by using a 200 mesh filter, and 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 sinensis, ligusticum wallichii, white paeony root, cinnamon, moutan bark, rhizoma curcumae, and 41.3 parts of ginseng, achyranthes root and liquorice respectively.
The freeze-dried powder of the channel warming soup control extract has the moisture of 5.2-6.8%, yellow to brown yellow powder, slight smell, bitter taste and sweet taste.
Compared with the prior art, the invention has the following advantages:
(1) In the invention, based on the classical formula of the traditional Chinese medicine, namely the decoction of the stomach and the channel warming, on the basis of the traditional decoction method, the extraction solvent, the decoction times, the decoction time and the water addition amount are inspected, and then the corresponding decoction of the stomach and channel warming is prepared, and the characteristic spectrum research is carried out on the extract, so that the method can be used for qualitative identification of the corresponding decoction.
(2) In the invention, the preparation of the control extract has important significance: firstly, providing technical support for quality control of a declaration control extract and a compound preparation of Chinese food and drug verification institute, and having stronger creativity; and secondly, the repeated working procedures of pretreatment, prescription, extraction, component identification and the like are avoided while the call of the multi-index overall quality control of the traditional Chinese medicine is responded, so that the experimental operation is simpler and more convenient, and the consumption of resources is reduced. Can provide guarantee for the quality control of traditional Chinese medicine classical prescription decoction and lay a foundation for international popularization.
(3) In the invention, the reference extract of the Wenjing decoction is subjected to quality control by taking the whole reference substance as a reference, so that the whole quality control in the true 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 reference extract of the Wenjing decoction represents the integral internal quality of the preparation, and can provide reference basis for the related preparation of the subsequent classical formula Wenjing decoction.
Drawings
FIG. 1 is a graph showing the water absorption rate of the Wenjing decoction of example 4.
FIG. 2 is a comparison characteristic spectrum of the decoction for warming meridians in example 9.
FIG. 3 is a characteristic spectrum of the extract of Wenzhen decoction of 10 batches in example 10.
Detailed Description
The invention provides a reference extract of a Wenjing decoction and a preparation method thereof, and the invention is further described in detail below in order to make the purposes, technical schemes and effects of the invention clearer and more definite. It should be understood that the specific embodiments described herein are for purposes of understanding only and are not intended to limit the present invention.
The experimental apparatus and materials involved in the examples are as follows:
an electronic balance: shanghai Fang Rui instruments, JY series one-day flat;
decocting pot: 4 liters of a full-automatic split ceramic medicine decocting pot for the family of delicious;
and (3) screening: nine-peak screen 200 mesh;
vacuum freeze dryer: LGJ-100F of Beijing pine source Huaxing technology development Co., ltd;
penicillin bottle capping machine: SZ20A;
a plurality of 2000ml stainless steel measuring cups; penicillin bottle: 10ml,30ml,50 ml;
high performance liquid chromatograph: waters 2695-2996 type high performance liquid chromatograph, agilent 1260 type high performance liquid chromatograph, shimeji 20-AD type high performance liquid chromatograph;
ultrasonic cleaner: KQ5200DB model (600W, 40KHz; kunshan ultrasonic instruments Co., ltd.);
an electronic balance: shanghai Fang Rui instruments, JY series one-day flat, ME204E/02, MS205DU,
XP26 (Metrele Tolyduo instruments Co., ltd.);
ultrapure water machine: cell type 1810A (Shanghai mueller scientific instruments limited);
chromatographic column: agilent ZORBAX SB-C18 250X 4.6mm, kromasil C18 5 μm 4.6X 250mm,
Phenomenex Luna 5um C18(2)100A 4.6×250mm。
Reagent: acetonitrile is chromatographic purity, water is ultrapure water, and the rest reagents are analytical purity;
reagent: gallic acid, paeoniflorin, and glycyrrhizic acid reference substance;
angelica sinensis, ligusticum wallichii, radix paeoniae alba, cinnamon, cortex moutan, rhizoma curcumae zedoariae (zedoary), achyranthes root and liquorice (liquorice) (provided by Sichuan new green pharmaceutical technology development Co., ltd.);
control extracts of Wenjing decoction (manufactured by Sichuan New Green pharmaceutical 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 reference extract of Wenjing decoction, which comprises the following steps:
A. pretreatment of medicinal materials: taking Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, zedoary, ginseng, twotooth achyranthes root, liquoric root and cassia bark, removing sediment and impurities from non-medicinal parts, moistening, cutting, drying, and then stir-baking the Chinese angelica, the zedoary and the liquoric root to obtain stir-baked Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, vinegar zedoary, ginseng, twotooth achyranthes root, stir-baked liquoric root and cassia bark decoction pieces;
B. decocting: weighing each decoction piece in the step A according to the formula of the decoction for warming channels, adding 6-8 times of water, soaking for 20-40min, decocting for 20-30min, decocting for 2-3 times, mixing the medicinal liquids, filtering, and collecting filtrate;
C. concentrating: concentrating the filtrate in the step B to a relative density of 1.02-1.06 at 50+ -2deg.C and under vacuum degree of 0.080Mpa to obtain concentrated solution;
D. and (3) freeze drying: c, pre-freezing the concentrated solution in the step C, sublimating and drying under the condition of the pressure of 0.0pa, resolving and drying, collecting powder at the temperature of 10-26 ℃ and the relative humidity of 40-60%, weighing, split charging into brown penicillin bottles, and sealing to obtain the freeze-dried powder of the extract of the Wenzhen soup.
Example 2
In the embodiment, in the step a, after the step a is performed by taking the medicinal angelica, the hemlock parsley, the white peony root, the moutan bark, the zedoary, the ginseng, the achyranthes root, the licorice and the cinnamon, the specific pretreatment method is as follows:
chinese angelica root: removing impurities, cleaning, moistening, cutting into 1-2mm slices, and drying at low temperature. Parching radix Angelicae sinensis with slow fire to yellow, taking out, and spreading to cool.
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.
Cortex moutan radicis): rapidly cleaning, moistening, cutting into 1-2mm slices, and sun drying.
Zedoary turmeric: removing impurities, soaking, cleaning, adding vinegar (20 kg rice vinegar for each 100kg Curcumae rhizoma), stirring, decocting to permeate into heart, taking out, cooling, slicing into 2-4mm thick pieces, and drying.
Ginseng: moistening thoroughly, cutting into 1-2mm slices, and drying.
Achyranthes root: removing impurities, cleaning, moistening, removing residual rhizoma Phragmitis, cutting into short sections of 5-10mm, and drying.
Licorice (licorice): removing impurities, cleaning, moistening, cutting into 2-4mm thick pieces, and drying. Parching Glycyrrhrizae radix tablet with slow fire to yellow, taking out, and spreading to cool.
Cinnamon: removing impurities and coarse skin. Mashing the materials when in use.
When the decoction pieces are moistened, the decoction pieces are generally moistened until the inner core is thoroughly moistened by hand-held examination; the length of the cut decoction pieces is checked, and the special-shaped pieces are not more than 10 percent. And then the qualified decoction pieces are sent into a decoction kettle for the next decoction step.
Example 3
The present example is an examination of the properties of the control extract of Wenzhen decoction.
The solid powder is prepared by the process of the reference extract of the Wenzhen decoction. The properties and moisture of the 10 batches of Wenzhen decoction control extracts are shown in tables 1 and 2 respectively.
Table 1:10 batches of Wenzhen decoction control extract character
Table 2: moisture examination of 10 batches of Wenzhen decoction control extract
From the detection results of the channel warming soup control extracts of a plurality of batches, the channel warming soup control extracts are yellow to brown yellow powder, have slight smell, and have bitter taste and sweet taste; the water content of the control extract of the Wenjing decoction 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, the water absorption of different decoction pieces is different, so that the water absorption of the decoction pieces with the function of warming channels needs to be examined, and the reference is made for the water addition amount. This example examined mainly the change in water absorption rate when the Wenying decoction control extract was prepared.
100g of decoction pieces with the prescription amount (calculated according to the proportion of 20.6 parts of angelica sinensis, ligusticum wallichii, white paeony root, cinnamon, moutan bark and curcuma zedoary respectively, 41.3 parts of ginseng, achyranthes bidentata and liquorice respectively) are weighed, 8 times of water (the weight of the decoction pieces with the prescription amount is the water volume) is respectively added into the decoction pieces, and the water absorption rate is calculated by measuring the decoction pieces respectively in 10min,20min,30min,50min,1h,1.5h,2h,4h,6h,8h,16h and 24h, and the water absorption rate curve is shown in the figure 1.
Table 3: water absorption data of the decoction for warming meridians
As can be seen from Table 3 and FIG. 1, the temperature course Shang Yinpian was rapidly absorbed in the first 1.5 hours, gradually decreased after 2 hours, and the water absorption was nearly saturated in 12 hours, and the average water absorption was 268.8%. The water absorption is about 2.5 times.
Reference is made to the opinion of the "water addition" section of the "quality control and Standard preparation technical requirement of Chinese medicine formulation" section (solicited opinion manuscript): because the texture 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 adding amount is 2-5 cm after soaking the decoction pieces of flowers, grasses or decoction pieces with longer decoction time, and the water adding amount is 8 times of the decoction pieces in the first decoction in the preparation step of the decoction for warming channels and the water adding amount is 6 times of the decoction pieces in combination with the previous test.
Example 5
On the basis of example 4, the water addition amount and the extraction times of the decoction for warming channels are examined, the water absorption rate is referred, the water addition amount of the first decoction is adjusted to be 8 times, the water addition amount of the second decoction is set to be 6 times, and the extraction is carried out for 2 times; or the multiple of the first decoction and the water adding amount is adjusted to 7 times, the water adding amount of the second decoction is adjusted to 6 times, the extraction is carried out for 2 times, the final result difference of the water adding amount of each time controlled to 6-8 times of the water adding amount is not big, but when the water adding amount is adjusted to 9 times, the time length of the subsequent concentration process is obviously prolonged, so that the first decoction and the water adding amount is adjusted to 8 times, the water adding amount of the second decoction is adjusted to 6 times, the extraction is carried out for 2 times, and the efficiency is higher.
Example 6
The embodiment is to examine the soaking time in the preparation process of the reference extract of the Wenying decoction.
Taking 100g of decoction pieces with the prescription amount of the decoction pieces 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 core is wet.
The results show that: taking decoction pieces with the dosage of the decoction pieces, 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. When the decoction pieces are soaked for 10min, most decoction pieces are not soaked thoroughly; when the decoction pieces are soaked for 20min, most of the inner cores are wet, and a small amount of the inner cores of the longer decoction pieces are not wet; and wetting all inner cores of the decoction pieces when soaking for 30min, and determining the soaking time to be 30min.
Example 7
This example is an examination of the cooling process in the process of preparing the Wenzhen soup control extract.
According to the requirements in the requirements of declaration data (claiming opinion manuscript) of the substance standard of the traditional Chinese medicine compound preparation of the ancient classical prescription, the extract is preferably prepared by adopting a freeze drying method in the drying process of the extract, so that the stability of the quality of the extract can be ensured, and the extract is easy to store. For the examination of the freeze-drying process parameters, two control conditions of the freeze-drying process are listed, and are shown in tables 4-1 and 4-2.
Table 4-1: freeze-drying process of reference extract of Wenzhen decoction
Table 4-2: freeze-drying process (II) of reference extract of Wenzhen decoction
The two freeze-dried powders are obtained by the freeze-drying process and the control parameters in the table. The detection of the two freeze-dried powders shows that the freeze-dried powder obtained by the technological parameters in the table 4-1 is looser and drier, and is more beneficial to storage. The process conditions corresponding to the control parameters of table 4-1 are finally selected.
And then the freeze-dried powder obtained by the process is quickly collected, weighed and packaged in brown penicillin bottles under the environment of the temperature of 10-26 ℃ and the relative humidity of 40-60%, and the bottles are sealed and labeled.
Example 8
In this embodiment, the decoction of the reference extract of the Wenying decoction is verified, and according to the above implementation, the investigation of the preparation process of the reference extract of the Wenying decoction is performed, and the finally determined preferred process is as follows: decocting decoction pieces with the dosage of the decoction for warming channels twice, adding 8 times of water for one decoction, soaking for 30 minutes, boiling, keeping micro-boiling, decocting for 30 minutes, filtering with 200 mesh sieve, and immediately cooling to room temperature; adding 6 times of water into the second decoction, boiling, keeping micro-boiling, decocting for 20 minutes, filtering with 200 mesh screen, and immediately cooling to room temperature; mixing the water decoctions, lyophilizing, and packaging.
With the preparation process, 10 batches of the reference extract of the Wenzhen decoction were decocted, and the results are shown in Table 5.
Table 5: data summary of 10 batches of Wenzhen decoction control extracts
As can be seen from Table 5, the powder yield of the control extract of 10 Wenzhen decoction batches was 27.37% on average. SD is 1.17. 70% -130% of the average value ranges from 19.16% -35.58%. The average value plus or minus 3 times SD is 23.86% -30.88%. The data are in a normal range and can be used as references of the production process.
Example 9
The embodiment is a characteristic spectrum construction method for using the freeze-dried powder of the Wenzhen soup control extract obtained in the technical scheme for the Wenzhen soup control extract, and then using the obtained spectrum for qualitative detection of the Wenzhen soup compound preparation.
a. Preparation of a control solution: mixing gallic acid, paeoniflorin and glycyrrhizic acid reference substance with 70% methanol to obtain mixed solution containing 40 μg per 1 ml.
b. Preparation of test solution: about 0.5g of the powder is taken, precisely weighed, placed in a conical bottle with a plug, precisely added with 25ml of 70% methanol, sealed, weighed, subjected to ultrasonic treatment (power 300W, frequency 25 kHz) for 30 minutes, cooled, weighed again, complemented with 70% methanol by weight, shaken uniformly, filtered, and the subsequent filtrate is taken, thus obtaining the product.
c. And (3) detection: c, injecting the reference substance solution and the test substance solution obtained in the step a and the step b into a high performance liquid chromatograph for detection, taking the characteristic spectrum of the reference substance solution as a reference spectrum, selecting a common peak from the characteristic spectrum of the test substance solution, and constructing the characteristic spectrum of the reference extract of the Wenzhen decoction.
The high performance liquid chromatography detection conditions meet the following conditions:
chromatographic column: octadecylsilane chemically bonded silica is used as a filler (column length is 250mm, inner diameter is 4.6mm, and granularity is 5 μm);
column temperature: 30 ℃;
flow rate: 1.0ml/min;
sample injection amount: 10 μl;
detection wavelength: 254nm;
the mobile phase A is acetonitrile, the mobile phase B is 0.1% phosphoric acid aqueous solution, and the gradient elution is carried out.
The gradient elution process comprises the following steps:
0 to 3min, 2 percent of mobile phase A and 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, 40-60% of mobile phase A, 60-40% of mobile phase B,
60 to 75 minutes, 60 to 95 percent of mobile phase A, 40 to 5 percent of mobile phase B,
75-80 min, 95% of mobile phase A and 5% of mobile phase B.
d. C, taking the characteristic spectrum of the reference substance solution in the step c as a reference spectrum, selecting a common peak from the characteristic spectrum of the test substance solution, and constructing the characteristic spectrum of the reference extract of the Wenzhen decoction.
The sample characteristic spectrum should show 16 characteristic peaks, wherein peak 1, peak 6 and peak 13 should correspond to the retention time of reference substances of gallic acid, paeoniflorin and glycyrrhizic acid respectively. The peak corresponding to the paeoniflorin reference peak is taken as an S1 peak, the relative retention time of the peak 2-peak 10 and the S1 peak is calculated, and the relative retention time is within the range of +/-8% of a specified value. The predetermined values were 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 peak was regarded as the S2 peak, and the relative retention time of the peaks 11 to 16 and the S2 peak was calculated so that the relative retention time was within.+ -. 8% of the predetermined value. The predetermined values were 0.862 (peak 11), 0.961 (peak 12), 1.148 (peak 14), 1.178 (peak 15), 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: glycyrrhizin; peak 13 (S2): glycyrrhizic acid.
Example 10
Feature spectrum verification of extract of Wenzhen decoction
According to the characteristic spectrum detection method of the warm channel soup control extract, 10 batches (S1-S10 are WJT200901, WJT200902, WJT200903, WJT200904, WJT200905, WJT200906, WJT200907, WJT200905, WJT200909 and WJT 200910) of warm channel soup control extracts are subjected to characteristic spectrum verification, and the result is shown in figure 3.
The quality control of the reference extract of the Wenzhen decoction can be carried out on the whole by adopting the characteristic spectrum so as to ensure the quality uniformity and stability; the result shows that the quality of the 10 batches of the temperature-channel decoction control extract is uniform and stable.
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.
Claims (9)
1. A method for constructing a characteristic spectrum of a decoction extract for warming channels is characterized in that,
a. preparation of a control solution: adding 70% methanol into gallic acid, paeoniflorin and glycyrrhizic acid reference substances respectively to obtain mixed solutions containing 40 μg per 1 ml;
b. preparation of test solution: taking about 0.5g of the powder, precisely weighing, placing into a conical bottle with a plug, precisely adding 25ml of 70% methanol, sealing, weighing, performing ultrasonic treatment for 30 minutes, cooling, weighing again, supplementing the lost weight with 70% methanol, shaking uniformly, filtering, and collecting the subsequent filtrate;
c. and (3) detection: c, injecting the reference substance solution and the test substance solution obtained in the step a and the step b into a high performance liquid chromatograph for detection, taking the characteristic spectrum of the reference substance solution as a reference spectrum, selecting a common peak from the characteristic spectrum of the test substance solution, and constructing a characteristic spectrum of a reference extract of the Wenzhen decoction;
d. c, taking the characteristic spectrum of the reference substance solution in the step c as a reference spectrum, selecting a common peak from the characteristic spectrum of the test substance solution, and constructing the characteristic spectrum of the Wenzhen soup reference extract, wherein the characteristic spectrum of the test substance should show 16 characteristic peaks, and peak 1, peak 6 and peak 13 should respectively correspond to the retention time of the reference substance peaks of gallic acid, paeoniflorin and glycyrrhizic acid reference substances, wherein the peak 1: gallic acid, peak 2: l-tryptophan, peak 3: protocatechuic acid, peak 4: chlorogenic acid, peak 5: albiflorin, peak 6: paeoniflorin, peak 8: glycyrrhizin; peak 13: glycyrrhizic acid;
the high performance liquid chromatography detection conditions are as follows:
chromatographic column: octadecylsilane chemically bonded silica is used as a filler, the column length is 250mm, the inner diameter is 4.6mm, and the granularity is 5 mu m;
column temperature: 30 ℃;
flow rate: 1.0ml/min;
sample injection amount: 10 μl;
detection wavelength: 254nm;
the mobile phase A is acetonitrile, the mobile phase B is 0.1% phosphoric acid aqueous solution, and the gradient elution is carried out;
the gradient elution process comprises the following steps:
0 to 3min, 2 percent of mobile phase A and 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, 40-60% of mobile phase A, 60-40% of mobile phase B,
60 to 75 minutes, 60 to 95 percent of mobile phase A, 40 to 5 percent of mobile phase B,
75-80 min, 95% of mobile phase A and 5% of mobile phase B;
the preparation method of the channel warming soup control extract comprises the following steps:
A. pretreatment of medicinal materials: taking Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, zedoary, ginseng, twotooth achyranthes root, liquoric root and cassia bark, removing sediment and impurities from non-medicinal parts, moistening, cutting, drying, and then stir-baking the Chinese angelica, the zedoary and the liquoric root to obtain stir-baked Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, vinegar zedoary, ginseng, twotooth achyranthes root, stir-baked liquoric root and cassia bark decoction pieces;
B. decocting: weighing each decoction piece in the step A according to the formula of the decoction for warming channels, adding 6-8 times of water, soaking for 20-40min, decocting for 20-30min, decocting for 2-3 times, mixing the medicinal liquids, filtering, and collecting filtrate;
C. concentrating: concentrating the filtrate in the step B to a relative density of 1.02-1.06 at 50+ -2deg.C and under vacuum degree of 0.080Mpa to obtain concentrated solution;
D. and (3) freeze drying: c, pre-freezing the concentrated solution in the step C, sublimating and drying under the condition of the pressure of 0.0pa, resolving and drying, collecting powder at the temperature of 10-26 ℃ and the relative humidity of 40-60%, weighing, split charging into brown penicillin bottles, and sealing to obtain the freeze-dried powder of the extract of the Wenzhen soup.
2. The method for constructing a characteristic spectrum of a decoction extract according to claim 1, wherein in the step a, the pretreatment method of the medicinal materials is as follows:
taking Chinese angelica, szechuan lovage rhizome, white paeony root, tree peony bark, zedoary, ginseng, twotooth achyranthes root and liquoric root, removing sediment and non-medicinal parts, taking Chinese cinnamon, and removing impurities and crude skin; spraying clear water for 2-3 times, moistening for 1-2 hours, rapidly cleaning cortex moutan, slightly soaking Curcumae rhizoma, 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 sections; drying radix Angelicae sinensis and cortex moutan at 50+ -5deg.C, drying rhizoma Ligustici Chuanxiong, radix Paeoniae alba, ginseng radix, achyranthis radix, glycyrrhrizae radix at 75+ -5deg.C to meet water requirement, and parching radix Angelicae sinensis, curcumae rhizoma, and Glycyrrhrizae radix to obtain parched radix Angelicae sinensis, vinegar Curcumae rhizoma, and parched Glycyrrhrizae radix.
3. The method for constructing a feature map of a wenjing decoction extract according to claim 2, wherein in the step D, the condition of sublimation drying is:
maintaining the temperature at-40 ℃ for 1h;
maintaining the temperature at-30 ℃ for 1h;
maintaining the temperature at-20 ℃ for 2 hours;
maintaining the temperature at-10deg.C for 3 hr;
the temperature was maintained at 0℃for 3 hours.
4. The method for constructing a feature map of a decoction extract according to claim 3, wherein in the step D, the conditions for analytical drying are:
maintaining the temperature at 10 ℃ for 3 hours and the pressure at 0.0pa;
maintaining the temperature at 20 ℃ for 2 hours and the pressure at 0.0pa;
maintaining the temperature at 30 ℃ for 2 hours and the pressure at 0.0pa;
the temperature was 45℃and the pressure was 0.0pa for 22 hours.
5. The method for constructing a feature map of a Wenzhen decoction extract according to claim 4, wherein in the step A,
the stir-fried angelica sinensis stir-frying method comprises the following steps: parching radix Angelicae sinensis slice with slow fire to yellow, taking out, and spreading to cool;
the stir-frying method of the vinegar curcuma zedoary comprises the following steps: adding vinegar into Curcumae rhizoma according to the ratio of 20kg rice vinegar per 100kg Curcumae rhizoma, stirring, decocting to penetrate heart, taking out, cooling, slicing into 2-4mm thick slices, and drying;
the stir-fried licorice root stir-frying method comprises the following steps: parching Glycyrrhrizae radix tablet with slow fire to yellow, taking out, and spreading to cool.
6. The method for constructing a characteristic spectrum of a decoction extract of a menorrhena-treating type according to claim 5, wherein in the step B, each decoction piece in the step A is weighed according to a formula of the menorrhena-treating type, and water with a volume of 8 times is added for soaking for 30min and decocting for 30min; decocting with 6 times of water for 20min, mixing decoctions, filtering, and collecting filtrate.
7. The method of claim 6, wherein in the step B, the filtering condition is that a 200 mesh filter is used for filtering, and the filtrate is collected.
8. The method for constructing a characteristic spectrum of a decoction extract according to any one of claims 1 to 7, wherein the decoction is prepared from the following components in parts by weight: 20.6 parts of angelica sinensis, ligusticum wallichii, white paeony root, cinnamon, moutan bark, rhizoma curcumae, and 41.3 parts of ginseng, achyranthes root and liquorice respectively.
9. The method for constructing a characteristic spectrum of a decoction extract for warming meridians according to claim 8, wherein the method comprises the following steps: the water content of the freeze-dried powder of the reference extract of the Wenzhen decoction is 5.2-6.8%, the powder is yellow to brown yellow, the smell is slight, and the taste is bitter and sweet.
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| CN110907553A (en) * | 2019-12-08 | 2020-03-24 | 山东沃华医药科技股份有限公司 | Meridian warming soup fingerprint detection method |
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| CN111044624A (en) * | 2019-10-31 | 2020-04-21 | 广州白云山中一药业有限公司 | Quality detection method of Chinese medicinal preparation |
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