CN109172635B - Preparation method of traditional Chinese medicine composition containing cassia twig - Google Patents

Preparation method of traditional Chinese medicine composition containing cassia twig Download PDF

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CN109172635B
CN109172635B CN201811056431.4A CN201811056431A CN109172635B CN 109172635 B CN109172635 B CN 109172635B CN 201811056431 A CN201811056431 A CN 201811056431A CN 109172635 B CN109172635 B CN 109172635B
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parts
inclusion
water
chinese medicine
traditional chinese
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CN109172635A (en
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季光
王冰
顾思浩
李玲
张彤
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Shanghai University of Traditional Chinese Medicine
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Abstract

The invention provides a preparation method of a cassia twig-containing traditional Chinese medicine composition, which is characterized in that effective parts of the traditional Chinese medicine composition are obtained by extraction, volatile components of the effective parts are collected by adopting a steam distillation method, the volatile components are subjected to cyclodextrin inclusion, and the volatile components and pharmaceutically acceptable auxiliary materials are prepared into an oral preparation. Compared with the traditional process, the improved inclusion process has the following advantages: 1. for the traditional Chinese medicine components which can not collect the volatile oil, the aromatic water can be directly extracted for inclusion, the volatile oil does not need to be purified continuously through complicated purification operation, the oil-water separation is not needed, and the inclusion operation is simpler and more convenient; 2. the inclusion process is easy to operate, has good repeatability, aromatic water does not need to be concentrated, cyclodextrin is directly added, the time consumption is shorter, the inclusion temperature is lower, and the cyclodextrin dosage is less; 3. the transfer rate of volatile components and the inclusion yield of the obtained inclusion compound are higher; 4. the water-soluble components and volatile components in the prescription are reserved, and the medicine is closer to the real state of clinical administration of a classical prescription.

Description

Preparation method of traditional Chinese medicine composition containing cassia twig
Technical Field
The invention belongs to the field of traditional Chinese medicines, and particularly relates to a preparation method of a traditional Chinese medicine composition containing cassia twig.
Background
Ling Gui Zhu gan Tang is from Zhang Zhong Jing jin Kui Yao L ü e, and has the effects of warming yang, resolving fluid retention, invigorating spleen and removing dampness. The prescription is mainly used for treating symptoms such as heart-down fullness, chest-rushing or chest-hypochondrium fullness due to deficiency of heart-spleen yang and adverse flow of qi due to retention of fluid, dizziness, palpitation, short breath, difficult urination and the like, and is a representative prescription for tonifying qi, warming yang and invigorating spleen to resolve fluid retention. The prescription consists of four commonly used medicines of tuckahoe, cassia twig, rhizoma atractylodis macrocephalae and liquorice, wherein the tuckahoe is a monarch drug and is used for excreting dampness, strengthening spleen, eliminating phlegm and resolving dampness; ramulus Cinnamomi is used as ministerial drug for warming yang, regulating qi, and distributing body fluid; the combination of the whole formula has the effects of warming yang and inducing diuresis by assisting with the white atractylodes rhizome to eliminate dampness and strengthen spleen and using the liquorice to tonify spleen and replenish qi. The traditional Chinese medicine composition is clinically used for treating weakness of spleen and stomach, lassitude and hypodynamia, palpitation and shortness of breath, cough and excessive phlegm, abdominal and limb spasm and pain, carbuncle and swelling and sore toxicity, relieving drug toxicity, severity and the like.
The astragalus and cassia twig five-ingredient decoction is also from Zhang Zhongjing, jin Kui Yao L ü e, and is a prescription for reviving yang qi, warming and activating blood, and regulating ying and wei. The prescription consists of five medicaments of astragalus, cassia twig, peony, ginger and Chinese date. In the formula, the astragalus root is sweet in taste, and can greatly tonify primordial qi and dredge channels and collaterals, and the astragalus root, the cassia twig and the ginger are matched to tonify qi, strengthen exterior, dispel cold and remove stagnation. The combination of astragalus root and white peony root has the functions of benefiting qi, nourishing blood and tonifying qi and blood. In addition, Gui Zhi is combined with Shao Dan to achieve the effects of harmonizing Ying and Wei, relieving muscular and muscular pain and alleviating pain. The medicines are combined, so that the traditional Chinese medicine composition can eliminate pathogenic factors and strengthen body resistance, can ensure sufficient qi and blood, smooth blood circulation, relieve pain and remove bone impediment, and has the effects of tonifying qi and nourishing blood, and promoting blood circulation by removing blood stasis and dredging collaterals. It is used clinically to treat dermatitis, peripheral neuritis, apoplexy sequelae, etc.
At present, no Chinese patent medicine exists in the market for both the tuckahoe, cassia twig, rhizoma atractylodis and licorice root decoction and the astragalus and cassia twig five-substance decoction, and the decoction is taken clinically. However, the formula of the traditional Chinese medicine for warming yang, namely the cassia twig, is the common medicinal flavor of the decoction, and the cassia twig is a common formula medicine in various classical formulas and modern formulas, wherein the main effective component of the cassia twig is a volatile substance with the content of about 1 percent, the chemical components are complex, and the cinnamaldehyde is the main component. Cinnamaldehyde has obvious analgesic and sedative effects, but the unstable and volatile characteristics of cinnamaldehyde have important influence on the stability of a pharmaceutical preparation. For such compound preparations, the general preparation method is: extracting with water, collecting volatile oil, spraying the volatile oil onto medicinal powder or starch, or adding the volatile oil into saturated solution of beta-cyclodextrin, stirring, and making into various dosage forms. Although the preparation method is simple to operate, the stability of the medicine is poor, the medicine cannot be stored for a long time, and the extraction and inclusion efficiency of the volatile oil of the medicine is low, so that the medicine effect is influenced.
The inclusion technology of Chinese medicine volatile oil is related to the existence state of Chinese medicine volatile components. The most commonly used volatile component inclusion techniques are reported to have the following two limitations: (1) the existing inclusion technology is more suitable for including the volatile oil of the traditional Chinese medicine, and an inclusion method which is not suitable for the volatile components of aromatic water does not exist; (2) in the conventional inclusion process, the general material addition sequence is as follows: adding the volatile oil into the saturated solution of beta-cyclodextrin, stirring, filtering and drying to obtain the clathrate compound. However, many herbal compositions may contain one or more volatile components, and the volatile oil has different densities or is close to water, so that oil-water separation is difficult, the volatile oil cannot be separated, and only the volatile components of aromatic water can be collected. Patent document 1(CN 102688277B) discloses a pharmaceutical composition for removing dampness and relieving arthralgia, a preparation and application thereof, wherein volatile oil is extracted by steam distillation and added into cyclodextrin solution for inclusion. Patent document 2(CN 101757641B) discloses a preparation process of cardamom volatile oil inclusion compound, which comprises extracting volatile oil by steam distillation, preparing beta-cyclodextrin into saturated solution, and slowly adding the volatile oil for inclusion. In the above processes, volatile oil can be obtained by steam distillation. While the method is easy to generate white floccule which is insoluble in water and oil during decoction (steam distillation), oil-water separation is difficult, and only aromatic water can be collected, but volatile oil cannot be obtained.
Disclosure of Invention
The invention provides a preparation method of a traditional Chinese medicine composition containing cassia twig. The invention establishes a new inclusion mode suitable for volatile components which contain oil and water and are difficult to separate in a compound preparation while keeping the effective components of the water decoction, namely, the invention directly adds beta-cyclodextrin into aromatic water for inclusion.
Specifically, the invention provides a preparation method of a cassia twig-containing traditional Chinese medicine composition, wherein the traditional Chinese medicine composition is prepared from traditional Chinese medicine raw materials, the traditional Chinese medicine raw materials comprise 9-90 parts by weight of cassia twig, and the preparation method comprises the following steps:
firstly, weighing traditional Chinese medicine raw materials according to a prescription, adding 6-12 times of water to soak for 30-120 min, extracting for 1-3 times, wherein the first time of steam distillation extraction is performed for 1-5 h, and collecting 0.5-2 times of aromatic water for later use; combining the water extract, and concentrating under reduced pressure at 60-80 ℃ until the relative density is 1.05-1.15 at the corresponding temperature;
filtering the water extraction concentrated solution or centrifuging at a high speed of 5000-15000 rpm, or adding 0.5-3 times of ethanol for alcohol precipitation, and concentrating the extracting solution or supernatant of the alcohol precipitation solution at 50-70 ℃ under reduced pressure until the relative density is 1.15-1.30;
drying the ethanol precipitation solution or the centrifugal concentrated solution after the reduced pressure concentration in a vacuum drying oven at 50-70 ℃ to obtain dry extract, and crushing to obtain extract powder;
weighing beta-cyclodextrin with 1/5-1/20 aromatic water amount, adding the beta-cyclodextrin into the collected aromatic water, keeping the temperature at 40-60 ℃, stirring for 1-3 h, cooling to room temperature after stirring, and refrigerating for 24h at-4 ℃; filtering, discarding the filtrate, drying the filtered substance in an oven at 40-60 ℃ for 4h, grinding to obtain a white powdery inclusion compound, and mixing with the extract powder.
In a preferred embodiment, the traditional Chinese medicine composition is prepared from the following traditional Chinese medicine raw materials in parts by weight: 12-120 parts of poria cocos, 9-90 parts of cassia twig, 9-90 parts of bighead atractylodes rhizome or honey bran-fried bighead atractylodes rhizome, and 6-60 parts of liquorice or honey-fried liquorice.
In another preferred embodiment, the Chinese medicinal raw materials comprise the following components in parts by weight: 36 parts of poria cocos, 27 parts of cassia twig, 27 parts of bighead atractylodes rhizome or honey bran-fried bighead atractylodes rhizome, and 18 parts of liquorice or honey-fried liquorice.
In another preferred embodiment, the traditional Chinese medicine composition is prepared from the following traditional Chinese medicine raw materials in parts by weight: 9-90 parts of astragalus membranaceus, 9-90 parts of Chinese herbaceous peony, 9-90 parts of cassia twig, 18-180 parts of ginger and 12-120 parts of Chinese date.
In another preferred embodiment, the Chinese medicinal raw materials comprise the following components in parts by weight: 27 parts of astragalus, 27 parts of Chinese herbaceous peony, 27 parts of cassia twig, 54 parts of ginger and 36 parts of Chinese date.
In another preferred embodiment, in the step one, 1-1.5 times of the amount of the medicinal material is collected.
In another preferred example, in the fourth step, 1/10-1/15 of beta-cyclodextrin in aromatic water is weighed.
The technical details of various aspects of the present invention will be described in detail later. The features, objects, and advantages of the invention will be apparent from the description and from the claims.
Drawings
Figure 1 cinnamic acid specificity inspection chromatograms. (a) A cinnamic acid reference; (b) a cassia twig negative test sample; (c) full prescription test article
FIG. 1 shows that: the negative control solution is not absorbed at the corresponding position of the cinnamic acid, which indicates that other medicines in the prescription have no interference to the measurement of the cinnamic acid, and the content measurement specificity of the cinnamic acid in the extracting solution is good.
FIG. 2 is a chromatogram for liquiritin specificity study. (a) Liquiritin reference substance; (b) licorice negative test sample; (c) full prescription test article
FIG. 2 shows that: the negative control solution is not absorbed at the corresponding position of the liquiritin, which shows that other medicines in the prescription have no interference to the liquiritin determination, and the content determination specificity of the liquiritin in the extracting solution is good.
FIG. 3 is a chromatogram for examining specificity of cinnamaldehyde. (a) Cinnamic aldehyde as a control; (b) a cassia twig negative test sample; (c) clathrate compound test article
FIG. 3 shows: the negative control solution is not absorbed at the corresponding position of the cinnamaldehyde, which indicates that other medicines in the prescription have no interference to the measurement of the cinnamaldehyde, and the content measurement specificity of the cinnamaldehyde in the clathrate compound is good.
FIG. 4 is a chromatogram of volatile components from the recipe. (a) Volatile oil; (b) inclusion compound; (c) removing the inclusion compound; (d) a cyclodextrin; (e) a physical mixture.
FIG. 4 shows that: in the inclusion process, the property of the inclusion compound is not changed, and volatile components of the Siberian cocklebur-cassia twig-atractylodes rhizome-licorice compound enter beta-cyclodextrin molecules to form a beta-cyclodextrin inclusion compound, and the modes of non-surface adsorption combination and the like are adopted.
Detailed Description
The traditional Chinese medicine composition is prepared from 4 traditional Chinese medicines including poria cocos, cassia twig, bighead atractylodes rhizome and liquorice. In the formula, the poria cocos is a monarch drug and plays roles of excreting dampness, tonifying spleen, eliminating phlegm and resolving dampness, the cassia twig is a ministerial drug and has the functions of warming yang, regulating qi, tonifying qi, promoting the production of body fluid, distributing body fluid, and the bighead atractylodes rhizome and the liquorice are used as assistants to tonify qi and invigorate spleen, so that the whole formula has the functions of warming yang and promoting diuresis. However, in the method, the oil-water separation is difficult during the steam distillation, and only aromatic water can be collected without obtaining volatile oil. Therefore, the invention aims to solve the common problem of aromatic water inclusion when the volatile components are extracted from the compound and provide a new inclusion technology, and the invention is the main aim of the invention. The invention finds a solution idea and a scheme suitable for a new technology of aromatic water inclusion through sufficient experimental research, and proves the solution through experimental data.
Specifically, taking the linggui zhu gan tang as an example, the inventor has made the following research works:
1 study of extraction Process
1.1 preparation of sample solutions
Weighing the best traditional Chinese medicine raw material formula, namely 36g of poria cocos, 27g of cassia twig, 18g of bighead atractylodes rhizome and 18g of liquorice, adding 8 times of water, soaking for 0.5h, extracting for 1h by a reflux device, filtering, combining filtrates, and concentrating the filtrate to 0.5g of crude drug/mL (about 200mL) to obtain a sample solution.
1.2 determination of Dry extract yield
Precisely measuring 10mL of sample solution, placing in an evaporation dish dried to constant weight, evaporating in a water bath, drying in an oven at 105 ℃ to constant weight, taking out, rapidly placing in a dryer for cooling for 30min, and precisely weighing. The dry extract yield was calculated as follows: the yield (%) of dry extract is (dry extract mass/corresponding medicinal material mass) × 100.
1.3 HPLC determination of cinnamic acid and liquiritin content in the extractive solution
1.3.1 cinnamic acid
1.3.1.1 chromatographic conditions
The chromatographic column is AltimaTMC18 chromatographic column (250 mm. times.4.6 mm, 5 μm), mobile phase of 0.05% phosphoric acid aqueous solution-acetonitrile (65:35, V/V), flow rate of 1.0mL min-1The detection wavelength is 285nm, the column temperature is 25 ℃, and the sample injection amount is 10 mu L.
1.3.1.2 preparation of control solutions
And precisely weighing 5mg of a cinnamic acid reference substance, and dissolving the cinnamic acid reference substance in a 10mL volumetric flask by using methanol to obtain a cinnamic acid reference substance solution.
1.3.1.3 Standard Curve preparation
Precisely measuring a proper amount of cinnamic acid reference substance solution, and diluting with 80% methanol to obtain a series of reference substance solutions. 10 mu L of each concentration of control solution is sucked and injected into a liquid chromatograph, the peak area is measured, and a standard curve Y is drawn, wherein the standard curve Y is 72.613X-123.53, r is 0.9994, and the cinnamic acid has good linear relation between 2.505 mu g and 100.20 mu g.
1.3.1.4 Special review
And (3) sucking the reference substance, the test substance and the negative control solution, respectively injecting into a high performance liquid chromatograph, analyzing according to chromatographic conditions, wherein the negative control solution is not absorbed at the corresponding position of the cinnamic acid, which shows that other medicines in the prescription do not interfere with the measurement, and the chromatogram is shown in figure 1.
1.3.2 Glycyrrhiza glycosides
1.3.2.1 chromatographic conditions
The chromatographic column is AltimaTMC18 column (250 mm. times.4.6 mm, 5 μm) with gradient elution with a mobile phase of 0.05% aqueous phosphoric acid (A) -acetonitrile (B) (0min, A: B: 81: 19; 8min, A: B: 81: 19; 35min, A: B: 50; 36min, A: B: 0: 100; 40min, A: B: 81: 19; 45min, A: B: 81:19) at a flow rate of 1.0mL min-1The detection wavelength is 237nm, the column temperature is 25 ℃, and the sample injection amount is 10 mu L.
1.3.2.2 preparation of control solutions
Precisely weighing 5mg of liquiritin reference substance, and dissolving in 10mL volumetric flask with methanol to obtain liquiritin reference substance solution.
1.3.2.3 Standard Curve preparation
Precisely measuring appropriate amount of liquiritin reference substance solution, and diluting with 80% methanol to obtain series of reference substance solutions. 10 μ L of each concentration of control solution is sucked up and injected into a liquid chromatograph, the peak area is measured, and a linear relation between 2.33 μ g and 466.4 μ g of liquiritin is good when liquiritin draws a standard curve Y which is 19.389X +14.279 and r is 1.
1.3.2.4 specialization examination
And (3) sucking the reference substance, the test sample and the negative control solution, respectively injecting into a high performance liquid chromatograph, analyzing according to chromatographic conditions, wherein the negative control solution is not absorbed at the corresponding position of liquiritin, which shows that other medicines in the prescription have no interference to the measurement, and the chromatogram is shown in figure 2.
1.3.3 preparation of test solutions
Sampling 1mL of sample solution, diluting 50% methanol to a constant volume of 5mL, and filtering with a microporous filter membrane to obtain the sample solution.
1.3.4 sample content determination
Injecting the sample solution into a liquid chromatograph, measuring the peak area, and substituting into a standard curve for calculation to obtain the final product.
1.4 selection of extraction times
Extracting for 1 time, 2 times and 3 times according to the method for preparing the sample under the item '1.1', processing three parts in parallel according to the method for testing the sample under the item '1.3.3', and measuring according to the chromatographic condition under the item '1.3', wherein the results are shown in the table 1.
Table 1 examination results of different extraction times (n ═ 3)
Figure BDA0001795899230000051
And (4) conclusion: after the 1 st extraction, more components are still not leached, the transfer rates of the 3 rd extraction of cinnamic acid and liquiritin are both less than 10 percent, the transfer rates are too low, and two extractions are selected from the aspect of energy conservation.
1.5 orthogonal experimental design optimized optimal water extraction process
One-factor experiments showed that extraction twice could result in 58.91% glycyrrhizin and 66.72% cinnamic acid being removed, so extraction twice was chosen. The soaking time (min) of A, the extraction time (h) of B and the water addition amount (times) of C are considered as main factors, and L is selected9(34) Orthogonal table design experiment, the design table of each factor level is shown in table 2, the experimental result is shown in table 3, and the analysis result of variance is shown in table 4.
TABLE 2 Water extraction Process factor levels
Figure BDA0001795899230000061
TABLE 3L9(34) Orthogonal design and experimental results
Figure BDA0001795899230000062
Injecting: the weight coefficient of liquiritin transfer rate was 0.4, the weight coefficient of cinnamic acid transfer rate was 0.4, the weight coefficient of dry extract yield was 0.2, and the composite score (M) ═ liquiritin transfer rate/highest liquiritin transfer rate × (cinnamic acid transfer rate/highest cinnamic acid transfer rate) × 0.4 × 100+ (dry extract yield/highest dry extract yield) × 0.2 × 100.
TABLE 4 Water extraction Process variance analysis Table
Figure BDA0001795899230000071
F0.05(2，2)＝19
The visual analysis result shows that the main and secondary relationship of the three factors is B > C > A, and the optimal process collocation is B3C3A2. The analysis result of comprehensive evaluation variance shows that the extraction time (B) is a significant influence factor in the water extraction process, so B is selected3. The soaking time (A) and the water adding amount (C) of the medicinal materials have no significant influence and can be properly adjusted according to the actual production condition. The preferred process conditions are soaking for 30min, 8 times of water, extracting for 2 times, each time for 1.5 h.
1.6 extraction verification test
Weighing the best traditional Chinese medicine raw material formula, and extracting according to the best water extraction process, wherein the transfer rate of liquiritin is 64.37%, the RSD is 4.97% (n is 3), the transfer rate of cinnamic acid is 62.52%, the RSD is 1.23% (n is 3), the yield of dry paste is 19.76%, and the RSD is 1.19% (n is 3). The preferred water extraction process has high extraction rate and stable process.
Table 5 water extraction process verification test results (n ═ 3)
Figure BDA0001795899230000072
2 extraction and inclusion of volatile components
The transfer rate of cinnamaldehyde in the traditional decoction extracted by an ancient method (simulating the ancient decoction process of a formula, namely six liters of water and three liters of boiled water) is about 10 percent, but the modern preparation comprises concentration and drying operations, and after the two steps of operations, the experiment shows that the cinnamaldehyde component cannot be detected in the concentrated solution and the extract powder. In order to restore the ancient method as much as possible, improve the stability of the cinnamaldehyde and ensure the curative effect of the poria, cassia, rhizoma atractylodis and licorice decoction, the experiment adopts a steam distillation method to extract aromatic water to enrich the volatile effective components in the prescription, and the collected aromatic water is included to prepare the inclusion compound.
2.1 selection of aromatic Water and essential oils
125g of cassia twig decoction pieces are weighed and extracted by a steam distillation method to obtain 0.2mL of volatile oil, and the yield is about 0.25%. The extraction density of the cassia twig volatile oil is close to that of water, the water-oil separation effect is poor, and white floccule which is insoluble in water and oil is easily generated in the extraction process. In the experiment, the aromatic water extractor is used for collecting the aromatic water, and no obvious layering is found in the process, so that the aromatic water is collected to replace the volatile oil.
Weighing the best traditional Chinese medicine raw material prescription decoction pieces, soaking for 30min, decocting with water for 5h, and collecting 1 time of aromatic water for later use.
2.2 preparation of Inclusion Compound
Weighing a certain amount of beta-cyclodextrin, adding into a corresponding amount of aromatic water, keeping the temperature and stirring for a specified time, after stirring, cooling to room temperature, refrigerating for 24h at 4 ℃, filtering, discarding filtrate, filtering to obtain a substance, drying in an oven at 40 ℃ for 4h to obtain a white powdery inclusion compound, and weighing the white powdery inclusion compound. The clathrate yield was calculated as follows.
The yield (%) of the inclusion compound was 100 times the mass of the inclusion compound/(the mass of β -cyclodextrin added + the mass of volatile oil contained in aromatic water added)
2.3 determination of Inclusion Rate of volatile oil
Weighing 0.1g of the inclusion compound in a conical flask, adding 25mL of 70% methanol, performing ultrasonic treatment for 30min, filtering through a 0.22 mu m microporous filter membrane, injecting HLPC, and determining the content of cinnamaldehyde. The inclusion rate is calculated according to the following formula:
inclusion rate (%) of cinnamaldehyde in the clathrate/cinnamaldehyde content in aromatic water × 100
2.4 HPLC determination of Cinnamaldehyde content in the Inclusion Compound
2.4.1 chromatographic conditions
The column was a Welchrom C18 column (150 mm. times.4.6 mm, 5 μm), the mobile phase was acetonitrile-0.05% phosphoric acid (38:62, V/V), the flow rate was 1.0mL min-1The detection wavelength is 290nm, the column temperature is 25 ℃, and the sample injection amount is 10 mu L.
2.4.2 preparation of control solutions
Precisely weighing 452.31mg of cinnamaldehyde reference substance, and dissolving in 10mL volumetric flask with acetonitrile to obtain cinnamaldehyde reference substance solution.
2.4.3 preparation of test solutions
Taking 0.1g of the clathrate prepared by the 2.1, adding 70% methanol, carrying out ultrasonic treatment for 30min, and fixing the volume to 25mL to obtain the product.
2.4.4 preparation of negative control solutions
Weighing the medicinal materials except ramulus Cinnamomi according to the proportion of the prescription, extracting according to the method under item "2.1", clathrating according to the method under item "2.2", and preparing according to the method under item "2.4.3".
2.4.5 Standard Curve preparation
Precisely transferring the above cinnamaldehyde control solution, and diluting with 70% methanol to obtain series of control solutions 4.496, 83.99, 22.48, 89.92, and 224.8 μ g/mL. 10 μ L of each concentration of the control solution was aspirated, injected into a high performance liquid chromatograph, and the peak area was measured, and a linear relationship between 4.496 μ g and 224.8 μ g of cinnamaldehyde was found to be good by plotting a standard curve Y of 104.86X +36.60 and r of 0.9999.
2.4.6 specialization examination
And (3) sucking the reference substance, the test sample and the negative control solution, respectively injecting into a high performance liquid chromatograph, analyzing according to chromatographic conditions, wherein the negative control solution is not absorbed at the corresponding position of the cinnamaldehyde, so that the other medicinal materials in the prescription are not interfered with the measurement, and the chromatogram is shown in figure 3.
2.5 selection of Inclusion temperature
Weighing a certain amount of beta-cyclodextrin, adding a proper amount of water, heating and dissolving in 80 ℃ water bath to prepare a beta-cyclodextrin saturated solution, and slowly cooling to a specified temperature (70 ℃, 50 ℃ and 30 ℃). Precisely measuring aromatic water 100mL, slowly adding the aromatic water solution into the beta-cyclodextrin saturated solution, keeping the temperature and stirring for 1h, cooling to room temperature after stirring is finished, refrigerating for 24h at 4 ℃, filtering, removing the filtrate, and drying the filtered substance in an oven at 40 ℃ for 4h to obtain a white powdery inclusion compound.
TABLE 6 preferred results of inclusion temperature (n ═ 2)
Figure BDA0001795899230000091
As is clear from the results in Table 6, the inclusion temperature of 50 ℃ is the best inclusion effect, so that 40 ℃, 50 ℃ and 60 ℃ are selected as the three levels of the inclusion temperature in the orthogonal test.
2.6 aromatic water: selection of the Cyclodextrin ratio
Weighing a certain amount of beta-cyclodextrin according to a proportion (aromatic water: beta-cyclodextrin: 5:1, 10:1 and 20:1), heating and dissolving in a water bath at 80 ℃ to prepare a beta-cyclodextrin saturated solution, and slowly cooling to 50 ℃. Precisely measuring 50mL of aromatic water, slowly adding the aromatic water solution into the beta-cyclodextrin saturated solution, keeping the temperature and stirring for 1h, cooling to room temperature after stirring is finished, refrigerating for 24h at 4 ℃, filtering, removing the filtrate, and drying the filtered substance in an oven at 40 ℃ for 4h to obtain a white powdery inclusion compound.
As can be seen from the results in table 7, since the inclusion effect was not greatly different between 5:1 and 10:1 for the aromatic water β -cyclodextrin, and was not good enough when 20:1 for the aromatic water β -cyclodextrin, 5:1, 10:1, and 15:1 were selected as three levels of the ratio of aromatic water to cyclodextrin in the orthogonal test.
Table 7 ratio of aromatic water to beta-cyclodextrin preferred results (n ═ 2)
Figure BDA0001795899230000092
2.7 selection of Inclusion method
The method comprises the following steps: slowly adding the aromatic water solution into the beta-cyclodextrin saturated solution; the method 2 comprises the following steps: adding a certain amount of beta-cyclodextrin into aromatic water. As is clear from table 8, in the inclusion compound of method 2, both the cinnamaldehyde transfer rate and the inclusion yield were higher than those of method 1, and therefore method 2 was selected as the inclusion method to be subsequently studied.
Table 8 inclusion method preferred results (n ═ 4)
Figure BDA0001795899230000101
2.8 orthogonal experiment design optimization optimal inclusion process
Preparing aromatic water A, cyclodextrin (mL: g), inclusion temperature B (DEG C), and inclusion CThe resultant time (h) is the main factor to be examined, and L is selected9(34) Orthogonal table design test, the design table of each factor level is shown in table 9, the test result is shown in table 10, the analysis result of variance is shown in table 11
TABLE 9 Inclusion Process factors and levels
Figure BDA0001795899230000102
TABLE 10L9(34) Orthogonal design and experimental results
Figure BDA0001795899230000103
Figure BDA0001795899230000111
Injecting: the weight coefficient of cinnamaldehyde inclusion rate was 0.6, the weight coefficient of clathrate yield was 0.4, and the composite score (M) ═ cinnamaldehyde inclusion rate/highest cinnamaldehyde inclusion rate) × 0.4 × 100+ (clathrate yield/highest clathrate yield) × 0.4 × 100.
TABLE 11 analysis of variance of inclusion test
Figure BDA0001795899230000112
F0.05(2，2)＝19
The visual analysis result shows the primary and secondary relationship A of three factors>B>C, the best process collocation is A1B1C3. Comprehensively evaluating the result of the anova, in the extraction process, the aromatic water, the cyclodextrin (A), the inclusion temperature (B) and the inclusion time (C) have no significant factors, and from the viewpoint of reducing the dosage of the medicament, the A is selected2The inclusion temperature (B) is selected according to the visual analysis result1From the viewpoint of energy saving, C is selected1. Therefore, the optimal inclusion process is A2B1C1Namely, aromatic water:the cyclodextrin ratio is 10:1, and inclusion is carried out at 40 ℃ for 1 h.
2.9 Inclusion verification test
The aromatic water is subjected to inclusion according to an optimal process, the inclusion rate of cinnamaldehyde is 72.06% (RSD is 2.13%, n is 3), and the inclusion yield is 83.73% (RSD is 0.84%, n is 3). Under the condition, the inclusion rate and the inclusion compound yield are relatively stable, which indicates that the process is reasonable and feasible.
2.10 inclusion Compound thin layer chromatography detection
To verify whether the aromatic water is included in the beta-cyclodextrin, the following thin layer chromatography was used. Dissolving aromatic water in petroleum ether to obtain a sample a; adding petroleum ether into the inclusion compound, shaking and standing to obtain a sample b; adding 70% methanol into the inclusion compound, performing ultrasonic treatment, and removing the inclusion compound to obtain a sample c; adding petroleum ether into beta-cyclodextrin, shaking and standing to obtain a test sample d; and (3) physically mixing the volatile oil and the beta-cyclodextrin, uniformly mixing, and adding petroleum ether to obtain a sample e. According to thin layer chromatography of the first part of the 2015 version of the Chinese pharmacopoeia, taking 2 mu L of each of the 5 test sample solutions, respectively dropping the solution on the same silica gel G thin layer plate, developing with petroleum ether (60-90 ℃) and ethyl acetate (17:3) as developing agents, taking out, drying in the air, and spraying dinitrophenylhydrazine ethanol test solution, as shown in figure 4, wherein the test samples a, c and e show yellow cassia twig volatile oil spots at the same positions, and b and d have no corresponding spots. The result shows that the property of the inclusion compound is not changed in the inclusion process, and the cassia twig volatile oil enters beta-cyclodextrin molecules to form beta-cyclodextrin inclusion compounds, non-surface adsorption combination and other modes.
Our research shows that under the preferable inclusion process, the inclusion rate and the inclusion yield are stable, and the process is reasonable and feasible.
The preparation method of the invention improves the traditional inclusion process, namely directly adding the beta-cyclodextrin into the aromatic water for stirring and inclusion, and the inclusion process operation is not reported. The new volatile oil inclusion mode obtained in the patent has the advantages of simple and easy process operation, high volatile component transfer rate and inclusion rate, stability, retention of effective components in the traditional decoction and clinical consistency.
The new volatile oil inclusion mode obtained in the patent not only retains the effective components in the traditional decoction, has clinical consistency with the decoction, but also has the characteristics of omitting the volatile oil purification operation, being simple and easy in inclusion process, high in volatile component transfer rate and inclusion rate, good in stability and the like.
The preparation method established by the invention can be used for collecting the inclusion of aromatic water when the Chinese herbal medicine compound is decocted, so that the prepared Chinese herbal medicine preparation is closer to the real state of clinical administration of classical formulas.
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
The features mentioned above with reference to the invention, or the features mentioned with reference to the embodiments, can be combined arbitrarily. All the features disclosed in this specification may be combined in any combination and each feature disclosed in this specification may be replaced by alternative features serving the same, equivalent or similar purpose. Thus, unless expressly stated otherwise, the features disclosed are merely generic examples of equivalent or similar features.
Example 1
Taking 12 parts of poria cocos, 9 parts of cassia twig, 9 parts of bighead atractylodes rhizome and 6 parts of liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Glycyrrhrizae radix, adding 8 times of water, soaking for 30min, extracting for 2 times, decocting with water for 2.5 hr for the first time, collecting 1 time of aromatic water, and decocting with water for 1.5 hr for the second time. Combining the water extract, concentrating to relative density of 1.13(60 deg.C);
step two: centrifuging the concentrated water extract at 5000rpm to obtain supernatant, and concentrating to relative density of 1.20(60 deg.C);
step three: drying the concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder;
step four: weighing 1/10 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 50 deg.C for 2 hr, cooling to room temperature after stirring, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate and the extract powder, adding adjuvant, and making into granule.
Table 12 inclusion method preferred results (n ═ 4)
Figure BDA0001795899230000131
P <0.01 compared to method 1; p <0.05 compared to method 1
According to the method of patent document 2, aromatic water is slowly added into a beta-cyclodextrin saturated solution, the experimental result is shown in method 1 in table 12, the transfer rate of the obtained inclusion compound cinnamaldehyde is 55.88%, and the inclusion yield is 77.85%; the invention omits the steps of preparing a saturated solution by beta-cyclodextrin and slowly adding aromatic water into the saturated solution of beta-cyclodextrin, improves the saturated solution, directly adds a certain amount of beta-cyclodextrin into the aromatic water for stirring, and the experimental result shows that the method 2 in the table 12 can obtain the inclusion compound with the cinnamaldehyde transfer rate of 75.12 percent and the inclusion yield of 85.89 percent. Statistical analysis is carried out on the beta-cyclodextrin inclusion compound through SPSS21.0, and by adopting the improved inclusion process, a certain amount of beta-cyclodextrin is directly added into aromatic water for stirring, so that the yield of volatile components and the inclusion yield of the prepared inclusion compound can be obviously improved. Compared with the method in patent document 2, the method of the invention has the advantages of time consumption twice shortened and simpler operation.
Example 2
60 parts of poria cocos, 45 parts of cassia twig, 45 parts of honey bran-fried bighead atractylodes rhizome and 30 parts of liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, rhizoma Atractylodis Macrocephalae processed with bran and radix Glycyrrhizae, soaking in 6 times of water for 30min, extracting for 3 times, decocting in water for 3 hr, collecting 0.5 times of aromatic water, and decocting in water for 2 hr. Combining the water extract, concentrating to relative density of 1.09(60 deg.C);
step two: adding 1.5 times of ethanol into the concentrated water extract, precipitating with ethanol to obtain an ethanol precipitation solution, and concentrating to relative density of 1.17(70 deg.C);
step three: drying the ethanol precipitation concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder;
step four: weighing 1/5 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 60 deg.C for 1 hr, cooling to room temperature, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 50 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the ethanol precipitation concentrated solution and clathrate, adding adjuvants, canning, and sterilizing to obtain oral liquid.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 67.12%, and the inclusion yield is 81.69%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 49.84 percent, and the inclusion yield is 72.32 percent.
Example 3
120 parts of poria cocos, 90 parts of cassia twig, 90 parts of bighead atractylodes rhizome and 60 parts of honey-fried liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Mel radix Glycyrrhizae Preparata, soaking in 8 times of water for 30min, extracting for 2 times, decocting with water for 1.5 hr for the first time, collecting 1.5 times of aromatic water, and decocting with water for 1.5 hr for the second time. Combining the water extract, concentrating to relative density of 1.09(80 deg.C);
step two: adding 1 time of ethanol into the water extraction concentrated solution for alcohol precipitation to obtain an alcohol precipitation solution, and concentrating until the relative density is 1.22(80 ℃);
step three: drying the ethanol precipitation concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder;
step four: weighing 1/15 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 40 deg.C for 3 hr, cooling to room temperature, and refrigerating at-4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate and the extract powder, adding adjuvants, and tabletting to obtain tablet.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 75.89%, and the inclusion yield is 91.68%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 57.92%, and the inclusion yield is 79.95%.
Example 4
16 parts of poria cocos, 12 parts of cassia twig, 12 parts of bighead atractylodes rhizome and 9 parts of liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Glycyrrhrizae radix, adding 6 times of water, soaking for 60min, extracting for 3 times, decocting with water for 1.5 hr each time, collecting 1.5 times of aromatic water, and decocting with water for 1.5 hr the second time and the third time. Combining the water extract, concentrating to relative density of 1.14(60 deg.C);
step two: centrifuging the concentrated water extract at 5000rpm to obtain supernatant, and concentrating to relative density of 1.24(60 deg.C);
step three: drying the concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder;
step four: weighing beta-cyclodextrin with 1/10 aromatic water amount, adding into the collected aromatic water, stirring at 40 deg.C for 1 hr, cooling to room temperature, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate with the extract powder, adding adjuvant, and making into pill.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 73.96%, and the inclusion yield is 82.17%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 54.35 percent, and the inclusion yield is 75.47 percent.
Example 5
80 parts of poria cocos, 60 parts of cassia twig, 60 parts of bighead atractylodes rhizome and 40 parts of liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Glycyrrhrizae radix, adding 8 times of water, soaking for 120min, extracting for 2 times, decocting with water for 2 hr for the first time, collecting 2 times of aromatic water, and decocting with water for 2 hr for the second time. Combining the water extract, concentrating to relative density of 1.15(70 deg.C);
step two: centrifuging the concentrated water extract at 15000rpm to obtain supernatant, and concentrating to relative density of 1.17(70 deg.C);
step three: drying the centrifugal concentrated solution in a vacuum drying oven at 50 ℃ to obtain dry extract, and crushing to obtain extract powder;
step four: weighing 1/20 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 40 deg.C for 3 hr, cooling to room temperature after stirring, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate and the extract powder, adding adjuvant, and making into granule.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 75.44%, and the inclusion yield is 84.63%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 56.86%, and the inclusion yield is 78.98%.
Example 6
24 parts of poria cocos, 18 parts of cassia twig, 18 parts of bighead atractylodes rhizome and 12 parts of liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Glycyrrhrizae radix, adding 10 times of water, soaking for 90min, extracting for 2 times, decocting with water for 5 hr for the first time, collecting 1.5 times of aromatic water, and decocting with water for 5 hr for the second time. Combining the water extract, concentrating to relative density of 1.15(60 deg.C);
step two: adding 3 times of ethanol into the water extraction concentrated solution for alcohol precipitation to obtain an alcohol precipitation solution, and concentrating until the relative density is 1.25(60 ℃);
step three: drying the ethanol precipitation concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder.
Step four: weighing 1/15 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 60 deg.C for 1 hr, cooling to room temperature, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate with the extract powder, adding adjuvant, and making into pill.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 66.62%, and the inclusion yield is 80.90%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 46.83 percent, and the inclusion yield is 70.96 percent.
Example 7
120 parts of poria cocos, 90 parts of cassia twig, 90 parts of bighead atractylodes rhizome and 60 parts of liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Glycyrrhrizae radix, adding 6 times of water, soaking for 30min, extracting for 3 times, decocting with water for the first time for 2.5 hr, collecting 1.5 times of aromatic water, and decocting with water for the second and third times for 2.5 hr. Combining the water extract, concentrating to relative density of 1.05(70 deg.C);
step two: adding 1 time of ethanol into the water extraction concentrated solution for alcohol precipitation to obtain an alcohol precipitation solution, and concentrating until the relative density is 1.15(70 ℃);
step three: drying the ethanol precipitation concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder.
Step four: weighing 1/8 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 60 deg.C for 3 hr, cooling to room temperature, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate and the extract powder, adding adjuvant, granulating, drying, and making into capsule.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 68.39%, and the inclusion yield is 82.57%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 48.54%, and the inclusion yield is 74.73%.
Example 8
The preparation method comprises the following steps of taking 48 parts of poria cocos, 36 parts of cassia twig, 36 parts of bighead atractylodes rhizome and 24 parts of honey-fried liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Mel radix Glycyrrhizae Preparata, soaking in 12 times of water for 120min, decocting with water for 4.5 hr, and collecting 0.5 times of aromatic water. Concentrating the water extract to relative density of 1.13(70 deg.C);
step two: centrifuging the concentrated water extract at 10000rpm to obtain supernatant, and concentrating to relative density of 1.30(70 deg.C);
step three: drying the concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder;
step four: weighing 1/10 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 50 deg.C for 3 hr, cooling to room temperature, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six, mixing the inclusion compound and the extract powder, adding auxiliary materials and preparing granules.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 74.98%, and the inclusion yield is 83.12%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 56.47%, and the inclusion yield is 78.56%.
Example 9
60 parts of poria cocos, 45 parts of cassia twig, 45 parts of bighead atractylodes rhizome and 30 parts of liquorice.
The method comprises the following steps: mixing Poria, ramulus Cinnamomi, Atractylodis rhizoma, and Glycyrrhrizae radix, adding 10 times of water, soaking for 30min, extracting for 2 times, decocting with water for the first time for 1.5 hr, collecting 1 time of aromatic water, and decocting with water for the second time for 1.5 hr. Combining the water extract, concentrating to relative density of 1.08(70 deg.C);
step two: adding 0.5 times of ethanol into the concentrated water extract, precipitating with ethanol to obtain an ethanol precipitation solution, and concentrating to relative density of 1.18(70 deg.C);
step three: drying the ethanol precipitation concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder;
step four: weighing 1/20 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 50 deg.C for 1 hr, cooling to room temperature, and refrigerating at 4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate with the extract powder, adding adjuvants, and tabletting to obtain tablet.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 69.77 percent, and the inclusion yield is 83.25 percent; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution for stirring, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 49.69%, and the inclusion yield is 74.41%.
Example 10
Taking 27 parts of astragalus, 27 parts of Chinese herbaceous peony, 27 parts of cassia twig, 54 parts of ginger and 36 parts of Chinese date.
The method comprises the following steps: mixing radix astragali, radix Paeoniae, ramulus Cinnamomi, rhizoma Zingiberis recens, and fructus Jujubae, adding 10 times of water, soaking for 30min, extracting for 2 times, decocting with water for the first time for 1.5 hr, collecting 1 time of aromatic water, and decocting with water for the second time for 1.5 hr. Combining the water extract, concentrating to relative density of 1.08(70 deg.C);
step two: adding 0.5 times of ethanol into the concentrated water extract, precipitating with ethanol to obtain an ethanol precipitation solution, and concentrating to relative density of 1.20(70 deg.C);
step three: drying the ethanol precipitation concentrated solution in a vacuum drying oven at 60 deg.C to obtain dry extract, and pulverizing to obtain extract powder;
step four: weighing 1/10 beta-cyclodextrin with aromatic water amount, adding into the collected aromatic water, stirring at 40 deg.C for 1 hr, cooling to room temperature, and refrigerating at-4 deg.C for 24 hr;
step five: filtering, discarding the filtrate, drying the filtrate in an oven at 40 deg.C for 4 hr, and grinding to obtain white powdery clathrate;
step six: mixing the clathrate and the extract powder, adding adjuvant, and making into granule.
According to the embodiment, a certain amount of beta-cyclodextrin is directly added into aromatic water to be stirred, the transfer rate of cinnamaldehyde in the obtained inclusion compound is 65.37%, and the inclusion yield is 80.05%; if the beta-cyclodextrin is prepared into a saturated solution, then the aromatic water is slowly added into the beta-cyclodextrin saturated solution to be stirred, the transfer rate of the cinnamaldehyde in the obtained inclusion compound is 40.24 percent, and the inclusion yield is 63.61 percent.
In the above embodiment, the improved inclusion process of the present invention has the following advantages compared with the conventional process: 1. for the traditional Chinese medicine components which can not collect the volatile oil, the aromatic water can be directly extracted, the volatile oil does not need to be purified continuously through complicated purification operation, the oil-water separation is not needed, and the operation is more convenient; 2. the inclusion process is easy to operate, has high repeatability, aromatic water does not need to be concentrated, cyclodextrin is directly added, the time consumption is shorter, the inclusion temperature is lower, and the cyclodextrin dosage is less; 3. the transfer rate of volatile components and the inclusion yield of the obtained inclusion compound are higher; 4. the water-soluble components and volatile components in the prescription are reserved, and the actual state of clinical administration of the traditional prescription is more similar.
The preparation method established by the invention can be used for inclusion of aromatic water collected during decoction of the Chinese herbal medicine compound, so that the prepared Chinese herbal medicine preparation is closer to Chinese herbal medicine decoction used clinically.
The various aspects of the invention are addressed above. It should be understood, however, that equivalent changes and modifications may be made thereto by those skilled in the art without departing from the spirit of the present invention, and that such changes and modifications are intended to be covered by the appended claims.

Claims (5)

1. The preparation method of the cassia twig-containing traditional Chinese medicine composition is characterized in that the traditional Chinese medicine composition is prepared from the following traditional Chinese medicine raw materials in parts by weight: 12-120 parts of poria cocos, 9-90 parts of cassia twig, 9-90 parts of bighead atractylodes rhizome or honey bran-fried bighead atractylodes rhizome, and 6-60 parts of liquorice or honey-fried liquorice; or the traditional Chinese medicine composition is prepared from the following traditional Chinese medicine raw materials in parts by weight: 9-90 parts of astragalus membranaceus, 9-90 parts of Chinese herbaceous peony, 9-90 parts of cassia twig, 18-180 parts of ginger and 12-120 parts of Chinese date; the preparation method comprises the following steps:
firstly, weighing traditional Chinese medicine raw materials according to a prescription, adding 6-12 times of water to soak for 30-120 min, extracting for 1-3 times, wherein the first time of steam distillation extraction is performed for 1-5 h, and collecting 0.5-2 times of aromatic water for later use; combining the water extract, and concentrating under reduced pressure at 60-80 ℃ until the relative density is 1.05-1.15 at the corresponding temperature;
filtering the water extraction concentrated solution or centrifuging at a high speed of 5000-15000 rpm, or adding 0.5-3 times of ethanol for alcohol precipitation, and concentrating the extracting solution or supernatant of the alcohol precipitation solution at 50-70 ℃ under reduced pressure until the relative density is 1.15-1.30;
drying the ethanol precipitation solution or the centrifugal concentrated solution after the reduced pressure concentration in a vacuum drying oven at 50-70 ℃ to obtain dry extract, and crushing to obtain extract powder;
weighing beta-cyclodextrin with 1/5-1/20 aromatic water amount, adding the beta-cyclodextrin into the collected aromatic water, keeping the temperature at 40-60 ℃, stirring for 1-3 h, cooling to room temperature after stirring, and refrigerating for 24h at-4 ℃; filtering, discarding the filtrate, drying the filtered substance in an oven at 40-60 ℃ for 4h, grinding to obtain a white powdery inclusion compound, and mixing with the extract powder.
2. The preparation method of the cassia twig-containing traditional Chinese medicine composition as claimed in claim 1, wherein the traditional Chinese medicine raw materials are in parts by weight: 36 parts of poria cocos, 27 parts of cassia twig, 27 parts of bighead atractylodes rhizome or honey bran-fried bighead atractylodes rhizome, and 18 parts of liquorice or honey-fried liquorice.
3. The preparation method of the cassia twig-containing traditional Chinese medicine composition as claimed in claim 1, wherein the traditional Chinese medicine raw materials are in parts by weight: 27 parts of astragalus, 27 parts of Chinese herbaceous peony, 27 parts of cassia twig, 54 parts of ginger and 36 parts of Chinese date.
4. The method for preparing a cassia twig-containing traditional Chinese medicine composition according to claim 1, wherein in the first step, aromatic water with the amount 1-1.5 times of the amount of the medicinal materials is collected.
5. The method for preparing the cassia twig-containing traditional Chinese medicine composition as claimed in claim 1, wherein in the fourth step, 1/10-1/15 amount of aromatic water of beta-cyclodextrin is weighed.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1616020A (en) * 2004-09-15 2005-05-18 北京博尔达生物技术开发有限公司 Xingnaojing powder injection and preparing method
CN105982984A (en) * 2015-02-28 2016-10-05 九芝堂股份有限公司 Pharmaceutical composition for treating liver diseases and preparing method thereof

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100469380C (en) * 2004-07-28 2009-03-18 昆明市中医医院 Stomach motility promoting medicine for treating stomach and intestine function failure and its preparation

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1616020A (en) * 2004-09-15 2005-05-18 北京博尔达生物技术开发有限公司 Xingnaojing powder injection and preparing method
CN105982984A (en) * 2015-02-28 2016-10-05 九芝堂股份有限公司 Pharmaceutical composition for treating liver diseases and preparing method thereof

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
"环糊精包结疲王颗粒中挥发油的实验研究";涂禾等;《四川中医》;20141015;第32卷(第10期);第57页左栏第1、3段、右栏第1-2段以及第58页左栏第4段至右栏第5段 *
一种制备川芎、三棱挥发油/β-环糊精包合物的新工艺研究;傅应华;《中成药》;20071020(第10期);第1440-1442页 *

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