CN113509530B - A Chinese medicinal compound preparation for treating asthma, and its preparation method and quality control method - Google Patents

A Chinese medicinal compound preparation for treating asthma, and its preparation method and quality control method Download PDF

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CN113509530B
CN113509530B CN202110544468.7A CN202110544468A CN113509530B CN 113509530 B CN113509530 B CN 113509530B CN 202110544468 A CN202110544468 A CN 202110544468A CN 113509530 B CN113509530 B CN 113509530B
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chinese medicine
traditional chinese
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asthma
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张珂
孙仁宽
李国玉
刘丹妮
范乐之
卢立娜
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Shenzhen Honghui Biomedicine Co ltd
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Abstract

The invention relates to a Chinese medicinal compound preparation for treating asthma, a preparation process and a quality control method thereof, wherein the formula is prepared from the following Chinese medicinal raw materials: the invention adopts different methods for extraction, prepares capsule preparation, reasonably combines and optimally prepares the capsule preparation, makes the functions of the capsule preparation complement each other, eliminates phlegm and stops cough, ventilates and relieves asthma, safely and effectively treats asthma.

Description

A Chinese medicinal compound preparation for treating asthma, and its preparation method and quality control method
Technical Field
The invention relates to the technical field of traditional Chinese medicine pharmacy, in particular to a traditional Chinese medicine compound preparation for treating asthma, a preparation process and a quality control method thereof.
Background
Bronchial asthma, called asthma for short, is one of the most common chronic non-infectious diseases in the world and has become a global social health problem. According to incomplete statistics, the current asthma incidence rate in the world is 5-16%, the incidence rate of children aged 6-7 years is 11.6%, the incidence rate of asthma in developed countries such as Europe and America is 15-20%, and the incidence rate of asthma in China is 2-4%. Repeated asthma attacks can easily lead to miswork and misconception, and can bring heavy economic and social burdens to patients, families and society. About 250000 patients die of asthma worldwide each year. Asthma is a disease of a complex nature, the pathogenesis of the asthma is increasingly complex, and the pathogenesis of the asthma is related to multiple factors such as heredity, immunity, nerves and spirit.
The traditional Chinese medicine science reports the occurrence of asthma as phlegm staying in the lung, and phlegm is caused by phlegm accumulation due to the invasion of exogenous pathogenic factors, improper diet, emotional stimulation, weakness, overstrain and the like, so that the phlegm is blocked in the airway and the lung qi is disturbed in the functions of dispersing and descending. The disease refers to the lung, spleen and kidney, and is generally caused by excess pathogenic factors and deficiency of healthy qi, and the symptoms are treated urgently in the treatment process, and the lung, spleen and kidney are regulated after the symptoms are relieved, as in the cloud of Zhu Danxi, the disease is mainly caused by strengthening healthy qi, and the disease is caused by attacking pathogenic factors as quickly. The traditional Chinese medicine has good clinical curative effect on asthma, and in recent years, Chinese medicine and pharmacologists have conducted intensive research on the action mechanism of the traditional Chinese medicine for treating asthma. The traditional Chinese medicine has obvious treatment effect and small side effect, and has important research significance.
Disclosure of Invention
The invention aims to provide a traditional Chinese medicine compound preparation for treating asthma and a preparation process thereof, and the compound preparation has certain effects of relieving cough and asthma and moistening lung and has good curative effect on asthma.
The invention also aims to provide a quality control method of the traditional Chinese medicine compound preparation.
The technical scheme is as follows:
the traditional Chinese medicine compound preparation for treating asthma is prepared from the following traditional Chinese medicine raw materials in parts by weight: 100-240g of Sijiqing, 80-160g of radix glehniae, 80-160g of salvia miltiorrhiza, 40-80g of liquorice, 40-80g of sea buckthorn, 40-80g of bitter apricot seed and 10-40g of tabasheer. The optimal ratio is 6:4:4:2:2:2:1, namely: 240g of Chinese holly leaf, 160g of coastal glehnia root, 160g of danshen root, 80g of liquoric root, 80g of sea-buckthorn, 80g of bitter apricot seed and 40g of tabasheer, wherein the total weight is 840 g.
One of the preparation processes of the traditional Chinese medicine compound preparation for treating asthma comprises the steps of cleaning and drying raw material medicines, crushing part of salvia miltiorrhiza and tabasheer, sieving the crushed parts by a 100-mesh sieve to obtain fine powder for later use, crushing the rest medicinal materials into tablets, putting the tablets into a copper vessel, adding 80% ethanol, repeatedly decocting for 2 times for 1 hour each time, wherein the volume of a first solvent is 10 times that of a second solvent is 8 times that of the first solvent, combining decoctions, and standing for 24 hours. Filtration and concentration of the filtrate to a relative density of 1.15-1.27(60 ℃). Adding the above fine powder, mixing, drying, grinding into fine powder, and encapsulating in No. 0 capsule to obtain the final product.
The second preparation process of the traditional Chinese medicine compound preparation for treating asthma comprises the following steps of preparing the raw medicinal materials according to the mass ratio: 240g of Chinese holly leaf, 160g of coastal glehnia root, 160g of danshen root, 80g of liquoric root, 80g of sea-buckthorn, 80g of bitter apricot seed and 40g of tabasheer, wherein the total mass is 840 g. The preparation method comprises the following steps: cleaning the medicinal materials, oven drying, extracting Saviae Miltiorrhizae radix with 10 times of water twice, mixing extractive solutions, adding ethanol to make alcohol concentration 40%, standing for 24 hr, filtering to remove precipitate, recovering solvent under reduced pressure, and vacuum drying or freeze drying to obtain loose powder of Saviae Miltiorrhizae radix total phenolic acid. Crushing the rest materials into pieces, placing into a copper vessel, adding 80% ethanol, repeatedly decocting for 2 times (1 hr each time), with the volume of the first solvent being 10 times and the volume of the second solvent being 8 times, mixing decoctions, and standing for 24 hr. Filtration and concentration of the filtrate to a relative density of 1.15-1.27(60 ℃). Adding the above fine powder, mixing, drying, grinding into fine powder, and encapsulating in No. 0 capsule to obtain the final product.
The third preparation process of the traditional Chinese medicine compound preparation for treating asthma comprises the following steps of preparing raw medicinal materials according to the mass ratio in the compound: 240g of Chinese holly leaf, 160g of coastal glehnia root, 160g of danshen root, 80g of liquoric root, 80g of sea-buckthorn, 80g of bitter apricot seed and 40g of tabasheer, wherein the total mass is 840 g. The preparation method comprises the following steps: cleaning all the medicinal materials, drying, crushing into pieces, putting into a copper vessel, adding 80% ethanol, repeatedly decocting for 2 times, 1 hr each time, with the volume of the first solvent being 10 times that of the second solvent being 8 times that of the first solvent, mixing decoctions, and standing for 24 hr. Filtering, recovering solvent under reduced pressure, vacuum drying or freeze drying, making into fine powder, and packaging into No. 0 capsule.
The treatment effect of the traditional Chinese medicine compound preparation for treating asthma is verified by an ovalbumin-induced mouse asthma model. The specific contents are as follows: ovalbumin is used for establishing a mouse asthma model, the medicine is prepared by the preparation method, and the medicine is administered to a mouse for 14 days. Pathological states of mouse trachea and lung tissues were examined by hematoxylin-eosin staining (HE staining), Masson staining (Masson).
The detection result shows that: the wall of the lung vessel and the bronchial wall of the mouse of the asthma model are thickened, and epithelial cells of the tracheal mucosa are proliferated. The bronchial monolayer columnar epithelial cells of the asthma model mouse fall off, and the monolayer columnar epithelial cells are converted into high-layer columnar epithelial cells. The asthma model has disordered arrangement of lung tissue cells, cell degeneration, obvious necrosis of cell nucleus and infiltration of inflammatory cells. The asthma mice treated by the traditional Chinese medicine have changed lung inflammation infiltration conditions, and the arrangement of lung cells presents a normal state. The trachea epithelial cells reduce the withering and necrosis, and the state tends to be normalized.
The invention further provides a content determination method of the traditional Chinese medicine compound preparation, which comprises the following steps:
(1) preparation of control solutions: liquiritin, echinocandin, amygdalin, salvianolic acid B, psoralen, licochalcone B, rhododendron and quercitrin are used as standard reference substances, methanol is used as a solvent to prepare reference substance solutions with different concentrations, wherein the concentrations of the solutions are liquiritin 0.165mg/mL, echinocandin 0.08mg/mL, amygdalin 0.09mg/mL, salvianolic acid B0.085mg/mL, psoralen 0.06mg/mL, licochalcone B0.08 mg/mL, rhododendron 0.03mg/mL and quercitrin 0.10mg/mL respectively, and the reference substance solutions are obtained after the solutions pass through a 0.22 mu m filter membrane;
(2) preparation of a test solution: adding methanol into the compound Chinese medicinal preparation, stirring, centrifuging to obtain supernatant, and filtering with 0.22 μm filter membrane to obtain test solution;
(3) the detection method comprises the following steps: respectively injecting the reference solution and the test solution into an ultra-high performance liquid chromatograph to obtain a chromatogram, and calculating the content of liquiritin, echinacolone, amygdalin, salvianolic acid B, psoralen, licochalcone B, farrerol and quercitrin in the Chinese medicinal compound preparation according to the chromatogram;
wherein the chromatographic conditions of the ultra-high performance liquid chromatograph are as follows:
chromatographic column ACQUITY UPLC BEH C18 (2.1X 100mm, 1.7 μm),
the mobile phase A is acetonitrile, the mobile phase B is 0.1 percent of phosphoric acid water solution for gradient elution,
flow rate of 0.200 mL/min-1，
The detection wavelength is 254nm,
column temperature 30 deg.C
Gradient elution conditions:
Figure BDA0003073011760000031
Figure BDA0003073011760000041
the fingerprint quality control standard method of the traditional Chinese medicine compound preparation for treating asthma comprises the following steps:
(1) preparation of control solutions: precisely weighing 3.30mg of liquiritin, 1.60mg of echinocandin, 1.80mg of amygdalin, 1.70mg of salvianolic acid, 1.20mg of psoralen, 1.60mg of licochalcone, 0.60mg of rhododendron and 2.00mg of quercitrin as reference substances, and sequentially adding 1mL of methanol for ultrasonic dissolution. Respectively sucking 50 μ L of each reference solution, adding methanol to dilute to 1mL to obtain each reference solution with liquiritin 0.165mg/mL, licochalcone 0.08mg/mL, amygdalin 0.09mg/mL, salvianolic acid B0.085mg/mL, psoralen 0.06mg/mL, licochalcone B0.08 mg/mL, rhododendrin 0.03mg/mL, quercetin 0.10mg/mL, and filtering with 0.22 μm filter membrane to obtain each reference solution.
(2) Preparation of a test solution: precisely weighing 1g of each of the Chinese medicinal compound preparations prepared by different preparation methods, respectively placing into a triangular flask with a plug, adding 25mL of chromatographic methanol, weighing, ultrasonically dissolving for 30min, and complementing weight loss after placing at room temperature. Shaking up, sucking 1mL, centrifuging, taking supernatant, and filtering with 0.22 μm filter membrane to obtain the final product.
(3) The detection method comprises the following steps: measuring by ultra high performance liquid chromatography with 1 μ L of control solution and 5 μ L of test solution. The chromatographic conditions were that the column was ACQUITY UPLC BEH C18 (2.1X 100mm, 1.7 μm), and the gradient elution was carried out with mobile phase A of acetonitrile and mobile phase B of 0.1% phosphoric acid aqueous solution at a flow rate of 0.200 mL/min-1The detection wavelength is 254nm, and the column temperature is 30 ℃. Obtaining the ultra-high performance liquid chromatogram of the Chinese herbal medicine compound preparation.
The gradient elution method is as follows:
Figure BDA0003073011760000042
(5) comparing the chromatogram of each reference solution with the chromatogram of the test solution, and detecting the test solution by fingerprint method to monitor the quality of the compound preparation.
The invention adopts ultra-high performance liquid chromatography to construct the fingerprint of the traditional Chinese medicine compound, and the quality of the traditional Chinese medicine compound preparation is monitored by utilizing the fingerprint characteristics. The invention takes the main effective components in the Chinese herbal compound preparation as the reference substance, which represents most of the pharmacological activity in the Chinese herbal compound preparation, thereby detecting the main chemical components in the Chinese herbal compound preparation and being beneficial to controlling the quality of the Chinese herbal compound preparation. The method establishes the technical standard of the fingerprint of the traditional Chinese medicine compound preparation, effectively and comprehensively monitors the quality of the traditional Chinese medicine compound preparation through the characteristic that the fingerprint and each reference chromatogram share a peak, ensures the stability of the traditional Chinese medicine compound preparation, and ensures the controllability of the quality. The method not only controls the quality of the traditional Chinese medicine compound preparation, but also has simple operation, short time, small sample amount and certain economic value and practical significance.
Drawings
FIG. 1: the mouse trachea HE staining is shown in the figure, wherein the normal group A, the model group B, the low traditional Chinese medicine dose (200mg/kg) in the group C, the medium traditional Chinese medicine dose (400mg/kg) in the group D, the high traditional Chinese medicine dose (800mg/kg) in the group E and the positive group F (dexamethasone).
FIG. 2: HE staining of lung tissues of mice is shown in the figure, wherein the lung tissues of the mice are subjected to HE staining, and the lung tissues of the mice are subjected to normal group A, model group B, low traditional Chinese medicine dose (200mg/kg) of traditional Chinese medicine C, medium traditional Chinese medicine dose (400mg/kg) of traditional Chinese medicine D, high traditional Chinese medicine dose (800mg/kg) of traditional Chinese medicine E and positive group F (dexamethasone).
FIG. 3: the lung tissues of mice are Masson stained, and in the figure, a normal group A, a model group B, a traditional Chinese medicine low dose (200mg/kg) in a traditional Chinese medicine C, a traditional Chinese medicine medium dose (400mg/kg) in a traditional Chinese medicine D, a traditional Chinese medicine high dose (800mg/kg) in an E and a positive group F (dexamethasone) are shown.
FIG. 4: a fingerprint of Chinese medicinal compound preparation for treating asthma is prepared from amygdalin, liquiritin, quercitrin, licochalcone B, psoralen, salvianolic acid B, echinocandin, and rhododendrin, wherein the peak numbers 1, 2, 3, 4, 5, 6, 7, and 8 are sequentially indicated in the figure.
FIG. 5: a fingerprint of Chinese medicinal compound preparation for treating asthma (preparation method II) has peak numbers of 1, 2, 3, 4, 5, 6, 7, and 8 sequentially indicated as amygdalin, liquiritin, quercitrin, licochalcone B, psoralen, salvianolic acid B, echinocandin, and azaleatin.
FIG. 6: a fingerprint of Chinese medicinal compound preparation for treating asthma is prepared from amygdalin, liquiritin, quercitrin, licochalcone B, psoralen, salvianolic acid B, echinocandin, and rhododendrin, wherein the peak numbers 1, 2, 3, 4, 5, 6, 7, and 8 are sequentially indicated.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the invention thereto.
Example 1:
240g of Chinese holly leaf, 160g of coastal glehnia root, 8g of total salvianolic acid, 80g of liquorice, 80g of sea-buckthorn, 80g of bitter apricot seed and 40g of concretio silicea bambusae, wherein the total weight is 688 g.
Example 2:
240g of Chinese holly leaf, 160g of coastal glehnia root, 160g of danshen root, 80g of liquoric root, 80g of sea-buckthorn, 80g of bitter apricot seed and 40g of tabasheer, wherein the total weight is 840 g.
Or
100g of Chinese holly leaf, 80g of radix glehniae, 80g of salvia miltiorrhiza, 40g of liquorice, 40g of sea buckthorn, 40g of bitter apricot seed and 10g of tabasheer.
Example 3:
example 1 preparation of total salvianolic acids in a formula: extracting Saviae Miltiorrhizae radix with 10 times of water twice, mixing extractive solutions, adding ethanol to make alcohol concentration 40%, standing for 24 hr, filtering to remove precipitate, recovering solvent under reduced pressure, and vacuum drying or freeze drying to obtain loose powder.
Example 4:
example 2 preparation of the formula: cleaning and drying the medicinal materials, pulverizing part of Saviae Miltiorrhizae radix and concretio silicea Bambusae seu Schizostachyi, sieving with 100 mesh sieve to obtain fine powder, pulverizing the rest medicinal materials into pieces, placing into copper ware, adding 80% ethanol, decocting repeatedly for 2 times, each time for 1 hr, with the first solvent volume being 10 times and the second solvent volume being 8 times, mixing decoctions, and standing for 24 hr. Filtration and concentration of the filtrate to a relative density of 1.15-1.27(60 ℃). Adding the above fine powder, mixing, drying, grinding into fine powder, and encapsulating in No. 0 capsule to obtain the final product.
Example 5:
example 2 preparation of the formula: cleaning the medicinal materials, oven drying, extracting Saviae Miltiorrhizae radix with 10 times of water twice, mixing extractive solutions, adding ethanol to make alcohol concentration 40%, standing for 24 hr, filtering to remove precipitate, recovering solvent under reduced pressure, and vacuum drying or freeze drying to obtain loose powder. Crushing the rest materials into pieces, placing into a copper vessel, adding 80% ethanol, repeatedly decocting for 2 times (1 hr each time), with the volume of the first solvent being 10 times and the volume of the second solvent being 8 times, mixing decoctions, and standing for 24 hr. Filtration and concentration of the filtrate to a relative density of 1.15-1.27(60 ℃). Adding the above fine powder, mixing, drying, grinding into fine powder, and encapsulating in No. 0 capsule to obtain the final product.
Example 6:
example 2 preparation of the formula: cleaning all the medicinal materials, drying, crushing into pieces, putting into a copper vessel, adding 80% ethanol, repeatedly decocting for 2 times, 1 hr each time, with the volume of the first solvent being 10 times that of the second solvent being 8 times that of the first solvent, mixing decoctions, and standing for 24 hr. Filtering, recovering solvent under reduced pressure, vacuum drying or freeze drying, making into fine powder, and packaging into No. 0 capsule.
Example 7:
example 2 therapeutic effect of the formulated drug on asthma.
1. Experimental methods
BALB/C mice, SPF grade, 6-8 weeks old, female, 18-22 g body weight, 84 mice were randomly divided into A, B, C, D, E, F groups, namely normal group, model group, traditional Chinese medicine low dose treatment group, traditional Chinese medicine medium dose treatment group, traditional Chinese medicine high dose treatment group, and positive drug (dexamethasone sodium phosphate injection) treatment group.
Experimental groups and dosages
Figure BDA0003073011760000071
The preparation method of the OVA sensitizing solution comprises the following steps: 100 mu g of OVA of Grade II OVA dry powder, 2mg of aluminum hydroxide and 200 mu L of normal saline are prepared into 0.5mg/mL OVA sensitizing solution finally; the 1% OVA excited atomized liquid is OVA100mg, is dissolved in 10mL of physiological saline, is used after being fully dissolved and filtered and sterilized by a bacteria filter, and is prepared fresh before each use.
(1) B, C, D, E, F groups of mice were sensitized by intraperitoneal injection of Ovalbumin (OVA) sensitizing solution at a dose of 100uL/10g on days 1 and 14 of the experiment, respectively. Mice in group A are sensitized by intraperitoneal injection and treated by corresponding atomization by replacing OVA with equal amount of normal saline.
(2) C, D, E administration of Chinese medicinal compound extract with different concentrations to mice on 21-34 days; the mice in groups A and B are respectively subjected to intragastric lavage by replacing the medicine in the treatment group with 100 mu L/10g of physiological saline. Group F mice were injected intraperitoneally with dexamethasone 2mg/Kg (2mg/10 mL).
(3) From 28 days to 34 days after the administration for 1 hour each day from the beginning of the experiment, the mice were placed in a self-made closed container and atomized and excited with 20mL of 1% OVA excitation solution 1 time a day for 30min each time. In the experiment, positive reactions of dysphoria, tachypnea, abdominal muscle twitch, incontinence of urine and feces, frequent scratching of the nose, myasthenia of limbs and the like of the mice are observed by attentions.
(4) On day 35 of the experiment, animals were dissected, serum, lung tissue, alveolar lavage fluid were collected and stored separately in preparation for later index detection.
2. Pathological index detection
2.1 hematoxylin-eosin (HE) staining of Lung tissue and trachea samples
After anesthesia with 7% chloral hydrate, the mouse is fixed on a wood board, lung tissues and organs of a trachea of the mouse are rapidly and finely taken out and placed in 10% paraformaldehyde with the volume 2 times of the volume of the organs, and the effect of fixing the tissues is achieved. After 24 hours of fixation, paraffin embedding, sectioning, parallel HE staining, immunohistochemistry and the like are carried out, and pathological changes of each tissue are observed by an optical lens. The specific process is as follows:
a. paraffin embedding and slicing of tissues
(1) Placing the fixed tissue in 50% alcohol for 12 h;
(2) placing the tissue specimen in 70% alcohol for 4h, 80% alcohol for 30min, 90% alcohol for 30min, 95% alcohol I, 95% alcohol II, 100% alcohol I and 100% alcohol II respectively for 45 min;
(3) the xylene is transparent;
(4) wax dipping and embedding;
(5) slicing: the sections were cut with a microtome and had a thickness of 4 μm.
b. Hematoxylin-eosin (HE) staining of sections:
(1) slicing and dewaxing by conventional xylene;
(2) sequentially placing in 100% alcohol for 2min → 95% alcohol for 1min → 80% alcohol for 1min → 75% alcohol for 1min → distilled water for 2 min;
(3) staining with hematoxylin for 5 min;
(4) washing with tap water for 10 min;
(5) carrying out alcohol differentiation for 30s by hydrochloric acid;
(6) soaking in tap water for 15 min;
(7) placing in eosin dye solution for 2 min;
(8) conventional gradient alcohol dehydration, xylene clarity, neutral gum mounting: 95% alcohol (I) 1min → 95% alcohol (II) 1min → 100% alcohol (I) 1min → 100% alcohol (II) 1min → xylenecarbolic acid (3:1)1min → xylene (I) 1min → xylene (II) 1min → neutral gum sealing.
2.2 Lung tissue Masson staining
2.2.1 detection principle:
masson's trichrome staining, also known as Masson staining, is an authoritative and classical technique for staining collagen fibers, and usually refers to staining nuclei and selectively revealing collagen fibers and muscle fibers. The dyeing principle of the method is related to the size of anionic dye molecules and the penetration of tissues: the size of the molecule is represented by molecular weight, and the small molecular weight is easy to penetrate through tissues with compact structures and low permeability; while the large molecular weight can only enter tissues with loose structures and high permeability, aniline blue has large molecular weight, and the dyed muscle fibers are red and the collagen fibers are blue and are mainly used for distinguishing collagen fibers and muscle fibers.
2.2.2 reagents
Figure BDA0003073011760000091
2.2.3 detection method
1. Fixing the tissue in Bouin's fixative (purchased from another place) or Zenker's fixative (purchased from another place) or 10% neutral formalin fixative (purchased from another place), washing with running water, and conventionally dehydrating and embedding;
2. slicing and dewaxing to water conventionally;
3. taking a proper amount of Weibert iron hematoxylin A liquid and Weibert iron hematoxylin B liquid, mixing the two in equal amount to obtain Weibert iron hematoxylin staining solution, staining the mixture by the Weibert iron hematoxylin staining solution, and slightly washing the mixture by running water;
4. the acid ethanol differentiation solution is differentiated for several seconds, and washed for several minutes by running water;
5. returning the bluing liquid to blue for several seconds, and flushing with running water for several minutes;
6. dyeing the ponceau red pinkish dyeing solution for several minutes, and slightly washing with running water;
7. preparing acetic acid working solution from distilled water and acetic acid solution according to a certain proportion, and washing slices with the acetic acid working solution;
8. after the phosphomolybdic acid solution treatment, the phosphomolybdic acid solution on the glass slide is poured off (without washing with water);
9. re-dyeing with aniline blue staining solution, and pouring off the staining solution on the glass slide (without washing with water);
10. treating the slices with acetic acid working solution until the slices have no blue drop (under-lens control if necessary);
11. the 95% ethanol is dehydrated rapidly, after the absolute ethanol is dehydrated for a plurality of times, the xylene is transparent, and the neutral gum is sealed.
3 results of detection
3.1 hematoxylin-eosin (HE) staining of Lung tissue and trachea samples
According to fig. 1, the results of fig. 2 show that the wall of the lung vessel and the wall of the bronchus of the mouse in the asthma model can be thickened, and the epithelial cells of the tracheal mucosa are proliferated. The bronchial monolayer columnar epithelial cells of the asthma model mouse fall off, and the monolayer columnar epithelial cells are converted into high-layer columnar epithelial cells. The asthma model has disordered arrangement of lung tissue cells, cell degeneration, obvious necrosis of cell nucleus and infiltration of inflammatory cells. The asthma mouse treated by the traditional Chinese medicine compound provided by the invention has the advantages that the lung inflammation infiltration condition is changed, and the lung cell arrangement is in a normal state. The trachea epithelial cells reduce the withering and necrosis, and the state tends to be normalized. The Chinese medicinal compound has a relatively obvious treatment effect on asthma.
3.2 Lung tissue Masson staining
As shown in FIG. 3, the lung tissue showed blue color of collagen fibers, mucus and cartilage, red color of muscle fibers, cellulose and red blood cells, and blue-black color of cell nuclei. The mouse lung cells in the asthma model are disorganized and the fibrosis is severe. The lung tissue of the mice after the treatment by the drug administration has reduced red fiber part, and the fibrosis degree is reduced and tends to be normalized along with the increase of the drug administration dose. The Chinese medicinal compound preparation also has certain therapeutic effect on lung inflammation and injury caused by asthma.
Example 8:
establishing a fingerprint spectrum analysis method.
1. Instruments and reagents
Waters ACQUITY UPLC ultra high performance liquid chromatography, Empower 2.0 chromatography workstation, KQ3200B ultrasonic cleaning machine (Kunshan ultrasonic instruments Co., Ltd.), BSA224S electronic balance (1/10)4g) (Beijing Saedodus scientific instruments Co., Ltd.), a TGL-16G type centrifuge (Shanghai Angting scientific instruments Co., Ltd.), an SZ-93 type automatic double-unit pure water distiller (Shanghai Yangrong Biochemical instruments Co., Ltd.), and a synthetic fiber filtration membrane (pore size 0.22 μm) (Shunhuang Biotechnology Co., Ltd.).
Chromatographic grade methanol (J.K Baker, usa), chromatographic grade acetonitrile (J.K Baker, usa), analytical grade phosphoric acid (wuhan chemical reagent factory), double purified water (self-made in laboratory).
2. Preparation of reference and test articles
2.1 preparation of control solutions: precisely weighing 3.30mg of liquiritin, 1.60mg of echinocandin, 1.80mg of amygdalin, 1.70mg of salvianolic acid, 1.20mg of psoralen, 1.60mg of licochalcone, 0.60mg of rhododendron and 2.00mg of quercitrin as reference substances, and sequentially adding 1mL of methanol for ultrasonic dissolution. Respectively sucking 50 μ L of each reference solution, adding methanol to dilute to 1mL to obtain each reference solution with liquiritin 0.165mg/mL, licochalcone 0.08mg/mL, amygdalin 0.09mg/mL, salvianolic acid B0.085mg/mL, psoralen 0.06mg/mL, licochalcone B0.08 mg/mL, rhododendrin 0.03mg/mL, quercetin 0.10mg/mL, and filtering with 0.22 μm filter membrane to obtain each reference solution.
2.2 preparation of test solution: precisely weighing 1g of each of the Chinese medicinal compound preparations prepared by different preparation methods, respectively placing into a triangular flask with a plug, adding 25mL of chromatographic methanol, weighing, ultrasonically dissolving for 30min, and complementing weight loss after placing at room temperature. Shaking up, sucking 1mL, centrifuging, taking supernatant, and filtering with 0.22 μm filter membrane to obtain the final product.
3. Chromatographic analysis conditions
The chromatographic conditions are as column ACQUITY UPLC BEH C18 (2.1X 100mm, 1.7 μm); gradient elution is carried out by mobile phase A of acetonitrile and mobile phase B of 0.1 percent of phosphoric acid aqueous solution; flow rate of 0.200 mL/min-1(ii) a The detection wavelength is 254 nm; the column temperature is 30 ℃; the sample volume is 1 μ L of the reference solution, and 5 μ L of the sample solution is measured by ultra high performance liquid chromatography.
The gradient elution method is as follows:
Figure BDA0003073011760000111
4. the result of the detection
Comparing the ultra-high performance liquid fingerprint of the compound preparation with each control chromatogram, wherein 8 chromatographic peaks with RT values of 3.735min, 23.456min, 28.676min, 32.647min, 33.286min, 34.945min, 38.028min and 45.889min are confirmed to be amygdalin, liquiritin, quercitrin, licochalcone B, psoralen, salvianolic acid B, echinocandin and rhododendron, which form the fingerprint characteristics of the compound preparation and can be used as the basis for quality control of the compound preparation. The fingerprint spectrum corresponding to the traditional Chinese medicine compound preparation obtained by three preparation processes in the content of the invention is shown in figure 4, figure 5 and figure 6.

Claims (2)

1. A fingerprint spectrum measuring method of a traditional Chinese medicine compound preparation is provided, wherein the traditional Chinese medicine compound preparation is prepared from the following traditional Chinese medicine raw materials by weight: 100g of Sijiqing, 80-160g of radix glehniae, 80-160g of salvia miltiorrhiza, 40-80g of liquorice, 40-80g of sea buckthorn, 40-80g of bitter apricot seed and 10-40g of tabasheer, wherein the determination method comprises the following steps:
(1) preparation of control solutions: precisely weighing 3.30mg of liquiritin as reference substances, 1.60mg of echinocandin, 1.80mg of amygdalin, 1.70mg of salvianolic acid B, 1.20mg of psoralen, 1.60mg of licochalcone B, 0.60mg of rhododendron and 2.00mg of quercitrin, sequentially adding 1mL of methanol for ultrasonic dissolution, respectively sucking 50 μ L of the reference substance solution, adding methanol for dilution to 1mL to obtain the reference substance solutions with the concentration of liquiritin 0.165mg/mL, echinocandin 0.08mg/mL, amygdalin 0.09mg/mL, salvianolic acid B0.085mg/mL, psoralen 0.06mg/mL, licochalcone B0.08 mg/mL, rhododendron 0.03mg/mL and quercitrin 0.10mg/mL, and filtering by a filter membrane 0.22 μm to obtain the reference substance solutions;
(2) preparation of a test solution: precisely weighing 1g of each of the Chinese medicinal compound preparations prepared by different preparation methods, respectively placing into triangular flasks with stoppers, adding 25mL of chromatographic methanol, weighing, ultrasonically dissolving for 30min, standing at room temperature, supplementing weight loss, shaking, sucking 1mL, centrifuging, collecting supernatant, and filtering with 0.22 μm filter membrane to obtain the final product;
(3) the detection method comprises the following steps: precisely sucking 1 μ L of control solution and 5 μ L of test solution, respectively, and measuring by ultra high performance liquid chromatography under conditions of chromatographic column of ACQUITY UPLC BEH C18(2.1 × 100mm, 1.7 μm), gradient eluting with mobile phase A of acetonitrile and mobile phase B of 0.1% phosphoric acid water solution at flow rate of 0.200 mL/min-1Detecting at 254nm and 30 deg.C to obtain ultra-high performance liquid chromatography fingerprint of the compound Chinese medicinal preparation;
the gradient elution method is as follows:
Figure DEST_PATH_IMAGE002
comparing and monitoring the quality of the compound Chinese medicinal preparation according to the chromatogram of each reference solution and the fingerprint of the test solution.
2. The determination method according to claim 1, wherein the compound traditional Chinese medicine preparation is prepared from the following traditional Chinese medicine raw materials by weight: 240g of Chinese holly leaf, 160g of coastal glehnia root, 160g of danshen root, 80g of liquoric root, 80g of sea-buckthorn, 80g of bitter apricot seed and 40g of tabasheer.
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