CN106728195B

CN106728195B - Seven-ingredient scutellaria detoxification granule, preparation method thereof and product quality control method

Info

Publication number: CN106728195B
Application number: CN201611153085.2A
Authority: CN
Inventors: 刘升; 杨春辉; 连亚平; 杨红召; 王延珍; 冯文丽; 刘联盟; 高贵超; 胡安君
Original assignee: Henan Muxiang Biotechnology Co ltd; Henan Soar Veterinary Pharmaceutical Co Ltd
Current assignee: Henan Muxiang Biotechnology Co ltd
Priority date: 2016-12-14
Filing date: 2016-12-14
Publication date: 2020-07-24
Anticipated expiration: 2036-12-14
Also published as: CN106728195A

Abstract

The invention belongs to the technical field of veterinary medicines, and discloses seven-ingredient scutellaria detoxification particles, a preparation method thereof and a product quality control method. Is prepared from the following raw material medicaments: scutellaria baicalensis, coptis chinensis, Chinese pulsatilla roots, pomegranate bark, schisandra chinensis, gypsum and dried orange peel. Taking the raw materials, and respectively preparing into coarse powder; extracting Scutellariae radix coarse powder with ethanol, filtering, recovering ethanol, concentrating to obtain soft extract, and drying to obtain Scutellariae radix dry extract powder; decocting Coptidis rhizoma coarse powder with water, filtering, membrane separating, concentrating into soft extract, and spray drying to obtain Coptidis rhizoma dry extract powder; adding water into the coarse powder of the rest raw materials, extracting under boiling condition by continuous countercurrent, filtering, separating the filtrate with membrane to obtain clear solution, concentrating into soft extract, and spray drying to obtain dry extract powder; mixing the above dry extract powders, adding adjuvants, mixing, granulating, and drying. The granules have reasonable formula and high absorption rate, can be added by mixed drinking or mixed feeding, are convenient to use, and are beneficial to intensive and large-scale culture.

Description

Seven-ingredient scutellaria detoxification granule, preparation method thereof and product quality control method

Technical Field

The invention belongs to the technical field of veterinary medicines, and particularly relates to a seven-ingredient scutellaria detoxification granule, a preparation method thereof and a product quality control method.

Background

The piglet diarrhea has various manifestations and complex reasons, and an ideal effect can be achieved only by dialectical analysis and comprehensive treatment clinically; if the treatment is only performed on the diarrhea, the condition of the patient is possibly delayed, and serious consequences are caused. The disease brings great harm to animal husbandry.

Diarrhea is not a single disease but one of the symptoms of a systemic disease or a syndrome of gastrointestinal diseases. Only through this symptom, we can see various factors causing diarrhea through careful inference and analysis.

The factors causing diarrhea are very complex, and various factors such as microbiological factors, toxic factors, parasitic factors, internal medicine disease factors, nutritional factors, stress factors, neurological factors, functional factors and the like are common in clinic. Microbial factors are caused by infection of bacteria, viruses and other pathogenic microorganisms, wherein diarrhea caused by infection of coronavirus, escherichia coli, salmonella and clostridium welchii is most common; poisoning factors include veterinary drug poisoning, pesticide poisoning, salt poisoning, and feed poisoning; parasitic factors are mainly caused by the parasitism of nematodes, roundworms, coccidian and toxoplasma in vivo; the medical disease factors include gastroenteritis, hepatitis and the like; other factors include excessive protein, excessive fright, insufficient secretion of gastric acid, low temperature, cold water consumption, and stress caused by improper flora.

The diarrhea of the piglets is one of the important reasons for economic loss of pig raising, and if the treatment is not timely, the diarrhea has great influence on the survival rate and the growth and development of the piglets. At present, domestic pig farms generally adopt antibiotics for treatment, which causes a large amount of antibiotics to remain in pigs.

Disclosure of Invention

In order to overcome the defects in the prior art, the invention aims to provide a detoxifying granule containing seven ingredients of scutellaria baicalensis, a preparation method thereof and a product quality control method.

In order to achieve the purpose, the technical scheme adopted by the invention is as follows:

a detoxifying granule of seven-ingredient radix scutellariae is prepared from the following raw material medicines in percentage by weight: 20-40% of scutellaria baicalensis, 10-30% of coptis chinensis, 10-30% of Chinese pulsatilla root, 10-20% of pomegranate bark, 10-20% of schisandra chinensis, 10-20% of gypsum and 10-20% of dried orange peel.

The prescription mechanism of the invention is as follows: in the formula, the scutellaria baicalensis is cold in nature and bitter in taste, has the effects of clearing heat and drying dampness, cooling blood and preventing miscarriage and detoxifying, and is a monarch drug for treating high fever, polydipsia, lung heat cough and damp-heat dysentery; the coptis chinensis and the Chinese pulsatilla root are bitter and cold in nature and are used as ministerial drugs to strengthen the effects of the monarch drugs in clearing heat and removing toxicity, relieving sore throat and reducing swelling; pomegranate rind is sour and astringent, astringes intestines, stops bleeding, expels parasites, and treats chronic diarrhea and chronic dysentery; although the five flavors are complete, the schisandra chinensis is mainly sour and salty, and has warm property but not warm and dry property, which is good at astringing lung qi, nourishing kidney yin, arresting seminal emission, relieving diarrhea, promoting the production of body fluid and arresting sweating, the combination of pomegranate bark and schisandra chinensis can enhance the effect of relieving diarrhea, and the compatibility of gypsum and the combination of gypsum can release interior heat and half-exterior and half-interior heat through the functions of clearing away qi and dividing heat and blocking the testicle ventilation; the tangerine peel is warm, pungent and bitter, and has the effects of strengthening spleen and stomach, promoting qi circulation, relieving epigastric distention, lowering adverse qi and reducing phlegm. The medicines are combined to play a role in clearing heat, drying dampness, detoxifying, resisting bacteria, diminishing inflammation, astringing lung, astringing intestine, regulating spleen and stomach functions, thereby turning pathogenesis and cutting off disease potential. The product can be adjusted and treated from multiple aspects such as antivirus, antibiosis, antiphlogosis, antipyresis, spleen and stomach regulation, and the like, thereby relieving the diseases such as heat clearing, pathogen dispersing, spleen and stomach disharmony, and the like.

After the formula is prepared according to the theory of traditional Chinese veterinary medicines, the formula of the invention is mainly used for preventing and treating piglet diarrhea caused by microbial factors, has stronger heat-clearing and detoxifying, antibacterial and anti-inflammatory capabilities, and is more effective in clinical use. The seven-ingredient scutellaria detoxification granules are granules from yellow brown to dark brown; the granule has slightly sweet and bitter taste, is mainly used for treating and preventing piglet diarrhea caused by microbial factors, is convenient to use and is beneficial to absorption. The usage and dosage are as follows: mixing with feed, and mixing with the feed at a dose of 60-180g per kg for 3-5 days.

The preparation method comprises the following steps: taking the raw materials according to a certain proportion, and preparing the raw materials into coarse powder respectively; extracting Scutellariae radix coarse powder with 6-8 times of 60-70% ethanol for several times, each for 1-2 hr, filtering, mixing filtrates, recovering ethanol, concentrating to obtain soft extract with relative density of 1.20-1.25 at 60 deg.C, and spray drying to obtain Scutellariae radix dry extract powder; decocting Coptidis rhizoma coarse powder with 6-8 times of water for several times, each for 1-2 hr, filtering, mixing filtrates, membrane separating the filtrate, concentrating to obtain soft extract with relative density of 1.20-1.25 at 60 deg.C, and spray drying to obtain Coptidis rhizoma dry extract powder; adding 6-8 times of water by weight of the rest coarse powder of the raw materials into the coarse powder of the other raw materials, performing continuous countercurrent extraction for 0.5-1.5 hours under a boiling state, filtering, performing membrane separation on the filtrate to obtain clear liquid, concentrating the clear liquid into thick paste with the relative density of 1.20-1.25 at 60 ℃, and performing spray drying to obtain dry extract powder for later use; mixing the above dry extract powders, adding adjuvants 2-4 times of the total weight of the dry extract powders, mixing, using ethanol as binder, granulating, and drying to obtain QIWEIBANQIJIEDU granule.

The continuous countercurrent extraction is a method for continuously and fully carrying out contact extraction by moving medicinal materials and a solvent in opposite directions in a leaching container. The material and the solvent can keep relative motion, so that the concentration of the material liquid is diffused and updated continuously, and the leaching speed of the material liquid is high.

Preferably, the two membrane separations are ultrafiltration separations, the material is polypropylene or polysulfone, and the molecular weight cut-off is 6-10 ten thousand.

Preferably, the auxiliary materials comprise the following components in percentage by weight: 50-70% of lactose and 30-50% of soluble starch.

The quality control method of the product comprises the steps of identifying the scutellaria baicalensis, the coptis chinensis, the Chinese pulsatilla root, the pomegranate rind, the schisandra chinensis and the dried orange peel in the obtained seven-ingredient scutellaria baicalensis detoxification granules by adopting a T L C method, checking the moisture, the granularity, the dissolubility, the loading and the microbial limit according to the item of granules in the appendix of the second part of 2015 of pharmacopoeia of the people's republic of China, and measuring the content of the baicalin and the hesperidin by adopting an HP L C method.

Has the advantages that: in the method, the raw material medicines are crushed into coarse powder, which is beneficial to dissolving out the effective components and shortens the extraction time compared with the extraction of decoction pieces; continuous counter-current extraction has many advantages: the extraction speed is high, the extraction of active ingredients is sufficient, the extraction yield is high, the solvent consumption is low, the concentration of the liquid medicine is high, the subsequent treatment processes such as evaporation concentration and the like are reduced, the moving speed of the coarse powder of the medicinal materials in the roller is adjustable, so that the length of the extraction time can be adjusted according to the characteristics of the medicinal materials, the medicinal materials are extracted under a mild dynamic environment, the heating temperature is low, the damage of the active ingredients is less, the impurity content in the liquid medicine is low, the continuous production is realized, and the treatment capacity is high. In general, the seven-ingredient scutellaria detoxification granules conform to the category of new veterinary medicines released by the state; through technical transformation, unnecessary impurities are removed, the content of effective components is increased, and absorption of piglets is facilitated, so that the treatment effect is improved. In addition, the granule has reasonable formula and high absorption rate, can be added by mixed drinking or mixed feeding, is convenient to use, and is beneficial to intensive and large-scale culture.

Detailed Description

Example 1

A detoxifying granule of seven-ingredient radix scutellariae is prepared from the following raw material medicines in percentage by weight: 20% of scutellaria baicalensis, 20% of coptis chinensis, 20% of Chinese pulsatilla root, 10% of pomegranate bark, 10% of schisandra chinensis, 10% of gypsum and 10% of dried orange peel.

The preparation method comprises the following steps: taking the raw materials according to a certain proportion, and preparing the raw materials into coarse powder respectively; adding 7 weight times of 60v% ethanol into the coarse powder of the scutellaria baicalensis, extracting for 2 hours, filtering, adding 7 weight times of 60v% ethanol into the dregs of a decoction, extracting for 1 hour, filtering, combining the two extraction filtrates, recovering ethanol, concentrating to obtain thick paste with the relative density of 1.23 at 60 ℃, and performing spray drying to obtain dry extract powder of the scutellaria baicalensis for later use; decocting Coptidis rhizoma coarse powder with 7 weight times of water for 1.5 hr, filtering, decocting the residue with 7 weight times of water for 1 hr, mixing the two decoctions, membrane separating the filtrate, concentrating to obtain soft extract with relative density of 1.23 at 60 deg.C, and spray drying to obtain Coptidis rhizoma dry extract powder; adding 7 weight times of water into the rest coarse powder of other raw materials, extracting under boiling state for 1 hr by countercurrent, filtering, separating the filtrate with membrane to obtain clear solution, concentrating into soft extract with relative density of 1.23 at 60 deg.C, and spray drying to obtain dry extract powder; mixing the above dry extract powders, adding 3 times of adjuvants, mixing, granulating with 85v% ethanol as binder, and drying to obtain QIWEIBANQIJIEDU granule; wherein, the two membrane separations are both ultrafiltration separations, the material is polypropylene, and the molecular weight cut-off is 8 ten thousand; the auxiliary materials comprise the following components in percentage by weight: 60% of lactose and 40% of soluble starch.

Example 2

A detoxifying granule of seven-ingredient radix scutellariae is prepared from the following raw material medicines in percentage by weight: 30% of scutellaria baicalensis, 10% of coptis chinensis, 10% of Chinese pulsatilla root, 20% of pomegranate bark, 10% of schisandra chinensis, 10% of gypsum and 10% of dried orange peel.

The preparation method comprises the following steps: taking the raw materials according to a certain proportion, and preparing the raw materials into coarse powder respectively; adding 70v% ethanol 6 times by weight into Scutellariae radix coarse powder, extracting for 2 hr, filtering, adding 70v% ethanol 6 times by weight into the residue, extracting for 1 hr, filtering, mixing the two extractive filtrates, recovering ethanol, concentrating to obtain soft extract with relative density of 1.20 at 60 deg.C, and spray drying to obtain Scutellariae radix dry extract powder; decocting Coptidis rhizoma coarse powder with 6 weight times of water for 2 hr, filtering, decocting the residue with 6 weight times of water for 1 hr, mixing the two decoctions, membrane separating the filtrate, concentrating to obtain soft extract with relative density of 1.20 at 60 deg.C, and spray drying to obtain Coptidis rhizoma dry extract powder; adding 6 weight times of water into the rest coarse powder of other raw materials, extracting under boiling state for 0.5 hr by countercurrent, filtering, performing membrane separation to the filtrate to obtain clear solution, concentrating into soft extract with relative density of 1.20 at 60 deg.C, and spray drying to obtain dry extract powder; mixing the above dry extract powders, adding 2 times of adjuvants, mixing, granulating with 80v% ethanol as binder, and drying to obtain QIWEIBANQIJIEDU granule; wherein, the two membrane separations are both ultrafiltration separations, the material is polypropylene, and the molecular weight cut-off is 6 ten thousand; the auxiliary materials comprise the following components in percentage by weight: 50% of lactose and 50% of soluble starch.

Example 3

A detoxifying granule of seven-ingredient radix scutellariae is prepared from the following raw material medicines in percentage by weight: 30% of scutellaria baicalensis, 10% of coptis chinensis, 10% of Chinese pulsatilla root, 10% of pomegranate rind, 10% of schisandra chinensis, 10% of gypsum and 20% of dried orange peel.

The preparation method comprises the following steps: taking the raw materials according to a certain proportion, and preparing the raw materials into coarse powder respectively; adding 70v% ethanol 8 times by weight into Scutellariae radix coarse powder, extracting for 2 hr, filtering, adding 70v% ethanol 8 times by weight into the residue, extracting for 1 hr, filtering, mixing the two extractive filtrates, recovering ethanol, concentrating to obtain soft extract with relative density of 1.25 at 60 deg.C, and spray drying to obtain Scutellariae radix dry extract powder; decocting Coptidis rhizoma coarse powder with 8 weight times of water for 2 hr, filtering, decocting the residue with 8 weight times of water for 1 hr, mixing the two decoctions, membrane separating the filtrate, concentrating to obtain soft extract with relative density of 1.25 at 60 deg.C, and spray drying to obtain Coptidis rhizoma dry extract powder; adding 8 weight times of water into the rest coarse powder of other raw materials, extracting under boiling state for 1.5 hr by countercurrent, filtering, separating the filtrate with membrane to obtain clear solution, concentrating into soft extract with relative density of 1.25 at 60 deg.C, and spray drying to obtain dry extract powder; mixing the above dry extract powders, adding 4 times of adjuvants, mixing, granulating with 80v% ethanol as binder, and drying to obtain QIWEIBANQIJIEDU granule; wherein, the two membrane separations are both ultrafiltration separations, the material is polypropylene, and the molecular weight cut-off is 6 ten thousand; the auxiliary materials comprise the following components in percentage by weight: 70% of lactose and 30% of soluble starch.

Product quality control example 1:

the product is a yellow brown to brown granule; slightly sweet and bitter.

Authentication

(1) The thin-layer chromatography identification of the scutellaria baicalensis in the formula is as follows:

the test solution is prepared by collecting 5.0g of the product, grinding, adding 20m of methanol L and 1-2 drops of concentrated hydrochloric acid, performing ultrasonic treatment for 20 minutes, filtering, evaporating the filtrate, and dissolving the residue with 2ml of methanol to obtain the test solution.

The control solution is prepared by collecting baicalin control, adding methanol to obtain solution containing 0.5mg of baicalin per 1m of baicalin L, and making into control solution.

Preparation of negative solution: preparing a negative sample of the scutellaria-lack medicinal material according to the proportion and the preparation method of the prescription medicinal material, and using the negative sample as a negative control solution by operating the preparation method of the test solution.

Stationary phase: silica gel G thin layer plate.

Developing agent: ethyl acetate-butanone-formic acid-water (5: 3: 1, volume ratio).

The sample amount is 5-10 mu L.

The unfolding distance is as follows: 8-10 cm.

And (6) inspection: developing, taking out, air drying, spraying 1% ferric trichloride ethanol solution, and observing in sunlight.

And (4) conclusion: in the test sample chromatogram of examples 1-3, spots of the same color appear at the corresponding positions of the control chromatogram, and the chromatogram of the negative sample without scutellaria is not interfered at the corresponding positions.

(2) The thin-layer chromatography identification of coptis chinensis in the formula:

the sample solution is prepared by collecting 5.0g of the product, adding 2g of diatomaceous earth, grinding, adding 50m of methanol L, heating under reflux for 1 hr, filtering, and concentrating the filtrate to 2ml for dissolving to obtain sample solution.

The control solution is prepared by collecting berberine hydrochloride control, adding methanol to obtain solution containing 1 mg/1 m L as control solution.

Preparation of coptis chinensis-deficient negative solution: preparing a negative control sample lacking coptis root according to the proportion and the preparation method of the medicinal materials, taking 5.0g of the negative sample lacking coptis root, and preparing a negative solution lacking coptis root according to the preparation method of the test solution.

The development conditions are selected by sucking the three solutions 2-5 mu L respectively, dropping on the same silica gel G thin layer plate, placing in a development jar saturated by ammonia vapor with toluene-ethyl acetate-isopropanol-concentrated ammonia solution-methanol (6: 3: 1.5: 0.5, volume ratio) as developing agent, presaturating for 30 min, taking out, air drying, and inspecting under an ultraviolet lamp (365 nm).

And (4) conclusion: in the chromatogram of the test sample of examples 1-3, spots of the same color appear at the corresponding positions of the chromatogram of the reference sample, and the chromatogram of the negative sample lacking coptis does not interfere at the corresponding positions.

(3) The thin-layer chromatography identification of the pulsatilla chinensis in the formula is as follows:

the test solution is prepared by collecting 10g of the product, grinding, adding 20m of methanol L, performing ultrasonic treatment for 10 min, filtering, and concentrating the filtrate to 2m of L to dissolve to obtain test solution.

Preparation of control solutions: taking another radix Pulsatillae reference medicinal material 1g, and making into reference medicinal material solution by the same method.

Preparing a pulsatilla chinensis negative solution: preparing a pulsatilla chinensis negative control sample according to the proportion and the preparation method of the medicinal materials, and preparing a negative solution according to the preparation method of the test solution.

The development conditions are selected by sucking the three solutions 5-10 μ L respectively, dropping on the same silica gel G thin layer plate, taking the upper layer solution of n-butanol-acetic acid-water (4: 1: 2, volume ratio) as developing agent, developing, taking out, air drying, spraying with 10% sulphuric acid ethanol solution, heating at 105 deg.C until the spot color is clear.

And (4) conclusion: in the chromatograms of the test samples of examples 1-3, spots of the same color were observed at the corresponding positions of the chromatograms of the reference drugs, and the chromatogram of the anemone-deficient negative sample was free of interference at the corresponding positions.

(4) The thin-layer chromatography identification of the pomegranate rind in the formula is as follows:

the test solution is prepared by collecting 20g of the product, grinding, adding anhydrous ethanol 80m L, refluxing under heating for 1 hr, filtering, evaporating the filtrate to dryness, dissolving the residue in water 20m L, filtering, extracting the filtrate with petroleum ether (60-90 deg.C) under shaking for 2 times (20 m L each time), discarding petroleum ether solution, extracting the water solution with ethyl acetate under shaking for 2 times (20 m L each time), mixing the ethyl acetate solutions, evaporating to dryness, and dissolving the residue in methanol 1m L to obtain the test solution.

The control solution is prepared by adding methanol into gallic acid control to obtain solution containing 1mg of gallic acid per 1m L.

Preparation of negative solution: preparing a negative sample of the pomegranate rind-lacking medicinal material according to the proportion and the preparation method of the medicinal materials in the prescription, and using the negative sample as a negative control solution by operating the preparation method of the test solution.

Stationary phase: a polyamide film.

Developing agent: ethyl acetate-butanone-formic acid-water (10: 1, volume ratio).

Sample amount of spotting: 5-10 μ l.

The unfolding distance is as follows: 8-10 cm.

And (6) inspection: developing, taking out, air drying, spraying 1% ferric trichloride ethanol solution, and inspecting in sunlight.

And (4) conclusion: in the chromatogram of the test sample of the examples 1-3, spots with the same color are shown at the corresponding positions of the chromatogram of the reference medicinal material, and the chromatogram of the negative sample without pomegranate rind has no interference at the corresponding positions.

(5) Thin layer study of Schisandra chinensis in the recipe

The sample solution is prepared by collecting 10g of the product, grinding, adding chloroform 50m L, refluxing under heating for 30 min, filtering, evaporating filtrate, and dissolving residue in chloroform 1m L to obtain sample solution.

Preparation of control solutions: taking 1g of fructus Schisandrae chinensis as reference material, and making into reference material solution by the same method.

Preparation of negative solution: preparing a negative sample of the schisandra chinensis lacking medicinal material according to the proportion and the preparation method of the prescription medicinal material, and using the negative sample as a negative control solution by operating the preparation method of the test solution.

Stationary phase: silica gel GF₂₅₄A thin layer plate.

Developing agent: the upper solution of petroleum ether (30-60 ℃) -ethyl formate-formic acid (15: 5: 1, volume ratio) is used as a developing agent.

The sample amount is 5-10 mu L.

The unfolding distance is as follows: 8-10 cm.

And (6) inspection: developing, taking out, air drying, and inspecting under ultraviolet lamp (254 nm).

As a result: in the chromatogram of the test sample of examples 1-3, spots of the same color appear at the corresponding positions of the chromatogram of the control drug, and the negative control sample does not interfere at the corresponding positions.

(6) The thin-layer chromatography identification of dried orange peel in the formula is as follows:

the test solution is prepared by collecting 5g of the product, grinding, adding methanol 20m L, heating and refluxing for 30 min, filtering, and concentrating the filtrate to 2m L to dissolve to obtain test solution.

Preparation of control solutions: adding methanol into hesperidin control to obtain saturated solution as control solution.

Preparing a tangerine peel-lacking negative solution: preparing a pericarpium citri reticulatae lack negative control sample according to the proportion and the preparation method of the medicinal materials in the prescription, and preparing a negative solution according to the preparation method of the test solution.

The developing conditions are selected by sucking the three solutions 2-5 μ L respectively, dropping on the same silica gel G thin layer plate prepared with 0.5% sodium hydroxide solution, developing to about 3cm with ethyl acetate-methanol-water (100: 17: 13, volume ratio) as developing agent, taking out, air drying, developing to about 8cm with upper layer solution of toluene-ethyl acetate-formic acid-water (20: 10: 1, volume ratio) as developing agent, taking out, air drying, spraying with aluminum trichloride test solution, and inspecting under ultraviolet lamp (365 nm).

And (4) conclusion: in the chromatogram of the test sample of examples 1-3, spots with the same color appear at the corresponding positions of the chromatogram of the reference sample, and the chromatogram of the negative sample without dried orange peel does not interfere at the corresponding positions.

Product quality control example 2

According to the requirements of granules and quality standard draft in the appendix of the second part of the Chinese veterinary pharmacopoeia 2015 edition, the properties, granularity, moisture, solubility, loading, microbial limit and loading of the product are checked. The results are shown in Table 1.

Product quality control example 3 measurement of baicalin content

The determination method comprises the following steps:

[ Instrument and reagent ] high performance liquid chromatograph: agilent Technologies 1260, Agilent chromatography data workstation, uv variable wavelength detector (Agilent Technologies, inc.).

Comparison products: baicalin, batch number: 110715 and 201318 with the content of 93.3 percent, which are purchased from China institute for testing food and drug.

The detoxifying granule of seven ingredients of scutellaria: products of example 1, example 2, example 3.

The methanol and the acetonitrile are chromatographically pure, and other reagents are analytically pure.

[ chromatogram conditions and System applicability test ] uses octadecylsilane chemically bonded silica as filler; the fluidity A was methanol, the fluidity B was 0.2% phosphoric acid solution, and gradient elution was performed according to the procedure in Table 2; the detection wavelength was 278 nm. The number of theoretical plates is not less than 2000 calculated by baicalin peak.

[ preparation of control solution ] A proper amount of baicalin control (batch No. 110715-201318, content 93.3%, purchased from China institute for food and drug testing) was precisely weighed and added with methanol to prepare a solution containing 60 mug of baicalin per 1m L, thus obtaining the baicalin.

[ PREPARATION OF TEST SOLUTION ] this product is ground, about 5g is taken, precisely weighed, 70v% ethanol 40 m L is added, heating reflux is carried out for 3h, cooling is carried out, filtration is carried out, the filtrate is placed in a 100m L measuring flask, a small amount of 70v% ethanol is used for washing a container and residues in several times, the washing solution is filtered into the same measuring flask, 70v% ethanol is added to the scale, shaking is carried out uniformly, precisely measured 1m L is placed in a 10m L measuring flask, methanol is added to the scale, and shaking is carried out uniformly, thus obtaining the product.

[ measurement method ] A control solution and a test solution are respectively and precisely sucked by 10 mu L, injected into a liquid chromatograph, and measured to obtain the test solution.

The results of the product content measurements are shown in Table 3.

Control of product quality control comparative example 4 measurement of hesperidin content

The determination method comprises the following steps:

Comparison products: hesperidin, batch number: 110571-201405 with the content of 93.2 percent and purchased from China institute for food and drug testing.

[ chromatogram conditions and System suitability test ] using octadecylsilane chemically bonded silica as filler; methanol-acetic acid-water (35: 4: 61, volume ratio) is used as a mobile phase; the detection wavelength was 283 nm. The number of theoretical plates is not less than 2000 calculated according to hesperidin peak.

[ PREPARATION OF COMPARATIVE SOLUTION ] A proper amount of hesperidin COMPARATIVE (BATCH: 110571-201405, 93.2% in content, purchased from China institute for food and drug testing) was precisely weighed and added with methanol to prepare a solution containing 0.4mg per 1 ml.

[ preparation of test solution ] this product is ground, about 10g, precisely weighed, placed in a Soxhlet extractor, added with petroleum ether (60-90 ℃)80m L, heated and refluxed for 2-3 hours, the petroleum ether is discarded, the dregs are volatilized, added with methanol 80m L, heated and refluxed until the extract is colorless, cooled, filtered, the filtrate is placed in a 100m L measuring flask, the container is washed with a small amount of methanol for several times, the filtrate is filtered into the same measuring flask, added with methanol to the scale, and shaken uniformly, thus obtaining the product.

[ MEASUREMENT METHOD ] precisely sucking the reference solution and the sample solution at a ratio of 5 μ L, respectively, injecting into a liquid chromatograph, and measuring.

The results of the product content measurements are shown in Table 4.

Experimental example of animals

1 materials and methods

1.1 test drugs

Test 1 to test 3: example 3 high, medium and low doses of seven ingredient scutellaria detoxification granules.

The test group 4 is a drug control group, gentamicin sulfate injection with the specification of 10m L: 0.2g (20 ten thousand units).

1.2 test animals

7-day-old piglets in a warm county pig farm are suffered from sudden diarrhea (natural onset), the diarrhea spreads to the whole group, and sick piglets are mainly manifested as listlessness, anorexia and diarrhea of piglets. All pigs for the test adopt complete feed for piglets, and can freely eat and drink water.

1.3 test methods

1.3.1 test animal grouping and handling

Grouping by adopting a random principle, wherein each group comprises 10. Wherein the experimental groups 1-3 are three groups of the seven ingredient scutellaria detoxification granules of example 3 with high, medium and low dosages; the test group 4 is a gentamicin sulfate injection drug control group.

1.3.2 Observation of clinical efficacy

(1) Observation time: the observation is started after the first medication, and the observation is continued for 5 days after the medication is stopped;

(2) clinical symptoms and records: during the test period, the clinical manifestations of the pigs, such as spirit, appetite, water intake, number of diarrhea, number of days, morphological changes of the various excrements, etc. were observed and recorded every day.

1.3.3 evaluation criteria for therapeutic Effect

And (3) curing: after the medicine is taken, clinical symptoms disappear, the mental and ingestion conditions are recovered to be normal, the diarrhea stops, and the excrement is judged to be cured if the shape is normal. The percentage of the number of the piglets cured in each group to the number of the piglets tested in each group is the cure rate.

The method has the following advantages: after the medicine is taken, the clinical symptoms are relieved, the spirit and the ingestion condition are improved, the diarrhea frequency is reduced, and the excrement form is effectively improved. The percentage of the number of the effective piglets in each group to the number of the piglets in each group is the effective rate.

1.4 data analysis and processing

And SPSS17.0 statistical software is adopted for data analysis and processing. Counting data by X²Checking; the measurement data adopts t test or variance analysis, and the difference is significant when P is less than 0.05; p < 0.01 is very different.

2 results and analysis

On the 5 th day after stopping the administration, the curative effect of each dose group of the seven ingredient scutellaria detoxification granules was counted, and the results are shown in table 6.

As can be seen from Table 6: no piglets died in each group; after 5 days by administering the seven-ingredient scutellaria detoxification granules with different dosages, diarrhea stops or is relieved, and the spirit and appetite are improved, wherein the seven-ingredient scutellaria detoxification granules with the best high dosage group are used; the gentamicin sulfate injection group has undesirable treatment effect, and the analysis reason may be drug resistance.

The test result shows that: the seven-ingredient scutellaria detoxification granules are convenient to use and easy to absorb, have the effect of treating piglet diarrhea, and have the effect obviously better than that of a common gentamicin sulfate antibiotic medicine.

The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited by the above examples, and any other modifications without departing from the scope of the present invention should be replaced by equivalents, and all such modifications are included in the scope of the present invention.

Claims

1. A preparation method of a detoxifying granule containing seven ingredients of radix scutellariae is characterized in that: the traditional Chinese medicine is prepared from the following raw material medicines in percentage by weight: 30% of scutellaria baicalensis, 10% of coptis chinensis, 10% of Chinese pulsatilla root, 10% of pomegranate rind, 10% of schisandra chinensis, 10% of gypsum and 20% of dried orange peel; the preparation method comprises the following steps: taking the raw materials according to a certain proportion, and preparing the raw materials into coarse powder respectively; adding 70v% ethanol 8 times by weight into Scutellariae radix coarse powder, extracting for 2 hr, filtering, adding 70v% ethanol 8 times by weight into the residue, extracting for 1 hr, filtering, mixing the two extractive filtrates, recovering ethanol, concentrating to obtain soft extract with relative density of 1.25 at 60 deg.C, and spray drying to obtain Scutellariae radix dry extract powder; decocting Coptidis rhizoma coarse powder with 8 weight times of water for 2 hr, filtering, decocting the residue with 8 weight times of water for 1 hr, mixing the two decoctions, membrane separating the filtrate, concentrating to obtain soft extract with relative density of 1.25 at 60 deg.C, and spray drying to obtain Coptidis rhizoma dry extract powder; adding 8 weight times of water into the rest coarse powder of other raw materials, extracting under boiling state for 1.5 hr by countercurrent, filtering, separating the filtrate with membrane to obtain clear solution, concentrating into soft extract with relative density of 1.25 at 60 deg.C, and spray drying to obtain dry extract powder; mixing the above dry extract powders, adding 4 times of adjuvants, mixing, granulating with 80v% ethanol as binder, and drying to obtain QIWEIBANQIJIEDU granule; wherein, the two membrane separations are both ultrafiltration separations, the material is polypropylene, and the molecular weight cut-off is 6 ten thousand; the auxiliary materials comprise the following components in percentage by weight: 70% of lactose and 30% of soluble starch.