CN112138117A - Chinese medicinal effervescent granule for treating ruminant toxemia of pregnancy and preparation process thereof - Google Patents

Chinese medicinal effervescent granule for treating ruminant toxemia of pregnancy and preparation process thereof Download PDF

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Publication number
CN112138117A
CN112138117A CN202011040841.7A CN202011040841A CN112138117A CN 112138117 A CN112138117 A CN 112138117A CN 202011040841 A CN202011040841 A CN 202011040841A CN 112138117 A CN112138117 A CN 112138117A
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extract
recovering
concentrating
filtering
supernatant
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辛晓玲
李海利
王二耀
吕世杰
张子敬
陈付英
施巧婷
楚秋霞
朱肖亭
赵彩艳
余世锋
闫志浩
徐照学
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Institute of Animal Husbandry and Veterinary Medicine of Henan Academy of Agricultural Sciences
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Institute of Animal Husbandry and Veterinary Medicine of Henan Academy of Agricultural Sciences
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Abstract

The invention belongs to the technical field of veterinary medicines, and particularly relates to a traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy and a preparation process thereof. The traditional Chinese medicine preparation adopts nettle, agilawood, dried orange peel, emblic leafflower fruit, pinellia ternate, amomum villosum, mile swertia herb and spreading hedyotis herb, is a pure traditional Chinese medicine preparation, is strictly compatible according to monarch, minister, assistant and guide, has the effects of clearing heat, moistening dryness, regulating qi and blood, helping digestion, invigorating stomach, reducing the generation of ketone bodies, accelerating the oxidation of the ketone bodies, relieving acid production and toxin production, can effectively improve the serum calcium concentration and the serum total cholesterol concentration of sick ruminants, and reduces the serum inorganic phosphorus concentration, glutamic-oxalacetic transaminase, blood ketone and urine ketone of the sick ruminants, has reasonable drug effect, and has excellent curative effect on treating the toxemia of pregnancy.

Description

Chinese medicinal effervescent granule for treating ruminant toxemia of pregnancy and preparation process thereof
Technical Field
The invention belongs to the technical field of veterinary medicines, and particularly relates to a traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy and a preparation process thereof.
Background
Ruminant toxemia is a syndrome with high pathogenic rate caused by energy deficiency and abnormal carbohydrate metabolism, mainly occurs in ruminants such as cattle and sheep, and causes the ruminant toxemia mainly due to the following reasons:
firstly, the feed intake of ruminants is reduced before parturition or the feed intake of high-yield cows is reduced soon after parturition due to the relation with nutrition deficiency; or the diet is deficient in certain proteins.
The second is the large consumption of glucose caused by cold climate and serious parasite infection, which can also increase the occurrence of the disease.
Furthermore, the ruminant breeding is too early, and the nutrition level cannot be correspondingly improved in the later period of pregnancy.
The clinical symptoms of the gestational toxemia of the ruminants are mainly characterized in that the sick animals have lost appetite and can not rise over the ground, present serious ketosis symptoms, have gradually weakened functions and usually die in a lying mode after 7-10 days. In the whole course of the disease, the body temperature, the pulse and the respiration are normal, and part of the disease has neurological symptoms, such as long-time staring, head elevation, tremor of muscles at the head and the neck, final coma, accelerated heartbeat and most death. The obese sick animals are mostly attacked before parturition, the excrement is less and hard, and the obese sick animals have aggressiveness and excitation, are ataxia due to instable gait, are easy to fall down and are difficult to stand after falling down; if the disease occurs 2 months before delivery, the disease course can reach 10-14d, the patient refuses to eat, takes a chest lying posture, breathes fast, has cracked rhinoscope and has clear water-like nasal fluid; in the later stage, the patient discharges rotten yellow thin feces, is unconscious and dies in a quiet state, or produces paralysis, leftwards displacement of the true stomach, dyspepsia, retained fetal membranes, dystocia and the like.
According to the clinical manifestations, such as serious ketonemia, ketonuria, loss of appetite, asthenia, and stiff, the preliminary diagnosis can be made, and the laboratory diagnosis is needed for accurate diagnosis.
At present, the disease is widely generated on ruminants, and once the disease is generated, the disease is difficult to treat, so that huge economic losses are caused to a farm. To date, no vaccine, chemotherapeutic drug or other method has been reported to effectively control and prevent ruminant gestational toxicemia, and ruminant gestational toxemia has remained a problem that is troubling ruminants.
Disclosure of Invention
Aiming at the problem that no medicine for effectively controlling and preventing the gestational toxemia of the ruminant exists at present, the invention provides a traditional Chinese medicine effervescent granule preparation for treating the gestational toxemia of the ruminant and a preparation process thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows: a traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy comprises the following traditional Chinese medicine raw materials in parts by weight: 5-25 parts of nettle, 10-30 parts of agilawood, 5-30 parts of dried orange peel, 10-35 parts of emblic leafflower fruit, 5-35 parts of pinellia ternate, 5-35 parts of amomum villosum, 5-30 parts of swertia mileensis and 5-35 parts of oldenlandia diffusa.
The traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy comprises the following traditional Chinese medicine raw materials in parts by weight: 15 parts of nettle, 20 parts of agilawood, 20 parts of dried orange peel, 25 parts of emblic leafflower fruit, 25 parts of pinellia ternate, 20 parts of amomum villosum, 20 parts of swertia mileensis and 20 parts of oldenlandia diffusa.
The invention also provides a preparation method of the traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy, which comprises the following steps:
step one, cutting nettle, adding methanol for reflux extraction, and recovering methanol to obtain nettle liquid and nettle residue; concentrating the nettle liquid into a crude nettle extract, dissolving the crude nettle extract with purified water to prepare an aqueous solution, performing ultrasonic extraction and recovery on the aqueous solution sequentially by using normal hexane, ethyl acetate and normal butanol to obtain a refined nettle liquid, and concentrating the refined nettle liquid into the refined nettle extract for storage; adding ethanol into the nettle residue, heating and extracting, removing residue to obtain supernatant, concentrating the supernatant to obtain nettle concentrated solution, performing ultrasonic extraction on the nettle concentrated solution sequentially through petroleum ether, chloroform, ethyl acetate and n-butanol, recovering to obtain nettle extract, and storing for later use; step two, crushing the agilawood, adding ethanol, heating and extracting, filtering to obtain supernatant, concentrating the supernatant into a crude extract, adding absolute ethanol into the extract, performing ultrasonic extraction, filtering, reserving the supernatant, and concentrating to obtain a refined agilawood extract;
step three, crushing the dried orange peel, adding ethanol, heating and extracting, filtering dried orange peel dregs to obtain supernatant, recovering ethanol in the supernatant, and then reserving residual liquid to be concentrated into extract; adding ethanol into the residue, adjusting pH to 8-9 with NaOH, ultrasonic extracting, filtering, and collecting filtrate; adding HCl into the filtrate to adjust pH to 4-5, ultrasonic extracting, standing, collecting pericarpium Citri Tangerinae precipitate, and storing; adding petroleum ether into pericarpium Citri Tangerinae residue, heating for extraction, filtering, boiling, collecting supernatant, recovering petroleum ether, concentrating the residual liquid to obtain extract, and keeping;
step four, crushing the emblic leafflower fruits, decocting for 2-3 times, combining the supernatant, concentrating the supernatant into a crude extract, adding ethanol into the crude extract for ultrasonic extraction, recovering the ethanol and concentrating into an extract, sequentially performing ultrasonic extraction on the extract by diethyl ether and acetone to obtain a refined emblic leafflower fruit liquid, and concentrating the refined emblic leafflower fruit liquid into a refined extract;
step five, crushing pinellia ternate, adding water for soaking, adding a benzene solution for cold soaking, filtering and retaining supernatant, adding tartaric acid into the supernatant, performing ultrasonic extraction to obtain a tartaric acid extracting solution, adding ammonia water to adjust the pH value of the tartaric acid extracting solution to 6-7, adding chloroform for ultrasonic extraction to obtain a chloroform extracting solution, recovering chloroform and water, and concentrating into pinellia ternate extract;
step six, crushing the amomum villosum, soaking the amomum villosum in water, heating, extracting and filtering, collecting filtrate, concentrating the filtrate into a crude extract, adding petroleum ether into the crude extract, performing ultrasonic extraction, recovering the petroleum ether to retain oily liquid, adding absolute ethyl alcohol into the oily liquid, adjusting the pH value to 10-11 by using NaOH, heating, extracting, adding the petroleum ether, heating, extracting, recovering the absolute ethyl alcohol and the petroleum ether, and concentrating the residual liquid into oily matter;
step seven, crushing swertia mileensis, adding methanol, heating and extracting, filtering, recovering the methanol, and concentrating into a crude extract; adding methanol into the crude extract for dissolving, adding chloroform for ultrasonic extraction, filtering, collecting filtrate, recovering methanol and chloroform from the filtrate, and retaining precipitate for later use;
step eight, crushing oldenlandia diffusa, adding ether for soaking, filtering out residues, taking supernate, recovering ether, concentrating into extract, adding ethanol solution into the extract, regulating the pH value to 9 by using NaOH solution, soaking for 24h, then adding 10% KOH solution for alkalization, adding ether for ultrasonic extraction after alkalization, recovering ether, and concentrating into extract; adding ethanol into the residue, heating for extraction, filtering, collecting supernatant, performing ultrasonic extraction with acetone and methanol sequentially, recovering acetone and methanol, and concentrating the residual liquid to obtain extract; mixing the two extracts to obtain herba Hedyotidis Diffusae extract;
step nine, uniformly mixing the nettle extract, the nettle extracting solution, the agilawood extract, the dried orange peel precipitate, the dried orange peel extract, the emblic leafflower fruit extract, the pinellia ternate extract, the amomum villosum oily matter, the swertia mileensis precipitate and the oldenlandia diffusa extract to obtain a mixture;
and step ten, adding sodium bicarbonate into the mixture in parts, uniformly mixing, adding sugar powder and starch, uniformly stirring, putting into a granulator for granulation, drying in an oven at the temperature of 55-60 ℃, sieving, and subpackaging to obtain the finished product. The preparation method of the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following steps:
(1) chopping nettle, adding 5-8 times of methanol, reflux-extracting for 2.5h, filtering to obtain filtrate, recovering methanol with rotary evaporator, and concentrating the residual liquid to obtain extract;
(2) dissolving the extract in purified water to obtain 1-1.2 concentration water solution; adding 1 time of n-hexane into the aqueous solution, performing ultrasonic extraction for 30min, recovering the n-hexane, and retaining the aqueous solution;
(3) adding ethyl acetate in an amount which is 1 time of that of the aqueous solution in the step (2), performing ultrasonic extraction for 30min, recovering the ethyl acetate, and keeping the aqueous solution;
(4) adding 1 time of n-butanol into the aqueous solution obtained in the step (3), performing ultrasonic extraction for 30min, recovering the n-butanol, and keeping the aqueous solution; concentrating the water solution into extract by using a rotary evaporator, and storing for later use;
(5) adding 2-3 times of 90-95% ethanol into the residue obtained by filtering in step (1), heating and extracting for 3h, filtering to remove residue, and concentrating the supernatant to obtain concentrated solution;
(6) adding 1 time of petroleum ether into the concentrated solution, performing ultrasonic extraction for 1h, recovering the petroleum ether, and reserving petroleum ether extract;
(7) adding 1 time of chloroform into the petroleum ether extract, performing ultrasonic extraction for 1h, recovering the chloroform, and reserving the chloroform extract;
(8) adding 3-5% ethyl acetate into chloroform extract, performing ultrasonic extraction for 1h, and retaining ethyl acetate extract; adding 1 time of n-butanol into the ethyl acetate extract, and performing ultrasonic extraction for 1 h; recovering n-butanol to obtain herba Urticae Cannabinae extract.
The preparation method of the traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia comprises the following steps of crushing agilawood, adding 8-10 times of 95% ethanol, heating and extracting for 3 hours, filtering, reserving the supernatant, concentrating into an extract, adding absolute ethanol into the extract for dissolving, performing ultrasonic treatment for 30min, filtering out residues, reserving the supernatant, concentrating the supernatant into agilawood extract, and reserving for later use.
The preparation method of the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following steps:
(1) pulverizing pericarpium Citri Tangerinae, adding 8-10 times of 60-70% ethanol, heating and extracting for 2.5 hr, filtering the residue to obtain supernatant, recovering ethanol from the supernatant, and concentrating the residual liquid to obtain extract;
(2) adding 50-55% ethanol into the residue, adjusting pH to 8-9 with NaOH, ultrasonic extracting for 1.5 hr, filtering, and collecting filtrate;
(3) adding HCl into the filtrate obtained in the step (2) to adjust the pH value to 4-5, carrying out ultrasonic extraction for 2h, standing for 4h, collecting the dried orange peel precipitate, and reserving for later use;
(4) adding 2-3 times of petroleum ether into pericarpium Citri Tangerinae residue, heating and extracting for 3 hr, filtering, boiling and extracting for 30min, collecting supernatant, recovering petroleum ether, concentrating the residual liquid to obtain pericarpium Citri Tangerinae extract, and reserving for use.
The preparation method of the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following steps:
(1) pulverizing fructus Phyllanthi, adding 5-8 times of water, decocting for 1h, filtering residue, collecting supernatant, adding 3-5 times of water into residue, decocting for 30min, filtering, collecting supernatant, mixing the supernatants, and concentrating to obtain extract;
(2) adding 95% ethanol into the extract, ultrasonic extracting for 2 hr, filtering, collecting supernatant, recovering ethanol from the supernatant, and concentrating to obtain extract;
(3) adding 3 times of diethyl ether into the extract prepared in the step (2), performing ultrasonic treatment for 2h, recovering the diethyl ether, adding 1 time of acetone, performing ultrasonic extraction for 1h, recovering the acetone, concentrating into phyllanthus emblica extract, and storing for later use.
The preparation method of the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following concrete steps:
(1) pulverizing rhizoma Pinelliae, adding 1 times of clear water, moistening, stirring, adding 6-8 times of benzene, cold soaking for 24 hr, filtering, and keeping supernatant;
(2) adding tartaric acid 5-10 times the amount of the supernatant, and performing ultrasonic extraction for 4h to obtain tartaric acid pinellia ternate extract;
(3) adjusting pH of the tartaric acid pinellia ternate extract to 6-7 with ammonia water, adding 2 times of chloroform, and performing ultrasonic extraction for 2h to form chloroform solution; recovering water, chloroform, and concentrating to obtain rhizoma Pinelliae extract.
The preparation method of the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following steps:
(1) pulverizing YANGCHUNSHA, adding 8-10 times of water, soaking for 24 hr, heating and extracting for 4.5 hr, filtering, collecting filtrate, and concentrating to obtain extract;
(2) adding 3-5 times of petroleum ether into the extract, performing ultrasonic extraction for 30min, recovering petroleum ether, and keeping oily liquid;
(3) adding 2 times of anhydrous ethanol into the oily liquid, adjusting the pH value to 10-11 with NaOH, and heating and extracting for 1 h;
(4) adding 2 times of petroleum ether, heating and extracting for 3 hr, recovering anhydrous ethanol and petroleum ether, and concentrating the residual liquid to obtain oily substance.
The preparation method of the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following specific steps:
(1) pulverizing herba Swertiae Mileensis, adding 5-8 times of methanol, heating and extracting for 3 hr, filtering, recovering methanol from supernatant, and concentrating to obtain extract;
(2) dissolving the extract with 2-3 times of methanol, adding 5-8 times of chloroform, ultrasonic extracting for 1 hr, filtering, and collecting filtrate; recovering methanol and chloroform from the filtrate, and reserving the precipitate for later use.
The preparation method of the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following specific steps:
(1) pulverizing herba Hedyotidis Diffusae, adding 2 times of diethyl ether, soaking for 24 hr, filtering, collecting supernatant, and filtering to obtain residue; recovering diethyl ether from the supernatant, and concentrating to obtain extract;
(2) adding 60% ethanol solution into the extract, adjusting pH to 9 with NaOH, and soaking for 24 hr; adding 10% KOH solution for alkalization;
(3) adding 1 time of diethyl ether, performing ultrasonic extraction, recovering diethyl ether, and concentrating to obtain extract;
(4) adding 2 times of 65% ethanol into the residue, heating and extracting for 1 hr, filtering, and collecting supernatant; adding 1 time of acetone extract into the supernatant, and performing ultrasonic extraction for 2 h; adding 1 time of methanol, and performing ultrasonic extraction for 2 hours;
(5) recovering acetone and methanol, concentrating the residual liquid to obtain extract, and mixing the two extracts to obtain herba Hedyotidis Diffusae extract.
In the formula, the nettle is pungent in taste and cold in nature, and has the effects of activating blood circulation to stop pain, dispelling wind and removing dampness, removing food retention and relaxing bowels, relieving dyspepsia and detoxifying.
Chen Xiang is pungent and bitter in flavor and warm in nature, enters kidney, spleen and stomach meridians, and has the effects of lowering qi, warming middle energizer, eliminating dampness, promoting diuresis, warming kidney and receiving qi.
The dried orange peel is pungent and bitter in taste, warm in nature, enters spleen, stomach and lung channels, can nourish stomach, is pungent in flavor and capable of activating spleen and bitter in flavor and tonifying spleen, and has the effects of regulating qi, tonifying spleen, eliminating dampness and phlegm, harmonizing stomach and regulating middle energizer.
The emblic leafflower fruit is cool in nature and sweet in taste, enters lung and stomach channels, and has the effects of clearing heat and cooling blood, helping digestion and invigorating stomach, promoting the production of body fluid and relieving cough, inhibiting bacteria and reducing blood fat.
Pinellia ternate is pungent in flavor and warm in nature, enters spleen, stomach and lung channels, and has the effects of eliminating dampness and phlegm, lowering adverse qi and preventing vomiting, relieving distension and fullness and dispersing accumulation.
The amomum villosum which is pungent in taste and warm in nature and enters spleen and stomach channels contains various volatile oils, and the active ingredients can strengthen gastrointestinal smooth muscle peristalsis and increase the secretion of digestive enzyme without stimulating gastric acid secretion; but also can promote the survival of transplanted skin and reduce rejection; has effects in eliminating dampness, stimulating appetite, invigorating spleen, relieving diarrhea, regulating qi-flowing, and preventing miscarriage.
The mile swertia herb, which is bitter in taste, sweet in flavor and cold in nature, enters liver, gallbladder and bladder channels and has the effects of clearing liver and promoting bile flow, clearing heat and promoting diuresis, wherein the mile swertia herb contains oleanolic acid and flavonoids, can reduce serum glutamic pyruvic transaminase in blood and has a protective effect on liver cells.
Oldenlandia diffusa, cool in nature, slightly bitter in taste, entering stomach, large intestine and small intestine channels, and having the effects of clearing heat, promoting diuresis, detoxifying and resisting cancer; contains various volatile oil components, and has effects of enhancing immunity and resisting bacteria.
The invention has the beneficial effects that: the Chinese medicinal effervescent granule preparation for treating the toxemia of pregnancy of the ruminants adopts pure Chinese medicaments for preparation, is prepared according to monarch, minister, assistant and guide strictly, has the effects of clearing heat and moistening dryness, regulating qi and blood, promoting digestion and invigorating stomach, reducing the generation of ketone bodies, accelerating the oxidation of the ketone bodies, relieving acid production and toxigenicity, can effectively improve the serum calcium concentration and the serum total cholesterol concentration of the sick ruminants, and reduces the serum inorganic phosphorus concentration, the total cholesterol concentration, glutamic-oxaloacetic transaminase, serum ketonema and serum ketonuria of the sick ruminants, has reasonable medicinal effect, and has excellent curative effect on treating the toxemia of pregnancy of the ruminants. The preparation is a pure traditional Chinese medicine preparation, is safe and effective, has no residue compared with antibiotic medicines, and is suitable for popularization in animal production.
Detailed Description
In order to well prevent and control the toxemia of pregnancy of the ruminant, the invention provides a traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant according to the traditional Chinese medicine theory, and the traditional Chinese medicine effervescent granule preparation can effectively control the toxemia of pregnancy of the ruminant. The present invention will be further described with reference to the following examples.
Example 1: the embodiment provides a traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy, which comprises the following traditional Chinese medicine raw materials: 15 parts of nettle, 20 parts of agilawood, 20 parts of dried orange peel, 25 parts of emblic leafflower fruit, 25 parts of pinellia ternate, 20 parts of amomum villosum, 20 parts of swertia mileensis and 20 parts of oldenlandia diffusa.
The preparation method comprises the following steps:
step one, preparing a nettle extract and a nettle extracting solution, which specifically comprise the following steps:
(1) chopping nettle, adding 5-8 times of methanol, reflux-extracting for 2.5h, filtering to obtain filtrate, recovering methanol with rotary evaporator, and concentrating the residual liquid to obtain extract;
(2) dissolving the extract in purified water to obtain 1-1.2 concentration water solution; adding 1 time of n-hexane into the aqueous solution, performing ultrasonic extraction for 30min, recovering the n-hexane, and retaining the aqueous solution;
(3) adding ethyl acetate in an amount which is 1 time of the amount of the aqueous solution in the step (2), performing ultrasonic extraction for 30min, recovering the ethyl acetate, and keeping the aqueous solution;
(4) adding 1 time of n-butanol into the aqueous solution obtained in the step (3), performing ultrasonic extraction for 30min, recovering the n-butanol, and keeping the aqueous solution; concentrating the water solution into extract by using a rotary evaporator, and storing for later use;
(5) adding 2-3 times of 90-95% ethanol into the residue obtained by filtering in step (1), heating and extracting for 3h, filtering to remove residue, and concentrating the supernatant to obtain concentrated solution;
(6) adding 1 time of petroleum ether into the concentrated solution, performing ultrasonic extraction for 1h, recovering the petroleum ether, and reserving petroleum ether extract;
(7) adding 1 time of chloroform into the petroleum ether extract, performing ultrasonic extraction for 1h, recovering the chloroform, and reserving the chloroform extract;
(8) adding 3-5% ethyl acetate into chloroform extract, performing ultrasonic extraction for 1h, and retaining ethyl acetate extract; adding 1 time of n-butanol into the ethyl acetate extract, and performing ultrasonic extraction for 1 h; recovering n-butanol to obtain herba Urticae Cannabinae extract.
Step two, preparing agilawood extract
(1) Pulverizing lignum Aquilariae Resinatum, adding 8-10 times of 95% ethanol, heating and extracting for 3 hr, filtering, collecting supernatant, and concentrating into extract;
(2) dissolving the extract with anhydrous ethanol, ultrasonic treating for 30min, filtering to remove residue, collecting supernatant, concentrating the supernatant to obtain lignum Aquilariae Resinatum extract, and keeping.
Step three, preparing dried orange peel extract
(1) Pulverizing pericarpium Citri Tangerinae, adding 8-10 times of 60-70% ethanol, heating and extracting for 2.5 hr, filtering the residue to obtain supernatant, recovering ethanol from the supernatant, and concentrating the residual liquid to obtain extract;
(2) adding 50-55% ethanol into the residue, adjusting pH to 8-9 with NaOH, ultrasonic extracting for 1.5 hr, filtering, and collecting filtrate;
(3) adding HCl into the filtrate obtained in the step (2) to adjust the pH value to 4-5, carrying out ultrasonic extraction for 2h, standing for 4h, collecting the dried orange peel precipitate, and reserving for later use;
(4) adding 2-3 times of petroleum ether into pericarpium Citri Tangerinae residue, heating and extracting for 3 hr, filtering, boiling and extracting for 30min, collecting supernatant, recovering petroleum ether, concentrating the residual liquid to obtain pericarpium Citri Tangerinae extract, and reserving for use.
Step four, preparing the emblic leafflower fruit extract
(1) Pulverizing fructus Phyllanthi, adding 5-8 times of water, decocting for 1h, filtering residue, collecting supernatant, adding 3-5 times of water into residue, decocting for 30min, filtering, collecting supernatant, mixing the supernatants, and concentrating to obtain extract;
(2) adding 95% ethanol into the extract, ultrasonic extracting for 2 hr, filtering, collecting supernatant, recovering ethanol from the supernatant, and concentrating to obtain extract;
(3) adding 3 times of diethyl ether into the extract prepared in the step (2), performing ultrasonic treatment for 2h, recovering the diethyl ether, adding 1 time of acetone, performing ultrasonic extraction for 1h, recovering the acetone, concentrating into phyllanthus emblica extract, and storing for later use.
Step five, preparing pinellia ternate extract
(1) Pulverizing rhizoma Pinelliae, adding 1 times of clear water, moistening, stirring, adding 6-8 times of benzene, cold soaking for 24 hr, filtering, and keeping supernatant;
(2) adding tartaric acid 5-10 times the amount of the supernatant, and performing ultrasonic extraction for 4h to obtain tartaric acid pinellia ternate extract;
(3) adjusting pH of the tartaric acid pinellia ternate extract to 6-7 with ammonia water, adding 2 times of chloroform, and performing ultrasonic extraction for 2h to form chloroform solution; recovering water, chloroform, and concentrating to obtain rhizoma Pinelliae extract.
Step six, preparing the amomum villosum oily substance
(1) Pulverizing YANGCHUNSHA, adding 8-10 times of water, soaking for 24 hr, heating and extracting for 4.5 hr, filtering, collecting filtrate, and concentrating to obtain extract;
(2) adding 3-5 times of petroleum ether into the extract, performing ultrasonic extraction for 30min, recovering petroleum ether, and keeping oily liquid;
(3) adding 2 times of anhydrous ethanol into the oily liquid, adjusting the pH value to 10-11 with NaOH, and heating and extracting for 1 h;
(4) adding 2 times of petroleum ether, heating and extracting for 3 hr, recovering anhydrous ethanol and petroleum ether, and concentrating the residual liquid to obtain oily substance.
Step seven, preparing the swertia mileensis extract
(1) Pulverizing herba Swertiae Mileensis, adding 5-8 times of methanol, heating and extracting for 3 hr, filtering, recovering methanol from supernatant, and concentrating to obtain extract;
(2) dissolving the extract with 2-3 times of methanol, adding 5-8 times of chloroform, ultrasonic extracting for 1 hr, filtering, and collecting filtrate; recovering methanol and chloroform from the filtrate, and reserving the precipitate for later use.
Step eight, preparing the oldenlandia diffusa extract
(1) Pulverizing herba Hedyotidis Diffusae, adding 2 times of diethyl ether, soaking for 24 hr, filtering, collecting supernatant, and filtering to obtain residue; recovering diethyl ether from the supernatant, and concentrating to obtain extract;
(2) adding 60% ethanol solution into the extract, adjusting pH to 9 with NaOH, and soaking for 24 hr; adding 10% KOH solution for alkalization;
(3) adding 1 time of diethyl ether into the alkalified liquid, performing ultrasonic extraction, recovering the diethyl ether, and concentrating into extract for later use;
(4) adding 2 times of 65% ethanol into the residue, heating and extracting for 1 hr, filtering, and collecting supernatant; adding 1 time of acetone extract into the supernatant, and performing ultrasonic extraction for 2 h; adding 1 time of methanol, and performing ultrasonic extraction for 2 hours;
(5) recovering acetone and methanol, concentrating the residual liquid to obtain extract, and mixing the two extracts to obtain herba Hedyotidis Diffusae extract.
Step nine, mixing: mixing herba Urticae Cannabinae extract, lignum Aquilariae Resinatum extract, pericarpium Citri Tangerinae precipitate, pericarpium Citri Tangerinae extract, fructus Phyllanthi extract, rhizoma Pinelliae extract, YANGCHUNSHA oily matter, herba Swertiae Mileensis precipitate and herba Hedyotidis Diffusae extract uniformly to obtain mixture.
Step ten, granulating and subpackaging: adding sodium bicarbonate with the total amount of 80% into the mixture, mixing, adding appropriate amount of sugar powder and starch, adjusting humidity with 75% ethanol, kneading the granular powder into agglomerates, and lightly squeezing with hand to disperse the agglomerates; putting into a granulator, granulating, and sieving with a 14-mesh sieve to prepare granules; drying the granules with 14 mesh sieve in an oven at 55-60 deg.C, sieving with 16 mesh sieve, keeping the granules uniform, and subpackaging 50g per bag, which is equivalent to 50g of crude drug.
Example 2: the preparation method of the present embodiment is the same as that of embodiment 1, except that the addition amount of each traditional Chinese medicine of the traditional Chinese medicine preparation in the present embodiment is different, mainly that: the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following traditional Chinese medicine raw materials: 25 parts of nettle, 10 parts of agilawood, 30 parts of dried orange peel, 10 parts of emblic leafflower fruit, 35 parts of pinellia ternate, 35 parts of amomum villosum, 5 parts of swertia mileensis and 5 parts of oldenlandia diffusa.
Example 3: the preparation method of the present embodiment is the same as that of embodiment 1, except that the addition amount of each traditional Chinese medicine of the traditional Chinese medicine preparation in the present embodiment is different, mainly that: the traditional Chinese medicine effervescent granule preparation for treating the toxemia of pregnancy of the ruminant comprises the following traditional Chinese medicine raw materials: 5 parts of nettle, 30 parts of agilawood, 5 parts of dried orange peel, 35 parts of emblic leafflower fruit, 5 parts of pinellia ternate, 5 parts of amomum villosum, 30 parts of swertia mileensis and 35 parts of oldenlandia diffusa.
Test example 1: in order to verify the effect of the traditional Chinese medicine effervescent granules, the applicant takes cattle as a test object, tests are carried out in a certain cattle farm in Luoyang in 5 months in 2019, 28 diseased cattle are selected as test cattle, the test cattle are randomly divided into 2 groups, namely a test group and a control group, and each group has 14 cattle.
The test group feeds the traditional Chinese medicine granules with water; the control group had water normally. The test cattle of the test group and the test cattle of the control group are respectively subjected to blood sampling before and after the administration, and the blood index and the urine ketone index of the test cattle are detected, and the detection results are shown in table 1.
Figure 149409DEST_PATH_IMAGE001
After suffering from toxemia of pregnancy of the ruminant, the concentration of bovine serum calcium and the concentration of total cholesterol are obviously reduced; serum inorganic phosphorus concentration, glutamic-oxaloacetic transaminase, blood ketone and urine ketone are obviously increased. Therefore, when the concentration of calcium in bovine serum and the concentration of total cholesterol are obviously reduced; the serum inorganic phosphorus concentration, glutamic-oxaloacetic transaminase, blood ketone and urine ketone can be used as the diagnosis basis of the bovine pregnancy induced toxemia when being obviously increased.
As can be seen from Table 1, compared with normal cattle, the serum calcium concentration of the test cattle is reduced, the serum inorganic phosphorus concentration is increased, the serum total cholesterol concentration is reduced, the glutamic-oxaloacetic transaminase concentration is increased, and the blood ketone and urine ketone concentrations are obviously increased, so that the pregnancy toxemia of the cattle can be diagnosed. After the administration, as can be seen from table 1, the serum calcium concentration test group is significantly increased (P is less than 0.05) compared with the control group, the serum inorganic phosphorus concentration test group is significantly decreased (P is less than 0.05) compared with the control group, the serum total cholesterol concentration test group is significantly increased (P is less than 0.05) compared with the control group, and the serum glutamic-oxaloacetic transaminase test group is significantly decreased (P is less than 0.05) compared with the control group; the serum blood ketone and serum urine ketone test group is obviously reduced (P is less than 0.05) compared with the control group, and the traditional Chinese medicine preparation has better treatment effect on the toxemia of pregnancy of cattle.
Test example 2: in order to verify the effect of the traditional Chinese medicine effervescent granules, the applicant takes sheep as a test object, tests are carried out in an unsealed sheep farm in 2019 and 1 month, 40 diseased sheep are selected, the test sheep are randomly divided into 2 groups, namely a test group and a control group, and each group comprises 20 animals.
The test group feeds the traditional Chinese medicine granules with water; the control group had water normally. The test sheep of the test group and the test sheep of the control group are respectively subjected to blood sampling before and after administration, and the blood index and the urine ketone index of the test sheep are detected, and the detection results are shown in table 2.
Figure 535260DEST_PATH_IMAGE002
As can be seen from Table 2, the serum calcium concentration of the sick sheep is remarkably reduced, the serum inorganic phosphorus concentration is remarkably increased, the total cholesterol concentration is remarkably reduced, the glutamic-oxaloacetic transaminase is remarkably increased, and both blood ketone and urine ketone are remarkably increased, so that the ruminant gestational toxemia can be judged.
After the traditional Chinese medicine effervescent granules are prepared, the serum calcium concentration test group is remarkably increased (P is less than 0.05) compared with a control group, and the serum inorganic phosphorus concentration test group is remarkably reduced (P is less than 0.05) compared with the control group; compared with a control group, the serum total cholesterol concentration test group is obviously increased (P is less than 0.05), the serum glutamic-oxaloacetic transaminase test group is obviously reduced (P is less than 0.05), the blood ketone test group is obviously reduced (P is less than 0.05), and the urine ketone test group is obviously reduced (P is less than 0.05), so that the traditional Chinese medicine granule preparation has a better treatment effect on sheep toxemia of pregnancy.
Test example 3: in order to verify the effect of the traditional Chinese medicine effervescent granules, the applicant takes goats as test objects, tests are carried out in an unsealed goat farm in 5 months in 2019, 36 diseased goats are selected as test goats, the test goats are randomly divided into 2 groups, namely a test group and a control group, and each group has 18 goats.
The test group feeds the traditional Chinese medicine granules with water; the control group had water normally.
After the goat suffers from the toxemia of pregnancy of the ruminant, the calcium concentration and the total cholesterol concentration of the goat serum are obviously reduced; serum inorganic phosphorus concentration, glutamic-oxaloacetic transaminase, blood ketone and urine ketone are obviously increased. Therefore, when the concentration of calcium in the goat serum and the concentration of total cholesterol are obviously reduced; the serum inorganic phosphorus concentration, glutamic-oxaloacetic transaminase, blood ketone and urine ketone can be used as the diagnosis basis of goat pregnancy induced toxemia when being obviously increased.
Therefore, the test goats in the test group and the control group are respectively subjected to blood sampling before and after the administration of the medicament, and the blood indexes and the urine ketone indexes of the test goats are detected, and the detection results are shown in table 3.
Figure 204138DEST_PATH_IMAGE003
As can be seen from Table 3, the serum calcium concentration of the affected goat is significantly reduced, the serum inorganic phosphorus concentration is significantly increased, the total cholesterol concentration is significantly reduced, the glutamic-oxaloacetic transaminase is significantly increased, and the blood ketone and the urine ketone are significantly increased, so that the goat pregnancy induced toxemia is determined.
After the traditional Chinese medicine effervescent granules are prepared, a serum calcium concentration test group is remarkably increased (P is less than 0.05) compared with a control group, a serum inorganic phosphorus concentration test group is remarkably reduced (P is less than 0.05) compared with the control group, a serum total cholesterol concentration test group is remarkably increased (P is less than 0.05) compared with the control group, a serum glutamic-oxaloacetic transaminase test group is remarkably reduced (P is less than 0.05), and a blood ketone and urine ketone test group is remarkably reduced (P is less than 0.05) compared with the control group; therefore, the traditional Chinese medicine granular preparation has a good treatment effect on goat toxemia of pregnancy.
Clinical application effect
Specific case 1:
in 8 months in 2019, in a certain dairy farm in Shangqiu, some cows have lost appetite and cannot fall over, serious ketosis symptoms are presented, the body temperature, the pulse and the respiration are normal, certain cows have neurological symptoms, the patients stare at a gaze for a long time, the head is lifted, muscles of the head and the neck are tremor, finally coma, the heartbeat is accelerated, and the like. Diagnosing the ruminant gestational toxemia.
The Chinese medicinal effervescent granule preparation is used for drinking water twice a day, each time is 50 g/head, the next day, the symptoms of the affected cattle are relieved, the affected cattle can stand and drink the affected cattle with desire but can not eat grass and ruminate, the medicine is repeatedly used for 1 day, the affected cattle can eat a small amount of green grass on the third day, the affected cattle begin to ruminate, and the affected cattle can be recovered by follow-up on the fourth day.
Specific case 2:
in 2019, in 5 months, a sheep farm is unsealed, part of sheep get ill, the affected sheep have nervous symptoms, stare for a long time, have a high head, have tremor of head and neck muscles, finally are coma, have accelerated heartbeat, have little but hard excrement, are excited, are ataxia due to unstable gait, are easy to fall down, are difficult to stand after falling over the ground, and the like. Diagnosing the ruminant gestational toxemia.
The traditional Chinese medicine effervescent granule preparation is used for drinking water twice a day, 50 g/head of each time, the next day, a large amount of thin excrement of the affected sheep is discharged, rumination is started, a small amount of green hay is eaten, the medicine is repeatedly used for 2 days, and the patient can be recovered after follow-up on the fourth day.
Specific case 3:
in 3 months of 2019, a certain sheep farm is opened, part of sheep get ill, and clinical symptoms mainly show that the sick animals have lost appetite, cannot fall over, are normal in body temperature, pulse and respiration, have nervous symptoms in part, are stared at a high position for a long time, have tremor of muscles at the head and neck, are finally coma, have accelerated heartbeat and the like, and are diagnosed as the toxemia of pregnancy of the ruminants.
Drinking water by using the traditional Chinese medicine effervescent granule preparation twice a day, 30 g/sheep per time, and starting rumination of diseased sheep the next day to generate appetite; the medicine is repeatedly used for 1 day, and the disease is recovered after the follow-up on the 3 rd day.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and scope of the present invention are intended to be covered thereby.

Claims (10)

1. A traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy is characterized by comprising the following traditional Chinese medicine raw materials in parts by weight: 5-25 parts of nettle, 10-30 parts of agilawood, 5-30 parts of dried orange peel, 10-35 parts of emblic leafflower fruit, 5-35 parts of pinellia ternate, 5-35 parts of amomum villosum, 5-30 parts of swertia mileensis and 5-35 parts of oldenlandia diffusa.
2. The traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 1, is characterized by comprising the following traditional Chinese medicine raw materials in parts by weight: 15 parts of nettle, 20 parts of agilawood, 20 parts of dried orange peel, 25 parts of emblic leafflower fruit, 25 parts of pinellia ternate, 20 parts of amomum villosum, 20 parts of swertia mileensis and 20 parts of oldenlandia diffusa.
3. A process for the preparation of a Chinese medicinal effervescent granule formulation for the treatment of toxemia of pregnancy in ruminants as claimed in any one of claims 1-2, comprising the steps of:
step one, cutting nettle, adding methanol for reflux extraction, and recovering methanol to obtain nettle liquid and nettle residue; concentrating the nettle liquid into a crude nettle extract, dissolving the crude nettle extract with purified water to prepare an aqueous solution, performing ultrasonic extraction and recovery on the aqueous solution sequentially by using normal hexane, ethyl acetate and normal butanol to obtain a refined nettle liquid, and concentrating the refined nettle liquid into the refined nettle extract for storage; adding ethanol into the nettle residue, heating and extracting, removing residue to obtain supernatant, concentrating the supernatant to obtain nettle concentrated solution, performing ultrasonic extraction on the nettle concentrated solution sequentially through petroleum ether, chloroform, ethyl acetate and n-butanol, recovering to obtain nettle extract, and storing for later use;
step two, crushing the agilawood, adding ethanol, heating and extracting, filtering to obtain supernatant, concentrating the supernatant into a crude extract, adding absolute ethanol into the extract, performing ultrasonic extraction, filtering, reserving the supernatant, and concentrating to obtain a refined agilawood extract;
step three, crushing the dried orange peel, adding ethanol, heating and extracting, filtering dried orange peel dregs to obtain supernatant, recovering ethanol in the supernatant, and then reserving residual liquid to be concentrated into extract; adding ethanol into the residue, adjusting pH to 8-9 with NaOH, ultrasonic extracting, filtering, and collecting filtrate; adding HCl into the filtrate to adjust pH to 4-5, ultrasonic extracting, standing, collecting pericarpium Citri Tangerinae precipitate, and storing; adding petroleum ether into pericarpium Citri Tangerinae residue, heating for extraction, filtering, boiling, collecting supernatant, recovering petroleum ether, concentrating the residual liquid to obtain extract, and keeping;
step four, crushing the emblic leafflower fruits, decocting for 2-3 times, combining the supernatant, concentrating the supernatant into a crude extract, adding ethanol into the crude extract for ultrasonic extraction, recovering the ethanol and concentrating into an extract, sequentially performing ultrasonic extraction on the extract by diethyl ether and acetone to obtain a refined emblic leafflower fruit liquid, and concentrating the refined emblic leafflower fruit liquid into a refined extract;
step five, crushing pinellia ternate, adding water for soaking, adding a benzene solution for cold soaking, filtering and retaining supernatant, adding tartaric acid into the supernatant, performing ultrasonic extraction to obtain a tartaric acid extracting solution, adding ammonia water to adjust the pH value of the tartaric acid extracting solution to 6-7, adding chloroform for ultrasonic extraction to obtain a chloroform extracting solution, recovering chloroform and water, and concentrating into pinellia ternate extract;
step six, crushing the amomum villosum, soaking the amomum villosum in water, heating, extracting and filtering, collecting filtrate, concentrating the filtrate into a crude extract, adding petroleum ether into the crude extract, performing ultrasonic extraction, recovering the petroleum ether to retain oily liquid, adding absolute ethyl alcohol into the oily liquid, adjusting the pH value to 10-11 by using NaOH, heating, extracting, adding the petroleum ether, heating, extracting, recovering the absolute ethyl alcohol and the petroleum ether, and concentrating the residual liquid into oily matter;
step seven, crushing swertia mileensis, adding methanol, heating and extracting, filtering, recovering the methanol, and concentrating into a crude extract; adding methanol into the crude extract for dissolving, adding chloroform for ultrasonic extraction, filtering, collecting filtrate, recovering methanol and chloroform from the filtrate, and retaining precipitate for later use;
step eight, crushing oldenlandia diffusa, adding ether for soaking, filtering out residues, taking supernate, recovering ether, concentrating into extract, adding ethanol solution into the extract, regulating the pH value to 9 by using NaOH solution, soaking for 24h, then adding 10% KOH solution for alkalization, adding ether for ultrasonic extraction after alkalization, recovering ether, and concentrating into extract; adding ethanol into the residue, heating for extraction, filtering, collecting supernatant, performing ultrasonic extraction with acetone and methanol sequentially, recovering acetone and methanol, and concentrating the residual liquid to obtain extract; mixing the two extracts to obtain herba Hedyotidis Diffusae extract;
step nine, uniformly mixing the nettle extract, the nettle extracting solution, the agilawood extract, the dried orange peel precipitate, the dried orange peel extract, the emblic leafflower fruit extract, the pinellia ternate extract, the amomum villosum oily matter, the swertia mileensis precipitate and the oldenlandia diffusa extract to obtain a mixture;
and step ten, adding sodium bicarbonate into the mixture in parts, uniformly mixing, adding sugar powder and starch, uniformly stirring, putting into a granulator for granulation, drying in an oven at the temperature of 55-60 ℃, sieving, and subpackaging to obtain the finished product.
4. The preparation method of the Chinese medicinal effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 3, which is characterized in that: the first step specifically comprises the following steps:
(1) chopping nettle, adding 5-8 times of methanol, reflux-extracting for 2.5h, filtering to obtain filtrate, recovering methanol with rotary evaporator, and concentrating the residual liquid to obtain extract;
(2) dissolving the extract in purified water to obtain 1-1.2 concentration water solution; adding 1 time of n-hexane into the aqueous solution, performing ultrasonic extraction for 30min, recovering the n-hexane, and retaining the aqueous solution;
(3) adding ethyl acetate in an amount which is 1 time of that of the aqueous solution in the step (2), performing ultrasonic extraction for 30min, recovering the ethyl acetate, and keeping the aqueous solution;
(4) adding 1 time of n-butanol into the aqueous solution obtained in the step (3), performing ultrasonic extraction for 30min, recovering the n-butanol, and keeping the aqueous solution; concentrating the water solution into extract by using a rotary evaporator, and storing for later use;
(5) adding 2-3 times of 90-95% ethanol into the residue obtained by filtering in step (1), heating and extracting for 3h, filtering to remove residue, and concentrating the supernatant to obtain concentrated solution;
(6) adding 1 time of petroleum ether into the concentrated solution, performing ultrasonic extraction for 1h, recovering the petroleum ether, and reserving petroleum ether extract;
(7) adding 1 time of chloroform into the petroleum ether extract, performing ultrasonic extraction for 1h, recovering the chloroform, and reserving the chloroform extract;
(8) adding 3-5% ethyl acetate into chloroform extract, performing ultrasonic extraction for 1h, and retaining ethyl acetate extract; adding 1 time of n-butanol into the ethyl acetate extract, and performing ultrasonic extraction for 1 h; recovering n-butanol to obtain herba Urticae Cannabinae extract.
5. The preparation method of the Chinese medicinal effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 3, which is characterized in that: the third step comprises the following steps:
(1) pulverizing pericarpium Citri Tangerinae, adding 8-10 times of 60-70% ethanol, heating and extracting for 2.5 hr, filtering the residue to obtain supernatant, recovering ethanol from the supernatant, and concentrating the residual liquid to obtain extract;
(2) adding 50-55% ethanol into the residue, adjusting pH to 8-9 with NaOH, ultrasonic extracting for 1.5 hr, filtering, and collecting filtrate;
(3) adding HCl into the filtrate obtained in the step (2) to adjust the pH value to 4-5, carrying out ultrasonic extraction for 2h, standing for 4h, collecting the dried orange peel precipitate, and reserving for later use;
(4) adding 2-3 times of petroleum ether into pericarpium Citri Tangerinae residue, heating and extracting for 3 hr, filtering, boiling and extracting for 30min, collecting supernatant, recovering petroleum ether, concentrating the residual liquid to obtain pericarpium Citri Tangerinae extract, and reserving for use.
6. The preparation method of the Chinese medicinal effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 3, which is characterized in that: the fourth step specifically comprises the following steps:
(1) pulverizing fructus Phyllanthi, adding 5-8 times of water, decocting for 1h, filtering residue, collecting supernatant, adding 3-5 times of water into residue, decocting for 30min, filtering, collecting supernatant, mixing the supernatants, and concentrating to obtain extract;
(2) adding 95% ethanol into the extract, ultrasonic extracting for 2 hr, filtering, collecting supernatant, recovering ethanol from the supernatant, and concentrating to obtain extract;
(3) adding 3 times of diethyl ether into the extract prepared in the step (2), performing ultrasonic treatment for 2h, recovering the diethyl ether, adding 1 time of acetone, performing ultrasonic extraction for 1h, recovering the acetone, concentrating into phyllanthus emblica extract, and storing for later use.
7. The preparation method of the traditional Chinese medicine effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 3, wherein the step five specifically comprises the following steps:
(1) pulverizing rhizoma Pinelliae, adding 1 times of clear water, moistening, stirring, adding 6-8 times of benzene, cold soaking for 24 hr, filtering, and keeping supernatant;
(2) adding tartaric acid 5-10 times the amount of the supernatant, and performing ultrasonic extraction for 4h to obtain tartaric acid pinellia ternate extract;
(3) adjusting pH of the tartaric acid pinellia ternate extract to 6-7 with ammonia water, adding 2 times of chloroform, and performing ultrasonic extraction for 2h to form chloroform solution; recovering water, chloroform, and concentrating to obtain rhizoma Pinelliae extract.
8. The preparation method of the Chinese medicinal effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 3, which is characterized in that: the sixth step specifically comprises the following steps:
(1) pulverizing YANGCHUNSHA, adding 8-10 times of water, soaking for 24 hr, heating and extracting for 4.5 hr, filtering, collecting filtrate, and concentrating to obtain extract;
(2) adding 3-5 times of petroleum ether into the extract, performing ultrasonic extraction for 30min, recovering petroleum ether, and keeping oily liquid;
(3) adding 2 times of anhydrous ethanol into the oily liquid, adjusting the pH value to 10-11 with NaOH, and heating and extracting for 1 h;
(4) adding 2 times of petroleum ether, heating and extracting for 3 hr, recovering anhydrous ethanol and petroleum ether, and concentrating the residual liquid to obtain oily substance.
9. The preparation method of the Chinese medicinal effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 3, which is characterized in that: the seventh step specifically comprises the following steps:
(1) pulverizing herba Swertiae Mileensis, adding 5-8 times of methanol, heating and extracting for 3 hr, filtering, recovering methanol from supernatant, and concentrating to obtain extract;
(2) dissolving the extract with 2-3 times of methanol, adding 5-8 times of chloroform, ultrasonic extracting for 1 hr, filtering, and collecting filtrate; recovering methanol and chloroform from the filtrate, and reserving the precipitate for later use.
10. The preparation method of the Chinese medicinal effervescent granule preparation for treating ruminant toxemia of pregnancy according to claim 3, which is characterized in that: the eighth step specifically comprises the following steps:
(1) pulverizing herba Hedyotidis Diffusae, adding 2 times of diethyl ether, soaking for 24 hr, filtering, collecting supernatant, and filtering to obtain residue; recovering diethyl ether from the supernatant, and concentrating to obtain extract;
(2) adding 60% ethanol solution into the extract, adjusting pH to 9 with NaOH, and soaking for 24 hr; adding 10% KOH solution for alkalization;
(3) adding 1 time of diethyl ether, performing ultrasonic extraction, recovering diethyl ether, and concentrating to obtain extract;
(4) adding 2 times of 65% ethanol into the residue, heating and extracting for 1 hr, filtering, and collecting supernatant; adding 1 time of acetone extract into the supernatant, and performing ultrasonic extraction for 2 h; adding 1 time of methanol, and performing ultrasonic extraction for 2 hours;
(5) recovering acetone and methanol, concentrating the residual liquid to obtain extract, and mixing the two extracts to obtain herba Hedyotidis Diffusae extract.
CN202011040841.7A 2020-09-28 2020-09-28 Chinese medicinal effervescent granule for treating ruminant toxemia of pregnancy and preparation process thereof Pending CN112138117A (en)

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CN111450219A (en) * 2020-05-11 2020-07-28 仕裕(焦作)中药生物科技有限公司 A Chinese medicinal granule for treating acute carbohydrate hyperphagia of ruminant, and its preparation method

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