TWI419698B - Pharmaceutical composition for treating diabetes and its preparation method - Google Patents
Pharmaceutical composition for treating diabetes and its preparation method Download PDFInfo
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本發明涉及一種治療糖尿病的藥物組合物的製備方法,以及由所述方法製備得到的藥物組合物。The present invention relates to a process for the preparation of a pharmaceutical composition for treating diabetes, and a pharmaceutical composition prepared by the method.
糖尿病是由體內糖、蛋白質和脂肪代謝紊亂而造成的一種慢性進行性終身疾病,其特徵性表現為高血糖和糖尿。這種病將導致心臟和腎臟併發症、眼盲和截肢。近年來從臨床上觀察,糖尿病的發病率正在呈逐年上升趨勢。目前,全世界約有1·5億糖尿病患者,我國目前糖尿病人數已超過4000萬。在糖尿病病例中,少數為胰島素依賴型糖尿病(I型),大多數為非胰島素依賴型糖尿病(Ⅱ型)。大多數的糖尿病患者需要終身服藥。Diabetes is a chronic progressive life-threatening disorder caused by disorders of sugar, protein and fat metabolism in the body, characterized by hyperglycemia and diabetes. This disease can lead to heart and kidney complications, blindness and amputation. In recent years, clinical observation shows that the incidence of diabetes is increasing year by year. At present, there are about 150 million diabetic patients in the world, and the number of diabetes in China is over 40 million. Among the cases of diabetes, a small number are insulin-dependent diabetes mellitus (type I), and most are non-insulin-dependent diabetes mellitus (type II). Most people with diabetes need to take medication for life.
目前糖尿病治療仍以化學合成藥物為主,如磺胺類、雙胍類、葡萄糖苷酶抑制劑、格列奈類和胰島素增敏劑等。但這些藥物長期服用副作用均比較大。At present, the treatment of diabetes is still based on chemical synthetic drugs, such as sulfonamides, biguanides, glucosidase inhibitors, glinides and insulin sensitizers. However, the long-term side effects of these drugs are relatively large.
中醫藥在防治糖尿病方面有著悠久的歷史,經過幾千年的實踐,積累了大量的寶貴經驗,形成了獨特的學術體系。中醫藥典籍記載了很多具有降糖療效的中藥,如澤瀉、知母、西洋參、葛根、地黃、花粉等。傳統的中醫治療糖尿病是根據臨床症狀進行三消論治。但在糖耐量減低期及糖尿病發病的早期卻沒有很好的治療辦法。Traditional Chinese medicine has a long history of preventing and treating diabetes. After thousands of years of practice, it has accumulated a lot of valuable experience and formed a unique academic system. Chinese medicine classics record many traditional Chinese medicines with hypoglycemic effects, such as Alisma, Anemarrhena, American ginseng, Pueraria, Rehmannia, and pollen. Traditional Chinese medicine treatment of diabetes is based on clinical symptoms. However, there is no good treatment in the period of impaired glucose tolerance and early onset of diabetes.
糖尿病之位首責於肝胃,鬱熱內蘊是消渴病的病理基礎,「木郁達之」、“土鬱奪之”,故當以疏導為主,即“必伏其所主,而先其所因”。糖敏靈開鬱清胃,滋陰降火,通腑 瀉濁,標本兼治,鬱熱既清,則氣陰自複。《證治準繩.消癉》雲:“使道路散而不結,津液生而不枯,氣血和而不澀,則病自已矣。”,因此,糖尿病的治療以開鬱清胃,滋陰降火,通腑瀉濁。Diabetes is the first place to be responsible for the liver and stomach. The stagnation of heat is the pathological basis of diabetes, "Mu Yu Da Zhi", "Tu Yu Yu Zhi", so it is mainly based on dredging, that is, "it must be the owner of the disease, and First, the cause." Sugar-sensitive spirit opens the stomach and clears the stomach, nourishing yin and reducing fire, all night It is diarrhea, both the symptoms and the cure, and the stagnation of the stagnation is clear. "Criteria for the rule of law. Dispelling the cloud: "Let the roads to be scattered, the liquid is not dry, the blood is not dry, and the disease is self-defeating." Therefore, the treatment of diabetes is to clear the stomach, nourish the yin and reduce the fire. It is turbid.
根據傳統的中醫藥理論,過食少動所引起的胃腸鬱滯,使中焦大氣轉運受阻,大氣不轉,肝膽之疏泄亦郁閉,鬱而化熱,出現肝膽胃腸肺等三焦之熱。故以黃連,大黃為君,黃連清胃熱,大黃清瀉腸熱,此乃以苦治甜。白芍、黃芩、柴胡為臣,白芍柔肝斂陰,佐君以清三焦之熱而不傷陰,柴胡入少陽膽經和厥陰肝經,清肝膽之熱,疏泄脾胃,黃芩清肝肺之熱。枳實、生山楂理氣消食導滯,合大黃以暢腸胃,半夏合黃連辛開苦降,開暢中焦,故為佐。烏梅酸以斂陰生津,此乃酸以制甜,合天花粉以救肺胃之陰,故應稱之謂使也。According to the traditional Chinese medicine theory, the gastrointestinal stagnation caused by overeating and less movement makes the middle coke atmospheric transport blocked, the atmosphere does not turn, the hepatobiliary leakage is also closed, the stagnation and heat, the hepatobiliary gastrointestinal lung and other three coke fever. Therefore, the use of berberine, rhubarb for the king, huanglianqing stomach heat, rhubarb diarrhea intestinal heat, this is to cure sweet. White peony, scutellaria, and Bupleurum are the ministers. The white sputum is soft and the liver is convulsive. The sage is not to hurt the yin by the heat of the three cokes. The Bupleurum enters the Shaoyang biliary tract and the sputum yin and liver, clears the heat of the liver and gallbladder, and relieves the spleen and stomach. Hepatic and pulmonary heat.枳 、 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生 生Umeic acid is used to succumb to yin and spleen. This is the acid to make sweet, and the combination of Tianhua powder to save the lungs and the yin, so it should be called the yin.
本發明人以中醫“鬱熱”學說為理論依據,研究發現,由天花粉、柴胡、枳實、大黃、半夏、黃芩、黃連、白芍、烏梅等藥材組成的組合物對糖尿病具有很好的治療作用。所述藥物公開在本申請人早期的大陸地區專利申請200410020220.7之中,但是,該專利申請中採用了傳統的醇提方法,用該方法得到的提取物損失了大量的水溶性有效成分;不僅收率低,而且有效成分的含量很小,所以給藥劑量很大,相應的副作用也會增加。The inventor based on the theory of traditional Chinese medicine "sweet fever", the research found that the composition consisting of medicinal materials such as trichosanthin, Bupleurum, medlar, rhubarb, pinellia, astragalus, berberine, white peony, and ebony has good effect on diabetes. Therapeutic effect. The drug is disclosed in the applicant's early mainland patent application 200410020220.7, however, the patent application uses a conventional alcohol extraction method, and the extract obtained by the method loses a large amount of water-soluble active ingredient; The rate is low, and the content of the active ingredient is small, so the dose is large, and the corresponding side effects are also increased.
本發明的目的在於提供了一種具有下述組成的,用於治療糖尿病的藥物組合物,該藥物組合物是由本發明的下述的方法製成的,從而解決了現有技術中存在的上述問題。SUMMARY OF THE INVENTION An object of the present invention is to provide a pharmaceutical composition for treating diabetes which has the following composition, which is produced by the following method of the present invention, thereby solving the above problems in the prior art.
本發明的又一目的是提供了本發明藥物組合物的製備方法,所述的藥物組合物含有如下重量份的生藥材製備的提取物:天花粉5-40份、柴胡10-30份、枳實3-15份、大黃1-6份、半夏1-12份、黃芩3-15份、黃連1-12份、白芍3-15份和烏梅5-20份,並任選含有藥學上可接受的輔料;該組合物用下述方法之一製備:方法一,包括以下步驟:(1)按照所述重量份數比取所需的藥材;(2)將所述藥材加水回流提取,提取液過濾、減壓濃縮;(3)在濃縮液中加入乙醇至含醇量為65-75%,過濾;(4)將濾液減壓濃縮成浸膏;(5)任選的在上述浸膏中加入輔料製成藥劑學上可接受的劑型;方法二,包括以下步驟:(1)按照所述重量份數比取所需的藥材;(2)將所述藥材加水回流提取,將提取液放涼、過濾、合併得濾液;(3)將濾液過大孔吸附樹脂,用水洗脫,棄去,繼續用一定濃度的乙醇洗脫,合併洗脫液,減壓回收乙醇得浸膏;(4)任選的在上述浸膏中加入輔料製成藥劑學上可接受的劑型;方法三,包括以下步驟:(1)按照所述重量份數比取所需的藥材; (2)將其中的藥材柴胡、白芍、枳實、大黃、黃芩、黃連用一定濃度的乙醇回流提取,將將提取液放涼、過濾、合併;(3)在上一步驟所得到的藥渣中加入其他藥材,加水回流提取,提取液減壓濃縮,濃縮液加入乙醇至含醇量為65-75%,過濾;(4)將(2)和(3)所得濾液合併,濃縮成浸膏;(5)任選的在上述浸膏中加入輔料製成藥劑學上可接受的劑型;方法四,包括以下步驟:(1)按照所述重量份數比取所需的藥材;(2)將黃芩加水回流提取,合併提取液,調pH值至1.5-2.0;保溫,靜置,濾過,沈澱用水洗pH值至5-6,乾燥,得黃芩提取物乾粉;(3)將黃連加乙醇回流提取,合併提取液,濾過,回收乙醇至無醇味,調pH值至1-2;冷藏過夜,濾過,沈澱用水洗pH值至5-6,乾燥,得黃連提取物乾粉;(4)將其他藥材加水回流提取,提取液合併,濃縮,放涼,加入95%乙醇,使提取液的含醇量達到70%;靜置,濾過,回收乙醇得浸膏;乾燥,得提取物乾粉;和(5)將上述三個步驟得到的提取物乾粉混合均勻;並任選的加入輔料製成藥劑學上可接受的劑型。A further object of the present invention is to provide a process for the preparation of a pharmaceutical composition of the present invention, which comprises the following extracts prepared from raw materials: 5-40 parts of trichosanthin, 10-30 parts of Bupleurum, and medlar 3-15 parts, 1-6 parts of rhubarb, 1-12 parts of Pinellia, 3-15 parts of astragalus, 1-12 parts of berberine, 3-15 parts of white peony and 5-20 parts of ebony, and optionally containing pharmacy An acceptable excipient; the composition is prepared by one of the following methods: Method 1, comprising the steps of: (1) taking the desired medicinal material according to the parts by weight; (2) adding the medicinal material to reflux extraction , extracting the extract, and concentrating under reduced pressure; (3) adding ethanol to the concentrate to an alcohol content of 65-75%, filtering; (4) concentrating the filtrate under reduced pressure into an extract; (5) optionally in the above The excipient is added to the extract to form a pharmaceutically acceptable dosage form; the second method comprises the following steps: (1) taking the desired medicine according to the weight ratio; (2) adding the water to the reflux extraction, The extract is allowed to cool, filtered, and combined to obtain a filtrate; (3) the filtrate is passed through a macroporous adsorption resin, eluted with water, discarded, and continued to be used at a certain concentration. Ethanol elution, combining the eluate, recovering the ethanol to obtain an extract under reduced pressure; (4) optionally adding an auxiliary material to the above-mentioned extract to prepare a pharmaceutically acceptable dosage form; and the third method comprises the following steps: (1) Taking the desired medicinal material according to the weight ratio; (2) The medicinal materials Bupleurum, Radix Paeoniae Alba, Radix Paeoniae Alba, Rhubarb, Radix Astragali, Rhizoma Coptidis are refluxed with a certain concentration of ethanol, and the extracts are allowed to cool, filter and combine; (3) obtained in the previous step Adding other herbs to the dregs, adding water to reflux extraction, extracting the extract under reduced pressure, adding concentrated ethanol to the alcohol content of 65-75%, filtering; (4) combining the filtrates obtained by (2) and (3), concentrating a immersion cream; (5) optionally adding an auxiliary material to the above-mentioned extract to prepare a pharmaceutically acceptable dosage form; and the method 4 includes the following steps: (1) taking the desired medicinal material according to the weight ratio; (2) refluxing the extract of Astragalus membranaceus with water, combining the extracts, adjusting the pH to 1.5-2.0; keeping warm, standing, filtering, precipitating the pH to 5-6 with water, drying to obtain dried powder of Astragalus membranaceus extract; (3) Coptis chinensis is added with ethanol reflux extraction, the extract is combined, filtered, and the ethanol is recovered to a non-alcoholic taste, and the pH is adjusted to 1-2; refrigerated overnight, filtered, and the precipitate is washed with water to a pH of 5-6, and dried to obtain a dry powder of Coptis chinensis extract; (4) Add other herbs to the water for reflux extraction, combine the extracts, concentrate, let cool, add 95% ethanol, make The alcohol content of the liquid is up to 70%; it is allowed to stand, filtered, and the ethanol is recovered to obtain an extract; dried to obtain an extract dry powder; and (5) the dry powder obtained by the above three steps is uniformly mixed; and optionally added The excipients are formulated in a pharmaceutically acceptable dosage form.
用本發明方法製備的藥物組合物中,各種生藥材優選的重量比為:天花粉9份、柴胡12份、枳實9份、大黃3份、半夏6份、黃芩9份、黃連6份、白芍9份和烏梅 9份。In the pharmaceutical composition prepared by the method of the present invention, the preferred weight ratios of various raw materials are: 9 parts of trichosanthin, 12 parts of Bupleurum, 9 parts of medlar, 3 parts of rhubarb, 6 parts of Pinellia, 9 parts of astragalus, and berberine 6 Parts, 9 times of white peony and ebony 9 copies.
進一步的,在上述藥物配方的基礎上,本發明的藥物組合物在其配方中還可以加入山楂,這是因為山楂酸甘化陰,既可以防辛散太過傷陰,又可苦酸制甜。配伍開鬱清熱具有很好的療效。因此,優選的技術方案是各種生藥材的重量份數比為:天花粉5-40份、柴胡10-30份、枳實3-15份、大黃l-6份、半夏1-12份、黃芩3-15份、黃連l-12份、白芍3-15份、烏梅5-20份和山楂3-15份。Further, on the basis of the above-mentioned pharmaceutical formula, the pharmaceutical composition of the present invention can also be added to the hawthorn in the formula, because the behenic acid is sallow and yin, which can prevent the sputum from being too suffocating and the bitter acid. sweet. It has a good effect in combination with Kaiyuqing. Therefore, a preferred technical solution is that the ratio of parts by weight of various raw materials is: 5-40 parts of trichosanthin, 10-30 parts of Bupleurum, 3-15 parts of medlar, l-6 parts of rhubarb, 1-12 parts of Pinellia ternata. 3-15 parts of astragalus, l-12 parts of berberine, 3-15 parts of white peony, 5-20 parts of ebony and 3-15 parts of hawthorn.
因此,更優選本發明藥物組合物中各種生藥材的重量份數比為:天花粉10-30份、柴胡10-30份、枳實3-15份、大黃1-6份、半夏1-12份、黃芩3-15份、黃連1-12份、白芍3-15份、烏梅5-20份和山楂3-15份。Therefore, it is more preferred that the weight ratio of various raw materials in the pharmaceutical composition of the present invention is: 10-30 parts of trichosanthin, 10-30 parts of Bupleurum, 3-15 parts of medlar, 1-6 parts of rhubarb, and Pinellia 1 -12 parts, 3-15 parts of astragalus, 1-12 parts of berberine, 3-15 parts of white peony, 5-20 parts of ebony and 3-15 parts of hawthorn.
最優選的,本發明藥物組合物中各種生藥材的重量份數比為:天花粉30份、柴胡12份、枳實9份、大黃3份、半夏6份、黃芩9份、黃連6份、白芍9份、烏梅15份和山楂9份;或者是天花粉15份、柴胡12份、枳實9份、大黃3份、半夏6份、黃芩9份、黃連6份、白芍9份、烏梅15份和山楂9份。Most preferably, the weight ratio of various raw materials in the pharmaceutical composition of the present invention is: 30 parts of trichosanthin, 12 parts of Bupleurum, 9 parts of medlar, 3 parts of rhubarb, 6 parts of Pinellia, 9 parts of astragalus, and berberine 6 9 parts, 9 times of white peony, 15 parts of ebony and 9 parts of hawthorn; or 15 parts of trichosanthin, 12 parts of Bupleurum, 9 parts of medlar, 3 parts of rhubarb, 6 parts of Pinellia, 9 parts of Astragalus, 6 parts of berberine, 6 parts of white 9 parts, 15 pieces of ebony and 9 parts of hawthorn.
具體的,在本發明上述的方法一中,優選採用下述操作條件:1、在步驟(2)中,優選回流提取兩次,每次用10倍於所述藥材重量的水,每次1.5小時。優選提取液濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1。Specifically, in the first method of the present invention, the following operating conditions are preferably employed: 1. In the step (2), preferably, the extract is refluxed twice, each time using 10 times the weight of the medicinal material, each time 1.5. hour. Preferably, the extract is concentrated to a ratio of the original medicinal weight (kg) to the volume (L) of the concentrate of 1:1.
2、在步驟(3)中,加入的乙醇濃度優選為90-100%,優選為95%。加入乙醇後,所得到的濃縮液的含醇量優選 為70%。2. In step (3), the concentration of ethanol added is preferably from 90 to 100%, preferably 95%. After adding ethanol, the alcohol content of the obtained concentrate is preferably It is 70%.
由於採用了本發明上述水提醇沈的提取方法,由該方法製備得到的中藥組合物中有效成分的含量明顯提高,雜質的含量明顯減少,從而可減少給藥的劑量。Due to the above extraction method of the water extraction and alcohol precipitation of the present invention, the content of the active ingredient in the traditional Chinese medicine composition prepared by the method is remarkably improved, and the content of the impurities is remarkably reduced, thereby reducing the dose to be administered.
在本發明上述的方法二中,優選採用下述操作條件:1、在步驟(2)中,優選加水回流提取兩次,每次用10倍於所述藥材重量的水,每次提取1小時。In the above method 2 of the present invention, the following operating conditions are preferably employed: 1. In the step (2), it is preferred to add water twice to reflux and extract twice, each time using 10 times the weight of the medicinal material, one hour for each extraction. .
2、在步驟(3)中,大孔樹脂優選為AB-8型。樹脂和藥材重量比優選為1:1.5-1:3,進一步優選為1:2。提取液的上樣速度優選為4-6倍柱體積/小小時。水洗量優選為4-6倍柱體積。用於洗脫的乙醇濃度優選為80%-95%,進一步優選為90%。乙醇用量優選為2-5倍柱體積。減壓回收乙醇的溫度優選為60-80℃,減壓回收乙醇得到浸膏,浸膏的相對密度為1.25-1.35,優選為相對密度為1.30。2. In the step (3), the macroporous resin is preferably of the AB-8 type. The weight ratio of the resin to the medicinal material is preferably from 1:1.6 to 1:3, and more preferably 1:2. The loading speed of the extract is preferably 4-6 column volumes/hour. The amount of water washing is preferably 4-6 column volumes. The concentration of ethanol used for elution is preferably from 80% to 95%, further preferably 90%. The amount of ethanol used is preferably from 2 to 5 column volumes. The temperature at which the ethanol is recovered under reduced pressure is preferably 60-80 ° C, and ethanol is recovered under reduced pressure to obtain an extract having a relative density of from 1.25 to 1.35, preferably a relative density of 1.30.
本發明的上述製備方法採用了水提工藝,可以保證水溶性有效成分,如柴胡皂苷、黃連素(鹽酸小檗鹼)、黃芩苷、大黃酚、芍藥苷、辛弗林等得到最大程度的提取;採用大孔樹脂吸附、水洗去雜質、乙醇水溶液洗脫有效成分的提取步驟,在保留有效成分的同時,去除了其中大部分的雜質。The above preparation method of the invention adopts a water extraction process to ensure that the water-soluble active ingredients, such as saikosaponin, berberine (berberine hydrochloride), baicalin, chrysophanol, paeoniflorin, synephrine, etc., are maximized. The extraction step of using the macroporous resin adsorption, water washing to remove impurities, and the aqueous solution of ethanol to elute the active ingredient, while retaining the active ingredient, removes most of the impurities.
採用上述製備方法,本發明的中藥組合物中有效成分的含量明顯提高,雜質的含量大大減少,從而減少了給藥的劑量,同時也保證了產品批次之間的穩定性。By adopting the above preparation method, the content of the active ingredient in the traditional Chinese medicine composition of the invention is obviously increased, the content of impurities is greatly reduced, thereby reducing the dosage of administration, and also ensuring the stability between product batches.
在本發明上述的方法三中,優選採用下述操作條件:1、在步驟(2)中,所用乙醇的濃度為75-90%,優選 為80%;優選回流提取兩次,每次用10倍於步驟(2)所述藥材重量的乙醇,每次提取1.5小時。In the above method 3 of the present invention, the following operating conditions are preferably employed: 1. In the step (2), the concentration of the ethanol used is 75-90%, preferably It is 80%; preferably, it is extracted twice under reflux, each time using 10 times the weight of the medicinal material of step (2), and each extraction is 1.5 hours.
2、在步驟(3)中,優選將上一步驟所得到的藥渣中加入其他藥材,用水回流提取兩次,每次水的用量為步驟(3)加入的其他藥材與步驟(2)得到的藥渣的重量之和的10倍,每次提取1.5小時。優選把提取液濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1。所加入的乙醇濃度優選為90-100%,進一步優選為95%,使濃縮液的含醇量達到65-75%,優選70%。2. In the step (3), it is preferred to add the other medicinal materials to the dregs obtained in the previous step, and extract twice with water, each time the amount of water is the other medicinal materials added in the step (3) and the step (2). The sum of the weights of the dregs is 10 times, each time for 1.5 hours. Preferably, the extract is concentrated to a ratio of the original medicinal weight (kg) to the volume (L) of the concentrate of 1:1. The concentration of ethanol added is preferably from 90 to 100%, further preferably 95%, so that the alcohol content of the concentrate reaches 65 to 75%, preferably 70%.
在本發明的上述製備方法中,柴胡、白芍、枳實、大黃、黃芩、黃連等生藥材先醇提,殘渣再與其他藥材合併水提,保證了這六味藥材有效成分得到充分提取;其他藥材僅用水提取其中的有效成分,這是因為其中的有效成分都是水溶性。採用本發明的上述方法使本發明的中藥組合物中的有效成分含量明顯提高,雜質含量大大減少,從而可減少給藥的劑量。In the above preparation method of the present invention, the raw materials such as Bupleurum, Radix Paeoniae Alba, Radix Paeoniae Alba, Rhubarb, Radix Astragali, Rhizoma Coptidis, etc. are firstly extracted, and the residue is combined with other herbs to extract water, thereby ensuring that the active ingredients of the six herbs are fully extracted. Other medicinal materials extract only the active ingredients therein by water because the active ingredients are water-soluble. By the above method of the present invention, the content of the active ingredient in the traditional Chinese medicine composition of the present invention is remarkably improved, and the content of impurities is greatly reduced, so that the dose to be administered can be reduced.
在本發明上述的方法四中,優選採用下述操作條件:1、步驟(2)中,優選用水回流提取兩次,每次用10倍於黃芩重量的水,每次1小時。保溫溫度優選為75-85℃,進一步優選為80℃。In the above method 4 of the present invention, the following operating conditions are preferably employed: 1. In the step (2), it is preferably extracted twice with water under reflux, each time using 10 times the weight of the xanthine, one hour each time. The holding temperature is preferably 75 to 85 ° C, and more preferably 80 ° C.
2、步驟(3)中,優選用乙醇回流提取兩次,每次用10倍於黃連重量的乙醇,每次2小時。所用乙醇的濃度優選為70-85%,進一步優選為75%。2. In step (3), it is preferably extracted twice with ethanol under reflux, each time using 10 times the weight of berberine in ethanol for 2 hours each time. The concentration of ethanol used is preferably from 70 to 85%, further preferably 75%.
步驟(2)和步驟(3)中,pH調節劑優選為濃鹽酸。In the step (2) and the step (3), the pH adjuster is preferably concentrated hydrochloric acid.
3、步驟(4)中,優選用水回流提取其餘藥材2次, 每次加10倍於步驟(4)中所述藥材重量的水,每次1小時。合併後的提取液濃縮至相對密度為1.03-1.07,優選為相對密度為1.05。回收乙醇後,將乙醇提取液濃縮至相對密度為1.25-1.35的浸膏,優選為相對密度為1.30。3. In step (4), it is preferred to extract the remaining medicinal materials twice with water, Add 10 times more water to the weight of the medicinal material in step (4) for 1 hour each time. The combined extracts are concentrated to a relative density of 1.03-1.07, preferably a relative density of 1.05. After recovering the ethanol, the ethanol extract is concentrated to an extract having a relative density of 1.25 to 1.35, preferably having a relative density of 1.30.
在本發明的上述方法中,將黃芩、黃連和其他藥材分別單獨提取,並根據其自身的性質分別在一定的pH值條件下進行水提或醇提,使本發明中藥組合物中的有效成分含量明顯提高,雜質含量大大減少,從而減少了給藥的劑量。In the above method of the present invention, the astragalus, berberine and other medicinal materials are separately extracted, and respectively subjected to water extraction or alcohol extraction under a certain pH condition according to their own properties, so as to make the active ingredient in the traditional Chinese medicine composition of the present invention. The content is significantly increased, and the amount of impurities is greatly reduced, thereby reducing the dose administered.
用本發明的上述方法可製備得到具有上述組成的、用於治療糖尿病的藥物組合物,本發明的藥物組合物可以採用中藥製劑的常規方法,使用本領域常規的輔料,製備成任何常規的製劑。例如將上述原料藥研成散劑沖服,或將製成的浸膏乾燥、粉碎、過篩後,研成散劑沖服,或將其製成片劑或膠囊口服,或者將其製成注射劑等。但是這些不能用於限制本發明的保護範圍。A pharmaceutical composition for treating diabetes having the above composition can be prepared by the above method of the present invention, and the pharmaceutical composition of the present invention can be prepared into any conventional preparation by a conventional method of a traditional Chinese medicine preparation using conventional excipients in the art. . For example, the above-mentioned raw material medicine is ground into a powder, or the prepared extract is dried, pulverized, sieved, ground into a powder, or it is made into a tablet or a capsule orally, or it is made into an injection or the like. However, these cannot be used to limit the scope of protection of the present invention.
用本發明的方法製備得到的藥物組合物具有降低血糖的作用,對糖尿病有良好的治療效果。The pharmaceutical composition prepared by the method of the present invention has a blood sugar lowering effect and has a good therapeutic effect on diabetes.
本文中,當用百分數描述乙醇濃度或含醇量(即體系中含有乙醇的量)時,如果沒有特別說明,是指體積百分比濃度或體積百分數。Herein, when the ethanol concentration or the alcohol content (that is, the amount of ethanol contained in the system) is described by a percentage, it means a volume percentage concentration or a volume percentage unless otherwise specified.
下面通過實施例和試驗例進一步說明本發明的藥物及其有益效果,但不以任何方式限制本發明的保護範圍。The drug of the present invention and its beneficial effects are further illustrated by the following examples and test examples, but are not intended to limit the scope of the present invention in any way.
藥物配方:天花粉750g、柴胡1500g、枳實450g、大黃150g、半夏150g、黃芩450g、黃連150g、白芍450g和烏梅750g。Drug formula: 750g of trichosanthin, 1500g of Bupleurum chinense, 450g of medlar, 150g of rhubarb, 150g of Pinellia, 450g of Radix Astragali, 150g of Rhizoma Coptidis, 450g of Radix Paeoniae and 750g of ebony.
按照下述方法製備本發明的藥物組合物:9味藥材用10倍於其重量的水回流提取2次,每次1.5小時,將提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入90%乙醇至含醇量65%,過濾,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 9-flavored medicinal material was extracted twice with water 10 times its weight under reflux for 1.5 hours, and the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal weight ( The ratio of the volume (L) of the kg) to the concentrate is 1:1, 90% ethanol is added to the alcohol content of 65%, filtered, and concentrated under reduced pressure to form a thick paste.
採用實施例1同樣的配方,用下述方法製備本發明的藥物組合物:將柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的75%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅和半夏,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入90%乙醇至含醇量65%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 1, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Rhizoma, Rhubarb, Astragalus, and Coptidis Rhizome were refluxed twice with 10 times the weight of 75% ethanol, 1.5 hours each time, the extract was filtered and set aside; the powder obtained in the previous step was added with trichosanthin, ebony and pinellia, and extracted twice with water of 10 times the sum of the weights of the herbs and the dregs, each time. 1.5 hours, the extract was concentrated under reduced pressure to a ratio of the original medicinal material weight (kg) to the volume (L) of the concentrate was 1:1, 90% ethanol was added to the alcohol content of 65%, filtered, and used; The liquid was mixed and concentrated under reduced pressure into a thick paste.
採用實施例1同樣的配方,用下述方法製備本發明的藥物組合物:以上9味藥材加水回流提取2次,每次加水48.5kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大 孔吸附樹脂,大孔吸附樹脂用量為3.2kg,上樣速度為4倍柱體積/小時。先用4倍柱體積的水洗脫,棄去水洗脫液,然後用2倍柱體積的80%乙醇洗脫,將醇洗脫液合併,80℃下減壓回收乙醇至相對密度為1.25,70℃真空乾燥,乾膏粉碎過80目篩。過篩後的乾粉中加入乳糖製成膠囊。Using the same formulation as in Example 1, the pharmaceutical composition of the present invention was prepared by the following method: The above 9 herbs were extracted twice with water and refluxed, and 48.5 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. Over the AB-8 type The pore adsorption resin, the macroporous adsorption resin was used in an amount of 3.2 kg, and the loading speed was 4 column volumes/hour. First elute with 4 column volumes of water, discard the water eluate, then elute with 2 column volumes of 80% ethanol, combine the alcohol eluates, and recover the ethanol to a relative density of 1.25 at 80 ° C under reduced pressure. It was dried under vacuum at 70 ° C, and the dry paste was pulverized through an 80 mesh sieve. The dried powder after sieving is added with lactose to form a capsule.
採用實施例1同樣的配方,用下述方法製備本發明的藥物組合物:將黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,75℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 1, the pharmaceutical composition of the present invention was prepared by the following method: adding 10 times its weight of water to the xanthine, and extracting it twice under reflux for 1 hour each time; combining the extracts, adding concentrated hydrochloric acid to adjust the pH value The mixture was kept at 1.5-2.0, 75 ° C for 1 hour, allowed to stand, filtered; the precipitate was washed with water to a pH of 5-6, dried, and the dried paste was pulverized through an 80 mesh sieve to obtain an extract of Astragalus membranaceus.
將黃連加10倍其重量的70%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗pH值至5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Add 10 times of its weight to 70% ethanol and reflux it twice for 2 hours each time; combine the extracts, filter, recover the ethanol to a non-alcoholic taste, add concentrated hydrochloric acid to adjust the pH to 1-2, refrigerate overnight, filter; The precipitate was washed with water to a pH of 5-6, dried, and the dried paste was pulverized through an 80 mesh sieve to obtain a Coptidis extract.
將其餘7味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.03,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.25,乾燥,乾膏粉碎過80目篩。The remaining 7 herbs were added with 10 times their weight of water and refluxed for 2 times each time for 1 hour; the extract was concentrated under reduced pressure to a relative density of 1.03, allowed to cool, and 95% ethanol was added to make the alcohol content 70%; After standing, filtering, ethanol was recovered to a relative density of 1.25, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,向其中加入乳糖製成膠囊。Take three kinds of extract dry powder, mix well, add lactose to it to make capsules.
藥物配方:天花粉1200g、柴胡900g、枳實450g、大黃180g、半夏360g、黃芩450g、黃連360g、白芍450g 和烏梅600g。Drug formula: 1200g of trichosanthin, 900g of Bupleurum, 450g of medlar, 180g of rhubarb, 360g of Pinellia, 450g of Radix Astragali, 360g of berberine, 450g of Radix And ebony 600g.
按照下述方法製備本發明的藥物組合物:9味藥材用10倍其重量的水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入無水乙醇至含醇量75%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 9-flavored medicinal material was extracted twice with 10 times its weight of water, 1.5 hours each time, the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal material weight (kg). The ratio of the volume (L) of the concentrate was 1:1, anhydrous ethanol was added to the alcohol content of 75%, filtered, and concentrated under reduced pressure to a thick paste.
採用實施例5同樣的配方,用下述方法製備本發明的藥物組合物:柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量90%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅和半夏,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入無水乙醇至含醇量75%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 5, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Poria, Rhubarb, Astragalus, and Coptidis Rhizome were extracted twice with 10 times their weight by 90% ethanol, each time. 1.5 hours, the extract was filtered and set aside; the powder obtained in the previous step was added with trichosanthin, ebony and pinellia, and extracted twice with water of 10 times the sum of the weight of the medicinal material and the dregs, 1.5 hours each time. The extract is concentrated under reduced pressure until the ratio of the original medicinal material weight (kg) to the volume (L) of the concentrated solution is 1:1, anhydrous ethanol is added to the alcohol content of 75%, filtered, and used; the two extracts are mixed. Concentrate under reduced pressure into a thick paste.
採用實施例5同樣的配方,用下述方法製備本發明的藥物組合物:以上9味藥材加水回流提取2次,每次加水49.5kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為1.7kg,上樣速度為6倍柱體積/小時。先用6倍柱體積的水洗脫,棄去水洗脫 液。然後用5倍柱體積的95%乙醇洗脫,將醇洗脫液合併,70℃下減壓回收乙醇至相對密度為1.35,90℃真空乾燥,乾膏粉碎過80目篩。Using the same formulation as in Example 5, the pharmaceutical composition of the present invention was prepared by the following method: The above 9 herbs were extracted twice with water and refluxed, and 49.5 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 1.7 kg and a loading speed of 6 column volumes per hour. First elute with 6 column volumes of water, discard water to elute liquid. Then, the mixture was eluted with 5 column volumes of 95% ethanol, and the alcohol eluate was combined. The ethanol was recovered under reduced pressure at 70 ° C to a relative density of 1.35, vacuum dried at 90 ° C, and the dry paste was pulverized through an 80 mesh sieve.
在所得到的乾膏中加入澱粉壓成片劑。Starch is compressed into tablets in the obtained dry paste.
採用實施例5同樣的配方,用下述方法製備本發明的藥物組合物:黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,85℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 5, the pharmaceutical composition of the present invention was prepared by the following method: xanthine was added with 10 times its weight of water, and refluxed twice for 1 hour each time; the extract was combined, and concentrated hydrochloric acid was added to adjust the pH to 1.5-2.0, incubated at 85 ° C for 1 hour, allowed to stand, filtered; the precipitate was washed with water to a pH of 5-6, dried, and the dry paste was pulverized through an 80 mesh sieve to obtain an extract of Astragalus membranaceus.
黃連加10倍其重量的85%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗pH值至5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Coptis added 10 times its weight of 85% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to no alcohol flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; The pH was washed with water to 5-6, dried, and the dry paste was pulverized through an 80 mesh sieve to obtain a Coptidis extract.
其餘7味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.07,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.35,乾燥,乾膏粉碎過80目篩。The remaining 7 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.07, allowed to cool, and 95% ethanol was added to make the alcohol content 70%; After filtration, the ethanol was recovered to a relative density of 1.35, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,向其中加入澱粉壓成片劑。Three kinds of extract dry powder were taken, mixed evenly, and starch was added thereto to compress into tablets.
藥物配方:天花粉630g、柴胡840g、枳實630g、大黃210g、半夏420g、黃芩630g、黃連420g、白芍630g和烏梅630g。Drug formula: 630g of trichosanthin, 840g of Bupleurum, 630g of medlar, 210g of rhubarb, 420g of Pinellia, 630g of astragalus, 420g of Rhizoma coptiflora, 630g of Radix Paeoniae Alba and 630g of ebony.
按照下述方法製備本發明的藥物組合物:9味藥材用10倍其重量水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入95%乙醇至含醇量70%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 9-flavored medicinal materials were extracted twice with 10 times the weight of water and refluxed for 1.5 hours each time, the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal material weight (kg) and The volume ratio (L) of the concentrate was 1:1, 95% ethanol was added to the alcohol content of 70%, filtered, and concentrated under reduced pressure to a thick paste.
採用實施例9同樣的配方,用下述方法製備本發明的藥物組合物:柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的80%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅和半夏,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入95%乙醇至含醇量70%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 9, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Poria, Rhubarb, Astragalus, and Coptidis Rhizome were refluxed twice with 10 times the weight of 80% ethanol, each time. 1.5 hours after the extraction, the extract was filtered and set aside; the powder obtained in the previous step was added with trichosanthin, ebony and pinellia, and extracted with water 10 times the sum of the weight of the medicinal material and the dregs twice, 1.5 times each time. In an hour, the extract is concentrated under reduced pressure until the ratio of the original medicinal material weight (kg) to the volume (L) of the concentrate is 1:1, 95% ethanol is added to the alcohol content 70%, filtered, and used; Mix and concentrate under reduced pressure into a thick paste.
採用實施例9同樣的配方,用下述方法製備本發明的藥物組合物:以上9味藥材加水回流提取2次,每次加水50.4kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為2.52kg,上樣速度為5倍柱體積/小時。先用5倍柱體積的水洗脫。水洗脫液棄去。然後用3倍柱體積的90%乙醇洗脫,將醇洗脫液合併, 70℃下減壓回收乙醇至相對密度為1.30,80℃真空乾燥,乾膏粉碎過80目篩。Using the same formulation as in Example 9, the pharmaceutical composition of the present invention was prepared by the following method: the above 9 herbs were refluxed twice with water, and 50.4 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 2.52 kg and a loading speed of 5 column volumes per hour. First elute with 5 column volumes of water. The water eluate was discarded. The alcohol eluate was then combined by eluting with 3 column volumes of 90% ethanol. The ethanol was recovered under reduced pressure at 70 ° C to a relative density of 1.30, vacuum dried at 80 ° C, and the dry paste was pulverized through an 80 mesh sieve.
在所得到的乾膏中加入微晶纖維素製成濃縮丸。A concentrated pellet was prepared by adding microcrystalline cellulose to the obtained dry paste.
採用實施例9同樣的配方,用下述方法製備本發明的藥物組合物:黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,80℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 9, the pharmaceutical composition of the present invention was prepared by the following method: xanthine was added with 10 times its weight of water, and refluxed twice for 1 hour each time; the extract was combined, and concentrated hydrochloric acid was added to adjust the pH to 1.5-2.0, incubate at 80 ° C for 1 hour, let stand, filter; the precipitate is washed with water to a pH of 5-6, dried, and the dry paste is crushed through a 80 mesh sieve to obtain an extract of Astragalus membranaceus.
黃連加10倍其重量的75%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Coptis added 10 times its weight of 75% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to no alcohol flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; Wash with water to a pH of 5-6, dry, and dry the paste through a 80 mesh sieve to obtain the extract of Coptidis Rhizoma.
其餘7味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.05,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.30,乾燥,乾膏粉碎過80目篩。The remaining 7 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.05, allowed to cool, and 95% ethanol was added to make the alcohol content 70%; The solution was filtered, and the ethanol was recovered to a relative density of 1.30, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,加入微晶纖維素製成濃縮丸。Take three kinds of extract dry powder, mix well, add microcrystalline cellulose to make concentrated pellets.
藥物配方:天花粉750g、柴胡1500g、枳實450g、大黃150g、半夏150g、黃芩450g、黃連150g、白芍450g、烏梅750g和山楂450g。Drug formula: 750g of trichosanthin, 1500g of Bupleurum chinense, 450g of medlar, 150g of rhubarb, 150g of Pinellia, 450g of astragalus, 150g of berberine, 450g of white peony, 750g of ebony and 450g of hawthorn.
按照下述方法製備本發明的藥物組合物: 10味藥材用10倍其重量水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入90%乙醇至含醇量65%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention is prepared as follows: The 10 herbs were extracted twice with 10 times the weight of water and refluxed for 1.5 hours each time. The extract was filtered, and the extract was concentrated under reduced pressure until the ratio of the original drug weight (kg) to the volume (L) of the concentrate was 1: 1. Add 90% ethanol to 65% alcohol content, filter, and concentrate to a thick paste under reduced pressure.
採用實施例13同樣的配方,用下述方法製備本發明的藥物組合物:柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的75%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅、半夏和山楂,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入90%乙醇至含醇量65%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 13, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Poria, Rhubarb, Astragalus, and Coptis were refluxed twice with 10 times the weight of 75% ethanol, each time. 1.5 hours after the extraction, the extract was filtered and set aside; the powder obtained in the previous step was added with trichosanthin, ebony, pinellia and hawthorn, and extracted twice with water 10 times the sum of the weight of the medicinal material and the dregs. 1.5 hours after the extraction, the extract was concentrated under reduced pressure to a ratio of the original medicinal material weight (kg) to the volume (L) of the concentrate was 1:1, 90% ethanol was added to the alcohol content of 65%, filtered, and set aside; The extract was mixed and concentrated under reduced pressure into a thick paste.
採用實施例13同樣的配方,用下述方法製備本發明的藥物組合物:以上10味藥材加水回流提取2次,每次加水52.5kg,每次1小時。將將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為3.5kg,上樣速度為4倍柱體積/小時。先用4倍柱體積的水洗脫。水洗脫液棄去。然後用2倍柱體積的80%乙醇洗脫,將醇洗脫液合併,80℃下減壓回收乙醇至相對密度為1.35,70℃真空乾燥, 乾膏粉碎過80目篩。Using the same formulation as in Example 13, the pharmaceutical composition of the present invention was prepared by the following method: The above 10 herbs were refluxed twice with water, and 52.5 kg of water was added each time for 1 hour. The extract will be allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 3.5 kg and a loading speed of 4 column volumes per hour. First elute with 4 column volumes of water. The water eluate was discarded. Then, the mixture was eluted with 2 column volumes of 80% ethanol, and the alcohol eluate was combined. The ethanol was recovered under reduced pressure at 80 ° C to a relative density of 1.35, and vacuum dried at 70 ° C. The dry paste is pulverized through an 80 mesh sieve.
在所得到的乾膏中加入乳糖製成膠囊。Lactose was added to the obtained dry paste to prepare a capsule.
採用實施例13同樣的配方,用下述方法製備本發明的藥物組合物:黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,75℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 13, the pharmaceutical composition of the present invention was prepared by the following method: xanthine was added with 10 times its weight of water, and refluxed twice for 1 hour each time; the extract was combined, and concentrated hydrochloric acid was added to adjust the pH to 1.5-2.0, 75 ° C for 1 hour, standing, filtered; the precipitate was washed with water to a pH of 5-6, dried, and the dry paste was crushed through a 80 mesh sieve to obtain the Astragalus membranaceus extract.
黃連加10倍其重量的70%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。其餘8味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.07,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.25,乾燥,乾膏粉碎過80目篩。取三種提取物乾粉,混合均勻,加入乳糖製成膠囊。Coptis plus 10 times its weight of 70% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to a non-alcoholic flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; Wash with water to a pH of 5-6, dry, and dry the paste through a 80 mesh sieve to obtain the extract of Coptidis Rhizoma. The remaining 8 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.07, allowed to cool, and 95% ethanol was added to make the alcohol content 70%; The solution was filtered, and ethanol was recovered to a relative density of 1.25, dried, and the dry paste was pulverized through an 80 mesh sieve. Take three kinds of extract dry powder, mix well, add lactose to make capsules.
藥物配方:天花粉1200g、柴胡900g、枳實450g、大黃180g、半夏360g、黃芩450g、黃連360g、白芍450g、烏梅600g和山楂450g。Drug formula: 1200g of trichosanthin, 900g of Bupleurum, 450g of medlar, 180g of rhubarb, 360g of Pinellia, 450g of Radix, 360g of berberine, 450g of white peony, 600g of ebony and 450g of hawthorn.
按照下述方法製備本發明的藥物組合物:10味藥材用10倍其重量水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量 (kg)和濃縮液的體積(L)之比為1:1,加入無水乙醇至含醇量75%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 10 kinds of medicinal materials were extracted twice with 10 times the weight of water and refluxed for 1.5 hours each time, the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal weight. The ratio of (kg) to the volume (L) of the concentrate was 1:1, anhydrous ethanol was added to an alcohol content of 75%, filtered, and concentrated under reduced pressure to a thick paste.
採用實施例17同樣的配方,用下述方法製備本發明的藥物組合物:柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的90%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅、半夏和山楂,用10倍於所述藥材和藥渣重量之和的水回流提取2次每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入無水乙醇至含醇量75%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 17, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Poria, Rhubarb, Astragalus, and Coptis were refluxed twice with 10 times the weight of 90% ethanol, each time. After 1.5 hours, the extract was filtered and set aside; the powder obtained in the previous step was added with trichosanthin, ebony, pinellia and hawthorn, and extracted twice with water of 10 times the sum of the weights of the herbs and the dregs. 1.5 hours, the extract was concentrated under reduced pressure to a ratio of the original medicinal weight (kg) to the volume (L) of the concentrate was 1:1, anhydrous ethanol was added to the alcohol content of 75%, filtered, and used; Mix and concentrate under reduced pressure into a thick paste.
採用實施例17同樣的配方,用下述方法製備本發明的藥物組合物:以上10味藥材加水回流提取2次,每次加水54kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為1.8kg,上樣速度為6倍柱體積/小時。先用6倍柱體積的水洗脫。水洗脫液棄去。然後用5倍柱體積的95%乙醇洗脫,將醇洗脫液合併,70℃下減壓回收乙醇至相對密度為1.25,90℃真空乾燥,乾膏粉碎過80目篩。Using the same formulation as in Example 17, the pharmaceutical composition of the present invention was prepared by the following method: The above 10 herbs were refluxed twice with water, and 54 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 1.8 kg and a loading speed of 6 column volumes per hour. First elute with 6 column volumes of water. The water eluate was discarded. Then, it was eluted with 5 column volumes of 95% ethanol, the alcohol eluates were combined, and ethanol was recovered under reduced pressure at 70 ° C to a relative density of 1.25, dried at 90 ° C under vacuum, and the dry paste was pulverized through an 80 mesh sieve.
在所得到的乾膏中加入乳糖製成膠囊。Lactose was added to the obtained dry paste to prepare a capsule.
採用實施例17同樣的配方,用下述方法製備本發明的藥物組合物:黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,80℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 17, the pharmaceutical composition of the present invention was prepared by the following method: xanthine was added with 10 times its weight of water, and refluxed twice for 1 hour each time; the extract was combined, and concentrated hydrochloric acid was added to adjust the pH to 1.5-2.0, incubate at 80 ° C for 1 hour, let stand, filter; the precipitate is washed with water to a pH of 5-6, dried, and the dry paste is crushed through a 80 mesh sieve to obtain an extract of Astragalus membranaceus.
黃連加10倍其重量的70%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Coptis plus 10 times its weight of 70% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to a non-alcoholic flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; Wash with water to a pH of 5-6, dry, and dry the paste through a 80 mesh sieve to obtain the extract of Coptidis Rhizoma.
其餘8味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.03,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.35,乾燥,乾膏粉碎過80目篩。The remaining 8 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.03, allowed to cool, and 95% ethanol was added to make the alcohol content 70%; After filtration, the ethanol was recovered to a relative density of 1.35, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,加入乳糖製成膠囊。Take three kinds of extract dry powder, mix well, add lactose to make capsules.
藥物配方:天花粉833g、柴胡667g、枳實500g、大黃167g、半夏333g、黃芩500g、黃連333g、白芍500g、烏梅833g和山楂500g。Drug formula: 833g of trichosanthin, 667g of Bupleurum chinense, 500g of medlar, 167g of rhubarb, 333g of Pinellia ternata, 500g of Radix Astragali, 333g of Rhizoma Coptidis, 500g of Radix Paeoniae, 833g of ebony and 500g of Hawthorn.
按照下述方法製備本發明的藥物組合物:10味藥材用10倍其重量水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入95%乙醇至含醇量70%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 10 kinds of medicinal materials were extracted twice with 10 times the weight of water and refluxed for 1.5 hours each time, the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal material weight (kg) and The volume ratio (L) of the concentrate was 1:1, 95% ethanol was added to the alcohol content of 70%, filtered, and concentrated under reduced pressure to a thick paste.
採用實施例21同樣的配方,用下述方法製備本發明的藥物組合物:柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的80%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅、半夏和山楂,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入95%乙醇至含醇量70%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 21, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Poria, Rhubarb, Astragalus, and Coptis were refluxed twice with 10 times the weight of 80% ethanol, each time. 1.5 hours after the extraction, the extract was filtered and set aside; the powder obtained in the previous step was added with trichosanthin, ebony, pinellia and hawthorn, and extracted twice with water 10 times the sum of the weight of the medicinal material and the dregs. 1.5 hours after the hour, the extract was concentrated under reduced pressure to a ratio of the original medicinal material weight (kg) to the volume (L) of the concentrate was 1:1, 95% ethanol was added to the alcohol content 70%, filtered, and used; The extract was mixed and concentrated under reduced pressure into a thick paste.
採用實施例21同樣的配方,用下述方法製備本發明的藥物組合物:以上10味藥材加水回流提取2次,每次加水51.7kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為2.6kg,上樣速度為5倍柱體積/小時。先用5倍柱體積的水洗脫。水洗脫液棄去。然後用3倍柱體積的90%乙醇洗脫,將醇洗脫液合併,70℃下減壓回收乙醇至相對密度為1.30,80℃真空乾燥,乾膏粉碎過80目篩。Using the same formulation as in Example 21, the pharmaceutical composition of the present invention was prepared by the following method: The above 10 herbs were refluxed twice with water, and 51.7 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 2.6 kg and a loading speed of 5 column volumes per hour. First elute with 5 column volumes of water. The water eluate was discarded. Then, the mixture was eluted with 3 column volumes of 90% ethanol, and the alcohol eluate was combined. The ethanol was recovered under reduced pressure at 70 ° C to a relative density of 1.30, vacuum dried at 80 ° C, and the dry paste was pulverized through an 80 mesh sieve.
在所得到的乾膏中加入微晶纖維素製成濃縮丸。A concentrated pellet was prepared by adding microcrystalline cellulose to the obtained dry paste.
採用實施例21同樣的配方,用下述方法製備本發明的 藥物組合物:黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,80℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 21, the present invention was prepared by the following method. Pharmaceutical composition: Astragalus plus 10 times its weight of water, reflux extraction twice, each time 1 hour; combined extract, concentrated hydrochloric acid to adjust the pH to 1.5-2.0, 80 ° C for 1 hour, let stand, filtered; precipitation Wash with water to a pH of 5-6, dry, and pulverize the dry paste through an 80 mesh sieve to obtain an Astragalus membranaceus extract.
黃連加10倍其重量的75%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Coptis added 10 times its weight of 75% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to no alcohol flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; Wash with water to a pH of 5-6, dry, and dry the paste through a 80 mesh sieve to obtain the extract of Coptidis Rhizoma.
其餘8味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.05,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.30,乾燥,乾膏粉碎過80目篩。The remaining 8 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.05, let cool, and 95% ethanol was added to make the alcohol content 70%; The solution was filtered, and the ethanol was recovered to a relative density of 1.30, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,加入微晶纖維素製成濃縮丸。Take three kinds of extract dry powder, mix well, add microcrystalline cellulose to make concentrated pellets.
藥物配方:天花粉500g、柴胡750g、枳實500g、大黃250g、半夏500g份、黃芩500g、黃連500g、白芍500g、烏梅500g和山楂500g。Drug formula: 500g of trichosanthin, 750g of Bupleurum chinense, 500g of medlar, 250g of rhubarb, 500g of Pinellia, 500g of Radix Scutellariae, 500g of Rhizoma Coptidis, 500g of Radix Paeoniae Alba, 500g of ebony, 500g of Hawthorn and 500g of Hawthorn.
按照下述方法製備本發明的藥物組合物:10味藥材用10倍其重量水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入95%乙醇至含醇量70%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 10 kinds of medicinal materials were extracted twice with 10 times the weight of water and refluxed for 1.5 hours each time, the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal material weight (kg) and The volume ratio (L) of the concentrate was 1:1, 95% ethanol was added to the alcohol content of 70%, filtered, and concentrated under reduced pressure to a thick paste.
採用實施例25同樣的配方,用下述方法製備本發明的藥物組合物:柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的80%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅、半夏和山楂,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入95%乙醇至含醇量70%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 25, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Poria, Rhubarb, Astragalus, and Coptis were refluxed twice with 10 times the weight of 80% ethanol, and each was extracted twice. 1.5 hours after the extraction, the extract was filtered and set aside; the powder obtained in the previous step was added with trichosanthin, ebony, pinellia and hawthorn, and extracted twice with water 10 times the sum of the weight of the medicinal material and the dregs. 1.5 hours after the hour, the extract was concentrated under reduced pressure to a ratio of the original medicinal material weight (kg) to the volume (L) of the concentrate was 1:1, 95% ethanol was added to the alcohol content 70%, filtered, and used; The extract was mixed and concentrated under reduced pressure into a thick paste.
採用實施例25同樣的配方,用下述方法製備本發明的藥物組合物:以上10味藥材加水回流提取2次,每次加水50kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為2.5kg,上樣速度為4倍柱體積/小時。先用5倍柱體積的水洗脫。水洗脫液棄去。然後用4倍柱體積的92%乙醇洗脫,將醇洗脫液合併,75℃下減壓回收乙醇至相對密度為1.25,85℃真空乾燥,乾膏粉碎過80目篩。Using the same formulation as in Example 25, the pharmaceutical composition of the present invention was prepared by the following method: The above 10 flavored herbs were refluxed twice with water, and 50 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 2.5 kg and a loading speed of 4 column volumes per hour. First elute with 5 column volumes of water. The water eluate was discarded. Then, the alcohol eluate was eluted with 4 column volumes of 92% ethanol, and the ethanol was recovered under reduced pressure at 75 ° C to a relative density of 1.25, vacuum dried at 85 ° C, and the dry paste was pulverized through an 80 mesh sieve.
在所得到的乾膏中加入糊精製成片劑。A dextrin was added to the obtained dry paste to prepare a tablet.
採用實施例25同樣的配方,用下述方法製備本發明的藥物組合物: 黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,85℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 25, the pharmaceutical composition of the present invention was prepared by the following method: Add 10 times its weight of water to the scutellariae and extract twice by reflux for 1 hour. Combine the extract, add concentrated hydrochloric acid to adjust the pH to 1.5-2.0, incubate at 85 ° C for 1 hour, let stand, filter; wash the precipitate with water to pH The value is 5-6, dried, and the dry paste is pulverized through an 80 mesh sieve to obtain an extract of Astragalus membranaceus.
黃連加10倍其重量的85%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Coptis added 10 times its weight of 85% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to no alcohol flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; Wash with water to a pH of 5-6, dry, and dry the paste through a 80 mesh sieve to obtain the extract of Coptidis Rhizoma.
其餘8味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.05,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.25,乾燥,乾膏粉碎過80目篩。The remaining 8 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.05, let cool, and 95% ethanol was added to make the alcohol content 70%; The solution was filtered, and ethanol was recovered to a relative density of 1.25, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,加入糊精製成片劑。Take three kinds of extract dry powder, mix well, add dextrin to make tablets.
藥物配方:天花粉1200g、柴胡800g、枳實600g、大黃200g、半夏400g、黃芩400g、黃連200g、白芍400g、烏梅400g和山楂400g。Drug formula: 1200g of trichosanthin, 800g of Bupleurum chinense, 600g of medlar, 200g of rhubarb, 400g of Pinellia ternata, 400g of Radix Scutellariae, 200g of Rhizoma Coptidis, 400g of Radix Paeoniae Alba, 400g of ebony, 400g of Hawthorn and 400g of Hawthorn.
按照下述方法製備本發明的藥物組合物:10味藥材用10倍其重量水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入90%乙醇至含醇量68%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 10 kinds of medicinal materials were extracted twice with 10 times the weight of water and refluxed for 1.5 hours each time, the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal material weight (kg) and The volume ratio (L) of the concentrate was 1:1, 90% ethanol was added to the alcohol content of 68%, filtered, and concentrated under reduced pressure to a thick paste.
採用實施例29同樣的配方,用下述方法製備本發明的藥物組合物: 柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的85%乙醇回流提取2次,每次1.5小時,提取液濾過,備用;在上一步驟得到的藥渣中加入天花粉、烏梅、半夏和山楂,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入90%乙醇至含醇量68%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 29, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Radix Paeoniae Alba, Radix Paeoniae Alba, Rhubarb, Radix Astragali, Rhizoma Coptidis, and 10% by weight of 85% ethanol were refluxed twice for 1.5 hours each time. The extract was filtered and used; added to the dregs obtained in the previous step. Trichosanthin, ebony, pinellia and hawthorn, extracted twice with water 10 times the sum of the weight of the medicinal material and the dregs, 1.5 hours each time, the extract was concentrated under reduced pressure to the original medicinal material weight (kg) and concentrated. The volume (L) ratio of the liquid was 1:1, 90% ethanol was added to the alcohol content of 68%, filtered, and set aside; the two extracts were mixed and concentrated under reduced pressure to form a thick paste.
採用實施例29同樣的配方,用下述方法製備本發明的藥物組合物:以上10味藥材加水回流提取2次,每次加水50kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為2.0kg,上樣速度為6倍柱體積/小時。先用4倍柱體積的水洗脫。水洗脫液棄去。然後用3倍柱體積的92%乙醇洗脫,將醇洗脫液合併,65℃下減壓回收乙醇至相對密度為1.30,75℃真空乾燥,乾膏粉碎過80目篩。Using the same formulation as in Example 29, the pharmaceutical composition of the present invention was prepared by the following method: The above 10 medicinal materials were refluxed twice with water, and 50 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 2.0 kg and a loading speed of 6 column volumes per hour. First elute with 4 column volumes of water. The water eluate was discarded. Then, it was eluted with 3 column volumes of 92% ethanol, and the alcohol eluates were combined. The ethanol was recovered under reduced pressure at 65 ° C to a relative density of 1.30, vacuum dried at 75 ° C, and the dry paste was pulverized through an 80 mesh sieve.
在所得到的乾膏中加入乳糖製成膠囊劑。A lactose is added to the obtained dry paste to prepare a capsule.
採用實施例29同樣的配方,用下述方法製備本發明的藥物組合物:黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,75℃保溫1小 時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 29, the pharmaceutical composition of the present invention was prepared by the following method: xanthine was added with 10 times its weight of water, and refluxed twice for 1 hour each time; the extract was combined, and concentrated hydrochloric acid was added to adjust the pH to 1.5-2.0, 75 ° C insulation 1 small At the same time, it was allowed to stand and filtered; the precipitate was washed with water to a pH of 5-6, dried, and the dried paste was pulverized through an 80 mesh sieve to obtain an extract of Astragalus membranaceus.
黃連加10倍其重量的75%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Coptis added 10 times its weight of 75% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to no alcohol flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; Wash with water to a pH of 5-6, dry, and dry the paste through a 80 mesh sieve to obtain the extract of Coptidis Rhizoma.
其餘8味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.05,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.35,乾燥,乾膏粉碎過80目篩。The remaining 8 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.05, let cool, and 95% ethanol was added to make the alcohol content 70%; After filtration, the ethanol was recovered to a relative density of 1.35, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,加入乳糖製成膠囊劑。Take three kinds of extract dry powder, mix well, add lactose to make capsules.
藥物配方:天花粉1000g、柴胡600g、枳實600g、大黃250g、半夏300g、黃芩500g、黃連300g、白芍500g、烏梅500g和山楂300g。Drug formula: 1000g of trichosanthin, 600g of Bupleurum chinense, 600g of medlar, 250g of rhubarb, 300g of Pinellia, 500g of Radix Scutellariae, 300g of Rhizoma Coptidis, 500g of Radix Paeoniae Alba, 500g of ebony, and 300g of Hawthorn.
按照下述方法製備本發明的藥物組合物:10味藥材用10倍其重量水回流提取2次,每次1.5小時,提取液濾過,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入99%乙醇至含醇量74%,濾過,減壓濃縮成稠膏。The pharmaceutical composition of the present invention was prepared according to the following method: 10 kinds of medicinal materials were extracted twice with 10 times the weight of water and refluxed for 1.5 hours each time, the extract was filtered, and the extract was concentrated under reduced pressure to the original medicinal material weight (kg) and The volume (L) ratio of the concentrate was 1:1, 99% ethanol was added to an alcohol content of 74%, filtered, and concentrated under reduced pressure to a thick paste.
採用實施例33同樣的配方,用下述方法製備本發明的藥物組合物:柴胡、白芍、枳實、大黃、黃芩、黃連用10倍其重量的90%乙醇回流提取2次,每次1.5小時,提取液濾過, 備用;在上一步驟得到的藥渣中加入天花粉、烏梅、半夏和山楂,用10倍於所述藥材和藥渣重量之和的水回流提取2次,每次1.5小時,將提取液減壓濃縮至最初的藥材重量(kg)和濃縮液的體積(L)之比為1:1,加入99%乙醇至含醇量74%,濾過,備用;將兩提取液混合,減壓濃縮成稠膏。Using the same formulation as in Example 33, the pharmaceutical composition of the present invention was prepared by the following method: Bupleurum, Angelica, Poria, Rhubarb, Astragalus, and Coptidis Rhizome were refluxed twice with 10 times the weight of 90% ethanol, each time 1.5 hours later, the extract was filtered, In the dregs obtained in the previous step, adding the pollen, ebony, pinellia and hawthorn, and extracting twice with water of 10 times the sum of the weights of the herbs and the dregs, 1.5 times each time, the extract is reduced. The pressure is concentrated to a ratio of the original drug weight (kg) to the volume (L) of the concentrate is 1:1, 99% ethanol is added to the alcohol content 74%, filtered, and used; the two extracts are mixed and concentrated under reduced pressure. Thick cream.
採用實施例33同樣的配方,用下述方法製備本發明的藥物組合物:以上10味藥材加水回流提取2次,每次加水48.5kg,每次1小時。將提取液放涼,過濾,合併。過AB-8型大孔吸附樹脂,大孔吸附樹脂用量為1.7kg,上樣速度為5倍柱體積/小時。先用4倍柱體積的水洗脫。水洗脫液棄去。然後用5倍柱體積的85%乙醇洗脫,將醇洗脫液合併,70℃下減壓回收乙醇至相對密度為1.35,90℃真空乾燥,乾膏粉碎過80目篩。Using the same formulation as in Example 33, the pharmaceutical composition of the present invention was prepared by the following method: The above 10 herbs were refluxed twice with water, and 48.5 kg of water was added each time for 1 hour. The extract was allowed to cool, filtered and combined. The AB-8 type macroporous adsorption resin has a macroporous adsorption resin dosage of 1.7 kg and a loading speed of 5 column volumes per hour. First elute with 4 column volumes of water. The water eluate was discarded. Then, the mixture was eluted with 5 column volumes of 85% ethanol, and the alcohol eluate was combined. The ethanol was recovered under reduced pressure at 70 ° C to a relative density of 1.35, dried at 90 ° C under vacuum, and the dry paste was pulverized through an 80 mesh sieve.
在所得到的乾膏中加入乳糖製成膠囊劑。A lactose is added to the obtained dry paste to prepare a capsule.
採用實施例33同樣的配方,用下述方法製備本發明的藥物組合物:黃芩加10倍其重量的水,回流提取兩次,每次1小時;合併提取液,加濃鹽酸調pH值至1.5-2.0,80℃保溫1小時,靜置,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃芩提取物。Using the same formulation as in Example 33, the pharmaceutical composition of the present invention was prepared by the following method: xanthine was added with 10 times its weight of water, and refluxed twice for 1 hour each time; the extract was combined, and concentrated hydrochloric acid was added to adjust the pH to 1.5-2.0, incubate at 80 ° C for 1 hour, let stand, filter; the precipitate is washed with water to a pH of 5-6, dried, and the dry paste is crushed through a 80 mesh sieve to obtain an extract of Astragalus membranaceus.
黃連加10倍其重量的80%乙醇回流提取兩次,每次2小時;合併提取液,濾過,回收乙醇至無醇味,加入濃鹽酸調pH值至1-2,冷藏過夜,濾過;沈澱用水洗至pH值5-6,乾燥,乾膏粉碎過80目篩,得黃連提取物。Coptis plus 10 times its weight of 80% ethanol reflux extraction twice, each time 2 hours; combined extract, filtered, recovered ethanol to no alcohol flavor, added concentrated hydrochloric acid to adjust the pH to 1-2, refrigerated overnight, filtered; Wash with water to a pH of 5-6, dry, and dry the paste through a 80 mesh sieve to obtain the extract of Coptidis Rhizoma.
其餘8味藥材加10倍其重量的水回流提取2次,每次1小時;提取液合併減壓濃縮至相對密度為1.05,放涼,加入95%乙醇,使含醇量為70%;靜置,濾過,回收乙醇至相對密度為1.30,乾燥,乾膏粉碎過80目篩。The remaining 8 herbs were added with 10 times their weight of water for 2 times, one hour each time; the extract was concentrated under reduced pressure to a relative density of 1.05, let cool, and 95% ethanol was added to make the alcohol content 70%; The solution was filtered, and the ethanol was recovered to a relative density of 1.30, dried, and the dry paste was pulverized through an 80 mesh sieve.
取三種提取物乾粉,混合均勻,加入乳糖製成膠囊劑。Take three kinds of extract dry powder, mix well, add lactose to make capsules.
1)實驗動物:SPF級雄性SD大鼠,60只,體重200-220g。1) Experimental animals: SPF male SD rats, 60, weighing 200-220 g.
2)主要試劑、藥品和儀器:鏈脲佐菌素(Streptozotocin、STZ):美國sigma公司,批號024K1211;無水檸檬酸(C6 H8 O7 ·H2 O):天津化學試劑一廠,批號011121;檸檬酸鈉(Na3 C6 H5 07 .2H2 O):天津化學試劑一廠,批號011219;二甲雙胍:250mg/片,天津太平洋制藥有限公司生產,批號040121;試驗例的不同處方組藥物分別為按照實施例3、實施例8和實施例9製備的浸膏粉,編號分別為TL-1,TL-2和TL-3。2) Main reagents, drugs and instruments: Streptozotocin (STZ): American sigma company, batch number 024K1211; anhydrous citric acid (C 6 H 8 O 7 · H 2 O): Tianjin Chemical Reagent No. 1 Plant, batch number 011121; sodium citrate (Na 3 C 6 H 5 0 7 .2H 2 O): Tianjin Chemical Reagent No. 1 Plant, batch No. 011219; metformin: 250mg/tablet, produced by Tianjin Pacific Pharmaceutical Co., Ltd., batch number 040121; different test cases The prescription group drugs were the extract powders prepared according to Example 3, Example 8 and Example 9, respectively, and were numbered TL-1, TL-2 and TL-3, respectively.
穩毫型血糖儀(One-Touch Ultra):美國Lifescan公司,註 冊號20032400735。One-Touch Ultra: Lifescan, USA Book number 20032400735.
3)模型製備:SD大鼠適應1周後隔夜禁食,經腹腔注射STZ 65mg/kg(0.1mmol/l、pH4.4檸檬酸緩衝液製成2%(W/V)的溶液),3天後尾靜脈取血測血糖16.7mmol/L為造模成功。3) Model preparation: SD rats were conditioned for 1 week and fasted overnight. After intraperitoneal injection of STZ 65 mg/kg (0.1 mmol/l, pH 4.4 citrate buffer to make 2% (W/V) solution), 3 Taking blood from the tail vein to measure blood sugar 16.7mmol/L was successful in modeling.
4)給藥方法及觀察指標:成模的糖尿病大鼠隨機分成模型組、二甲雙胍125mg/kg組和不同處方組(用藥量相當於生藥15.5g/kg)。適應一周,檢測血糖後灌胃給藥,每日一次,藥物皆用生理鹽水配製成混懸液給藥,實驗期間皆自由攝食飲水,實驗周期15天。在給藥第7、14天,給藥後禁食2小時,尾靜脈取血one-touch ultra血糖儀測定血糖,同時檢測大鼠的體重。4) Administration method and observation index: The modeled diabetic rats were randomly divided into a model group, metformin 125 mg/kg group and different prescription groups (the dosage was equivalent to 15.5 g/kg of crude drug). After one week of treatment, the blood glucose was administered by intragastric administration once a day, and the drugs were administered with physiological saline to prepare a suspension. During the experiment, the drinking water was freely taken for 15 days. On the 7th and 14th day after the administration, the rats were fasted for 2 hours after the administration, and blood glucose was measured by a one-touch ultra blood glucose meter in the tail vein, and the body weight of the rats was simultaneously measured.
5)統計學處理:實驗數據用均數±標準差(±SD )表示,兩組間差異顯著性採用t檢驗。5) Statistical processing: experimental data with mean ± standard deviation ( ± SD ) indicates that the significance of the difference between the two groups was measured by t test.
6)結果由表1可見,不同處方組在用藥量相當於生藥15.5g/kg劑量時,給藥7、14天後,均使STZ高血糖大鼠的血糖明顯下降(P<0.01)。6) The results are shown in Table 1. When the dosage of the different prescription groups was equivalent to the dose of 15.5 g/kg of the crude drug, the blood glucose of the STZ hyperglycemic rats was significantly decreased after 7 and 14 days of administration (P<0.01).
表1.各組血糖的變化及比較(±SD
n=10)
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