CN100542597C - A preparation process and application of traditional Chinese medicine for treating symptoms of vocal cord nodules and vocal cord polyps - Google Patents

A preparation process and application of traditional Chinese medicine for treating symptoms of vocal cord nodules and vocal cord polyps Download PDF

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CN100542597C
CN100542597C CNB2006100431084A CN200610043108A CN100542597C CN 100542597 C CN100542597 C CN 100542597C CN B2006100431084 A CNB2006100431084 A CN B2006100431084A CN 200610043108 A CN200610043108 A CN 200610043108A CN 100542597 C CN100542597 C CN 100542597C
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黄小华
付彬
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BEILIN PHARMACEUTICAL Co Ltd XI'AN
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Abstract

本发明涉及一种中药制剂的制备工艺及其用途,特别是涉及一种治疗声带小结、声带息肉症状的中药制备工艺及其用途。本发明目的在于提供一种治疗声带小结、声带息肉症状的中药制剂的制备工艺。本发明另一目的在于提供在治疗声带小结、声带息肉的药物中的应用。本发明的制备工艺其工艺稳定、可行,成品的绿原酸含量比原工艺高,提高了原料的利用率、有效成分的提取率;本发明具有活血化淤功能,可降低全血粘度、血浆粘度、全血还原粘度、血纤维蛋白原含量和血小板附率;对慢性炎症肉芽组织增生具有抑制作用。The invention relates to a preparation process and application of a traditional Chinese medicine preparation, in particular to a preparation process and application of a traditional Chinese medicine for treating symptoms of vocal nodules and vocal cord polyps. The purpose of the invention is to provide a preparation process of a traditional Chinese medicine preparation for treating symptoms of vocal cord nodules and vocal cord polyps. Another object of the present invention is to provide the application in medicine for treating vocal cord nodules and vocal cord polyps. The preparation process of the present invention is stable and feasible, and the chlorogenic acid content of the finished product is higher than the original process, which improves the utilization rate of raw materials and the extraction rate of active ingredients; the present invention has the function of promoting blood circulation and removing stasis, and can reduce the viscosity of whole blood, plasma Viscosity, reduced viscosity of whole blood, fibrinogen content and platelet attachment rate; it has an inhibitory effect on chronic inflammatory granulation tissue hyperplasia.

Description

一种治疗声带小结、声带息肉症状的中药制备工艺及其用途 A preparation process and application of traditional Chinese medicine for treating symptoms of vocal cord nodules and vocal cord polyps

技术领域: Technical field:

本发明涉及一种中药制剂的制备工艺及其用途,特别是涉及一种治疗声带小结、声带息肉症状的中药制备工艺及其用途。The invention relates to a preparation process and application of a traditional Chinese medicine preparation, in particular to a preparation process and application of a traditional Chinese medicine for treating symptoms of vocal nodules and vocal cord polyps.

背景技术: Background technique:

咽喉病为临床常见病、多发病,发病率在全国范围内近年有增长趋势,目前我国咽喉病的患病人群不断增加,据有关医学临床报导,患各种各样急慢性咽喉疾病患者为国内总人数的12%左右,发病率之高,将引起医学界及国人的重视。Throat disease is a common clinical disease and frequently-occurring disease, and the incidence rate has been increasing nationwide in recent years. At present, the number of patients with throat disease in my country is increasing. About 12% of the total number of patients, the high incidence rate will cause the attention of the medical circle and the people of the country.

目前国内用于治疗咽喉病的纯中药制剂药品为数不多,尤其是治疗慢喉喑(声带小结、声带息肉、声带粘膜增厚)等纯中药品种几乎甚微。临床常用方法是西医治疗,采取声休运用抗生素控制或施行手术切除,中医除临床诊治加减处方用药外,形成疗效确切、辨证施治、标本兼治的中药制剂组方尚不多见。At present, there are not many pure Chinese medicine preparations for treating throat diseases in China, especially pure Chinese medicine varieties such as treating chronic laryngitis (vocal cord nodules, vocal cord polyps, and vocal cord mucosal thickening) are almost rare. The commonly used clinical method is Western medicine treatment, which uses antibiotics to control or surgical resection. In addition to adding and subtracting prescription drugs for clinical diagnosis and treatment, traditional Chinese medicine preparations with definite curative effects, syndrome differentiation, and both symptoms and root causes are rare.

CN1544077A公开了一种“治疗咽喉慢喉喑症状的中药”,其片剂、胶囊剂的制备工艺在原料的浓缩过程中损失较多,浓缩的浸膏密度不利于混合,不易干燥,费工、费时,并且原料的利用率、有效成分的提取率不高。在工业生产中,如何保证每批投料生产出的成品总量能在国家药品管理的允许的幅度内保持稳定,同时按国家法定药品检验各项数据及结果稳定,实验的重现性好,是一项重要的技术关键点。因此寻求研究成品稳定、高效,长效治疗各种咽喉疾病的系列药品有着重要的现实意义。CN1544077A discloses a kind of " Chinese medicine for the treatment of chronic and dull throat symptoms ", and its tablet, capsule preparation process loses more in the process of raw material concentration, and the concentrated extract density is unfavorable for mixing, is not easy to dry, takes a lot of work, It is time-consuming, and the utilization rate of raw materials and the extraction rate of active ingredients are not high. In industrial production, how to ensure that the total amount of finished products produced by each batch of materials can be kept stable within the range allowed by the national drug management, and at the same time, the data and results of the national statutory drug inspection are stable, and the reproducibility of the experiment is good. An important technical key point. Therefore it is of great practical significance to seek stable, efficient and long-acting series of medicines for the treatment of various throat diseases.

发明内容: Invention content:

本发明目的在于提供一种治疗声带小结、声带息肉症状的中药制剂的制备工艺。The purpose of the invention is to provide a preparation process of a traditional Chinese medicine preparation for treating symptoms of vocal cord nodules and vocal cord polyps.

本发明另一目的在于提供在治疗声带小结、声带息肉的药物中的应用。Another object of the present invention is to provide the application in medicine for treating vocal cord nodules and vocal cord polyps.

本发明目的是通过如下技术方案实现的:The object of the invention is achieved through the following technical solutions:

取处方量40%-60%的金银花、浙贝母、红花,处方量10%-30%的马勃,粉碎成细粉,过筛,混匀,备用;将莪术、桃仁、玄参、三棱、丹参、板蓝根、麦冬、泽泻、鸡内金、蝉蜕、木蝴蝶、蒲公英及金银花、浙贝母、红花、马勃四味药的粉碎后剩余量加8-12倍、6-10倍水煎煮二次,每次1-3小时,合并煎液,滤过,滤液浓缩至相对密度为1.28~1.32(60℃)的稠膏,加90%-100%乙醇使含醇量达50-70%,搅拌均匀,静置12-36小时,滤过,滤液回收乙醇,减压浓缩至相对密度为1.38~1.40(60℃)的清膏;加入制备的细粉及适量辅料混匀,干燥,粉碎,制成细小颗粒,即得。Take 40%-60% of the prescription amount of honeysuckle, Fritillaria, safflower, and 10%-30% of the prescription amount of puffball, grind into fine powder, sieve, mix, and set aside; Add 8-12 times, 6 -10 times of water decocted twice, each time for 1-3 hours, combined decoction, filtered, the filtrate was concentrated to a thick paste with a relative density of 1.28-1.32 (60°C), and 90%-100% ethanol was added to make the alcohol-containing The amount reaches 50-70%, stir evenly, stand still for 12-36 hours, filter, recover ethanol from the filtrate, concentrate under reduced pressure to a clear paste with a relative density of 1.38-1.40 (60°C); add the prepared fine powder and appropriate amount of auxiliary materials Mixed, dried, crushed, made into fine particles, that is.

本发明的制备工艺其工艺稳定、可行,成品的绿原酸含量比原工艺高,提高了原料的利用率、有效成分的提取率;本发明具有活血化淤功能,可降低全血粘度、血浆粘度、全血还原粘度、血纤维蛋白原含量和血小板附率;对慢性炎症肉芽组织增生具有抑制作用。水提工艺制备的成品治疗声带小结,总有效率56.67%,治疗声带息肉,总有效率为36.67%;水提醇沉工艺制备的成品治疗声带小结,总有效率90.00%,治疗声带息肉,总有效率86.67%;从而提高了治疗声带小结、声带息肉疾病的临床疗效。The preparation process of the present invention is stable and feasible, and the chlorogenic acid content of the finished product is higher than the original process, which improves the utilization rate of raw materials and the extraction rate of active ingredients; the present invention has the function of promoting blood circulation and removing stasis, and can reduce the viscosity of whole blood, plasma Viscosity, reduced viscosity of whole blood, fibrinogen content and platelet attachment rate; it has an inhibitory effect on chronic inflammatory granulation tissue hyperplasia. The finished product treated vocal cord summary prepared by the water extraction process has a total effective rate of 56.67%, and the total effective rate is 36.67% for the treatment of vocal cord polyps; The effective rate is 86.67%, thereby improving the clinical curative effect of treating vocal cord nodules and vocal cord polyposis.

具体实施方式 Detailed ways

下面实验例用于进一步说明本发明。The following experimental examples are used to further illustrate the present invention.

实验例1  水提工艺优选Experimental example 1 Water extraction process optimization

根据对水提工艺影响因素的分析,选择加水量、煎煮时间、煎煮次数作为主要因素,用正交试验法,以干膏量和绿原酸的转移率为考察指标,筛选出最佳工艺条件。According to the analysis of the influencing factors of the water extraction process, the amount of water added, the decoction time, and the number of decoctions were selected as the main factors. Using the orthogonal test method, the amount of dry paste and the transfer rate of chlorogenic acid were used as indicators to screen out the best. process conditions.

1、药材吸水量的考察:1. Investigation on the water absorption of medicinal materials:

按上述处方比例,称取水提部分药材共149.3g,加10倍量水浸泡至透心,滤过,测得平均吸水率为208%。According to the above-mentioned prescription proportions, a total of 149.3 g of the medicinal materials extracted by water was weighed, soaked in 10 times the amount of water until thoroughly filtered, and the average water absorption rate was measured to be 208%.

2、正交试验设计2. Orthogonal experimental design

经对提取工艺所涉及的提取次数、提取时间、加水量等因素进行分析对比,各设计3个水平,设计因素水平表,见表1。After analyzing and comparing the extraction times, extraction time, water addition and other factors involved in the extraction process, three levels were designed for each, and the design factor level table is shown in Table 1.

表1 水提正交试验因素水平表Table 1 Factor level table of water extraction orthogonal test

Figure C200610043108D00061
Figure C200610043108D00061

注:*括号内分别为第2、3次加水量Note: * The amount of water added in the brackets is the 2nd and 3rd times

3、试验方法3. Test method

按上述处方量比例,称取水提部分药材149.3g,共9份,按照L9(34)正交表设计的试验(表2),加水煎煮,滤过,量出滤液体积。测定出膏率和绿原酸转移率,结果见表2、表3。According to the proportion of the above prescription, weigh 149.3g of the water-extracted part of the medicinal materials, a total of 9 parts, according to the L 9 (3 4 ) orthogonal table design test (Table 2), add water to decoct, filter, and measure the volume of the filtrate. The ointment yield and chlorogenic acid transfer rate were measured, and the results are shown in Table 2 and Table 3.

干膏量的计算:精密吸取续滤液25ml,置已干燥至恒重的蒸发皿中,水浴蒸干,105℃干燥3小时,置干燥器中冷却30分钟,迅速称重,计算干膏量。Calculation of the amount of dry ointment: Precisely absorb 25ml of the filtrate, put it in an evaporating dish that has been dried to constant weight, evaporate to dryness in a water bath, dry at 105°C for 3 hours, cool in a desiccator for 30 minutes, weigh quickly, and calculate the amount of dry ointment.

绿原酸含量的测定:Determination of chlorogenic acid content:

色谱条件与系统适用性试验用十八烷基硅烷键合硅胶为填充剂;乙腈-0.4%磷酸溶液(10:90)为流动相;检测波长为327nm。理论板数按绿原酸峰计算应不低于2500。Chromatographic conditions and system suitability test used octadecylsilane bonded silica gel as filler; acetonitrile-0.4% phosphoric acid solution (10:90) as mobile phase; detection wavelength was 327nm. The number of theoretical plates should not be less than 2500 based on the chlorogenic acid peak.

对照品溶液的制备精密称取绿原酸对照品适量,置棕色容量瓶中,加50%甲醇制成每1ml含10μg的溶液,即得。Preparation of Reference Substance Solution Accurately weigh an appropriate amount of chlorogenic acid reference substance, put it in a brown volumetric flask, add 50% methanol to make a solution containing 10 μg per 1 ml, and obtain it.

供试品溶液的制备精密量取上述滤液10ml置25ml量瓶中,加50%甲醇10ml,超声处理30分钟,放冷,加50%甲醇至刻度,摇匀,即得。Preparation of the test solution Precisely measure 10ml of the above-mentioned filtrate, put it in a 25ml measuring bottle, add 10ml of 50% methanol, sonicate for 30 minutes, let it cool, add 50% methanol to the mark, shake well, and obtain.

测定法分别精密吸取对照品溶液和供试品溶液各5μl,注入液相色谱仪,测定,即得。Determination method Precisely draw 5 μl each of the reference substance solution and the test solution, inject it into the liquid chromatograph, measure it, and obtain it.

表2 L9(3)4正交试验结果表Table 2 L 9 (3) 4 Orthogonal Test Result Table

Figure C200610043108D00071
Figure C200610043108D00071

表3 方差分析结果Table 3 Results of variance analysis

Figure C200610043108D00072
Figure C200610043108D00072

Figure C200610043108D00081
Figure C200610043108D00081

F0.05(2,2)=19.00   F0.01(2,2)=99.00F 0.05 (2, 2) = 19.00 F 0.01 (2, 2) = 99.00

3.根据直观分析结合方差分析,水提最佳工艺条件为A2B2C3,但C2与C3很接近,从节省能源和工时出发,最佳提取工艺条件为A2B2C2,即水煎煮二次,第一次加10倍量水,第二次加8倍量水,每次2小时。3. According to intuitive analysis combined with variance analysis, the optimal process condition for water extraction is A 2 B 2 C 3 , but C 2 is very close to C 3 . From the perspective of saving energy and man-hours, the optimal extraction process condition is A 2 B 2 C 2 , that is, decoct twice with water, add 10 times the amount of water for the first time, and add 8 times the amount of water for the second time, 2 hours each time.

4.水提工艺的验证4. Verification of water extraction process

按上述处方量比例,称取水提部分药材149.3g,共3份,加水煎煮二次,第一次加10倍量水,第二次加8倍量水,每次2小时。滤过,测定出膏率和绿原酸转移率,结果见表4According to the proportion of the above prescription, weigh 149.3g of the water-extracted part of the medicinal material, a total of 3 parts, add water to decoct twice, add 10 times the amount of water for the first time, and add 8 times the amount of water for the second time, each time for 2 hours. Filtrate, measure paste yield and chlorogenic acid transfer rate, the results are shown in Table 4

表4  水提工艺验证结果Table 4 Water extraction process verification results

Figure C200610043108D00082
Figure C200610043108D00082

从表5可见,验证结果与正交试验结果基本一致。说明此工艺合理可行。故确定水煎煮二次,第一次加10倍量水,第二次加8倍量水,每次2小时。It can be seen from Table 5 that the verification results are basically consistent with the orthogonal test results. It shows that this process is reasonable and feasible. Therefore, it is determined to decoct twice with water, add 10 times the amount of water for the first time, and add 8 times the amount of water for the second time, each time for 2 hours.

实验例2  醇沉工艺优选Experimental example 2 Alcohol precipitation process optimization

1、醇沉条件的筛选1. Screening of alcohol precipitation conditions

药材的水提取物,因提出物易吸潮且杂质较大,故在制备过程中,应对其进行醇处理,以保留有效成分,除去杂质,减少服用量,因此,对不同浓度醇沉淀后的总出膏量及绿原酸含量,进行了考察。将有淀粉、粘液质的水煎液通过醇沉法纯化处理。对醇沉影响因素进行分析后,选择醇沉浓度(A)、药液相对密度(B)、静置时间(C),按L9(3)4设计正交试验,以干膏量和绿原酸的转移率作为评价指标进行综合分析。设计因素水平表,见表5。The water extract of medicinal materials, because the extract is easy to absorb moisture and has large impurities, it should be treated with alcohol during the preparation process to retain the active ingredients, remove impurities, and reduce the dosage. Therefore, for different concentrations of alcohol precipitation The total ointment output and chlorogenic acid content were investigated. The water decoction with starch and mucilage is purified by alcohol precipitation. After analyzing the influencing factors of alcohol precipitation, select the concentration of alcohol precipitation (A), the relative density of liquid medicine (B), and the standing time (C), and design an orthogonal experiment according to L9(3)4. The acid transfer rate was used as an evaluation index for comprehensive analysis. See Table 5 for the level table of design factors.

表5 4因素3水平排列表Table 5 4 Factor 3 Level Ranking Table

Figure C200610043108D00091
Figure C200610043108D00091

注:相对密度60℃测。Note: The relative density is measured at 60°C.

实验方法:按处方比例,称取金银花、浙贝母、红花各1/2量打粉,马勃筛取6.7g细粉外,称取其余十二味及上述四味药材的剩余量1493.1g,加水煎煮两次,每次2小时,加水量分别为药材总量的10倍、8倍,合并滤液,然后按正交试验方案要求操作。结果见表6、7。Experimental method: According to the proportion of the prescription, weigh 1/2 of each of honeysuckle, fritillaria, and safflower, and sift out 6.7g of fine powder with puffball, and weigh the remaining 1493.1g of the remaining twelve herbs and the above four herbs. , add water and decoct twice, each time for 2 hours, the amount of water added is 10 times and 8 times of the total amount of medicinal materials respectively, the filtrate is combined, and then operated according to the requirements of the orthogonal test program. The results are shown in Tables 6 and 7.

表6  L9(3)4正交试验结果表Table 6 L 9 (3) 4 Orthogonal Test Result Table

Figure C200610043108D00092
Figure C200610043108D00092

综合评分标准:规定绿原酸转移率Y满分60分,根据水提试验所得转移率,规定以转移率40%为满分,每1%为1.5分,计分为Y×1.5;出膏率X满分40分,根据出膏率的变动范围规定10%为0分,6%为40分,每增加1%减去40/(10-6)分,计分为[40-40/4(X-6)];二项指标总分100分,总评分计为Y×1.5+[40-40/4(X-6)]。Comprehensive scoring standard: The transfer rate Y of chlorogenic acid is stipulated with a full score of 60 points. According to the transfer rate obtained from the water extraction test, the transfer rate is 40% as the full score, and every 1% is 1.5 points, and the score is Y×1.5; the cream yield X The full score is 40 points, according to the fluctuation range of the paste rate, 10% is 0 points, 6% is 40 points, every 1% increase minus 40/(10-6) points, the score is [40-40/4(X -6)]; the total score of the two indicators is 100 points, and the total score is Y×1.5+[40-40/4(X-6)].

表7  方差分析结果Table 7 Results of variance analysis

Figure C200610043108D00101
Figure C200610043108D00101

F0.05(2,2)=19.00   F0.01(2,2)=99.00F 0.05 (2, 2) = 19.00 F 0.01 (2, 2) = 99.00

根据直观分析结合方差分析,A因素对绿原酸转移率和得膏率的影响具显著性,考虑生产中减少乙醇用量和缩短生产周期,确定A2B3C1为最佳提取工艺。According to visual analysis combined with variance analysis, factor A has a significant impact on the transfer rate of chlorogenic acid and the yield of ointment. Considering the reduction of ethanol consumption and shortening the production cycle in production, A 2 B 3 C 1 is determined to be the best extraction process.

实验例3 水提醇沉工艺与水提工艺优选Experimental Example 3 Water Extraction and Alcohol Precipitation Process and Optimization of Water Extraction Process

依据上述水提工艺和水提醇沉工艺确定的参数,按处方10倍量投料进行中试生产,对成型颗粒进行考察,比较两种工艺异同。According to the parameters determined by the above-mentioned water extraction process and water extraction and alcohol precipitation process, the pilot production was carried out according to 10 times the amount of the prescription, and the shaped particles were investigated to compare the similarities and differences of the two processes.

1.三批中试产品试验结果比较1. Comparison of test results of three batches of pilot products

三批中试产品试验结果见表8。The test results of the three batches of pilot products are shown in Table 8.

表8 不同工艺三批中试产品试验结果Table 8 Test results of three batches of pilot products with different processes

Figure C200610043108D00102
Figure C200610043108D00102

*A为水提工艺,B为水提醇沉工艺*A is the water extraction process, B is the water extraction and alcohol precipitation process

从上表可以看出,水提工艺提取出浸膏量和干膏量均较多,批次之间的差异较大,工艺不稳定,干膏量多,没有达到减少服用量的目的。水提醇沉工艺,有效的除去了非药用部位,保留了有效成分,工艺之间参数稳定,服用量符合国家药品用量规定。It can be seen from the above table that the water extraction process extracts a large amount of extract and dry paste, the difference between batches is large, the process is unstable, and the amount of dry paste is large, which does not achieve the purpose of reducing the dosage. The water extraction and alcohol precipitation process effectively removes the non-medicinal parts and retains the active ingredients. The parameters between the processes are stable, and the dosage meets the national drug dosage regulations.

2.颗粒引湿性考察2. Investigation on the hygroscopicity of particles

分别称取本品水提醇沉工艺和水提工艺制成的成型颗粒各约100g,放置于自然条件下(温度35℃,相对湿度70%),每24小时测其吸水率一次,结果见表9。Weigh about 100g each of the shaped granules produced by the water extraction and alcohol precipitation process and the water extraction process of this product, place them under natural conditions (temperature 35°C, relative humidity 70%), and measure their water absorption once every 24 hours. The results are shown in Table 9.

表9 不同工艺引湿性测试Table 9 Humidity test of different processes

Figure C200610043108D00111
Figure C200610043108D00111

*A为水提工艺,B为水提醇沉工艺*A is the water extraction process, B is the water extraction and alcohol precipitation process

由上表结果可以看出,水提醇沉工艺制备的成品其平均吸水率变化小,样品的稳定性较好。From the results in the above table, it can be seen that the average water absorption of the finished product prepared by the water extraction and alcohol precipitation process has little change, and the stability of the sample is better.

3.颗粒流动性考察3. Investigation of particle fluidity

用自制“漏斗”法对本品水提醇沉工艺和水提工艺制成的成型颗粒的流动性进行检查,结果见表10,11。Use the self-made "funnel" method to check the fluidity of the shaped particles produced by the water extraction and alcohol precipitation process and the water extraction process. The results are shown in Tables 10 and 11.

表10 不同工艺流动性测试Table 10 Fluidity tests of different processes

Figure C200610043108D00112
Figure C200610043108D00112

*A为水提工艺,B为水提醇沉工艺*A is the water extraction process, B is the water extraction and alcohol precipitation process

表11 不同工艺内容物休止角测定结果Table 11 Measurement results of angle of repose of content in different processes

*A为水提工艺,B为水提醇沉工艺*A is the water extraction process, B is the water extraction and alcohol precipitation process

由上表结果可以看出,水提醇沉工艺制备的成品颗粒流动性较好,易于颗粒的充填和分装,适合大规模生产。It can be seen from the results in the above table that the finished granules prepared by the water extraction and alcohol precipitation process have better fluidity, are easy to fill and pack the granules, and are suitable for large-scale production.

4.产品质量分析4. Product quality analysis

对水提醇沉工艺和水提工艺制成的成型颗粒按照拟订的质量标准进行检测,考察不同工艺对产品质量的影响,从而确定合理的生产工艺。实验结果见表12。The formed granules produced by the water extraction and alcohol precipitation process and the water extraction process are tested according to the proposed quality standards, and the influence of different processes on product quality is investigated, so as to determine a reasonable production process. The experimental results are shown in Table 12.

表12 三批不同工艺产品质量分析Table 12 Quality analysis of three batches of products with different processes

Figure C200610043108D00123
Figure C200610043108D00123

*A为水提工艺,B为水提醇沉工艺*A is the water extraction process, B is the water extraction and alcohol precipitation process

由上表的结果可以看出,水提工艺提出的非药用成份较多,干扰了对药品质量标准的检测,不能准确控制药品质量,工艺不稳定;水提醇沉工艺的样品鉴别项均能检出,绿原酸含量较高,含量的差异性小,表明醇沉后的工艺稳定性好。From the results in the above table, it can be seen that the water extraction process contains many non-medicinal ingredients, which interferes with the detection of drug quality standards, cannot accurately control the quality of drugs, and the process is unstable; the sample identification items of the water extraction and alcohol precipitation process are all It can be detected that the content of chlorogenic acid is relatively high, and the difference in content is small, indicating that the process stability after alcohol precipitation is good.

5.产品稳定性分析5. Product stability analysis

对水提醇沉工艺和水提工艺制成的胶囊剂,进行加速试验,在温度(40±2)℃,相对湿度(70±5)%的条件下放置六个月,每月取样检测一次,按稳定性重点考察项目检测,结果见表13、14。For the capsules made by water extraction and alcohol precipitation process and water extraction process, carry out accelerated test, place it under the conditions of temperature (40±2) ℃ and relative humidity (70±5)% for six months, and take samples for testing once a month , according to the key items of stability inspection, the results are shown in Tables 13 and 14.

表13 水提工艺制成成品稳定性检测Table 13 Stability testing of finished products made by water extraction process

Figure C200610043108D00131
Figure C200610043108D00131

表14 水提醇沉工艺制成成品稳定性检测Table 14 Stability testing of finished products made by water extraction and alcohol precipitation process

Figure C200610043108D00132
Figure C200610043108D00132

Figure C200610043108D00141
Figure C200610043108D00141

*A为水提工艺,B为水提醇沉工艺*A is the water extraction process, B is the water extraction and alcohol precipitation process

由表10、11可以看出,水提工艺的样品由于提出的非药用成份较多,干扰了对药品质量标准的检测,含量差异性大且吸湿性大;水提醇沉工艺的样品按照拟订的质量标准进行检测,鉴别项均能检出,橙皮苷含量较高,含量的差异性小,表明醇沉后的工艺稳定性好。It can be seen from Tables 10 and 11 that the samples of the water extraction process have more non-medicinal ingredients, which interfere with the detection of drug quality standards, and have large content differences and large hygroscopicity; the samples of the water extraction and alcohol precipitation process according to The proposed quality standard was tested, and the identification items could be detected. The content of hesperidin was relatively high, and the difference in content was small, indicating that the process stability after alcohol precipitation was good.

实验例4 抗炎作用的研究Experimental Example 4 Research on anti-inflammatory effect

抗慢性炎症试验(大鼠棉球皮下植入法)Anti-chronic inflammation test (rat cotton ball subcutaneous implantation method)

受试药物:Test drug:

名称:金嗓散结胶囊Name: Jinsang Sanjie Capsules

性状:内容物为棕褐色的颗粒及粉末;气微,味微苦。Properties: The content is brown granule and powder; slight gas, slightly bitter taste.

提供单位:西安碑林中药厂Provider: Xi'an Beilin Traditional Chinese Medicine Factory

批号:水提醇沉提取物胶囊940303;水提取物胶囊940301Batch No.: Water Extraction and Alcohol Precipitation Extract Capsules 940303; Water Extract Capsules 940301

含量:水提醇沉提取物胶囊940303 0.4g/粒Content: water extraction and alcohol precipitation extract capsule 940303 0.4g/capsule

      水提取物胶囊940301 0.4g/粒  Water extract capsule 940301 0.4g/capsule

对照药及主要试剂方法:强的松片[陕卫准字(1993)第000532号],西安制药厂生产,批号9303145;复方丹参片[ZZ-0253-奥卫药准字(1996)第132170号],广州白云山制药厂生产,批号:94021436。Control drug and main reagent methods: Prednisone Tablets [Shaanwei Zhunzi (1993) No. 000532], produced by Xi’an Pharmaceutical Factory, batch number 9303145; No.], produced by Guangzhou Baiyunshan Pharmaceutical Factory, batch number: 94021436.

仪器  LG-III型旋转筒式血液粘度测试仪,中国科学院传感技术公司生产;9103-B血小板粘附仪,中国科学院传感技术公司生产;3F-3型高速微量离心机,华兴机轮公司生产;读数显微镜,长春第一光学仪器厂生产;JA1003电子天平,上海精密科学仪器有限公司生产。Instrument LG-III rotating cylinder blood viscosity tester, produced by Sensing Technology Company of Chinese Academy of Sciences; 9103-B Platelet Adhesion Instrument, produced by Sensing Technology Company of Chinese Academy of Sciences; 3F-3 high-speed microcentrifuge, produced by Huaxing Jilun Company Production; reading microscope, produced by Changchun No. 1 Optical Instrument Factory; JA1003 electronic balance, produced by Shanghai Precision Scientific Instrument Co., Ltd.

受试动物  SD品系大鼠,体质量:200-250g ♂♀各半。陕医动证字第08-005号,由西安医科大学实验动物中心提供。Test animals SD strain rats, body weight: 200-250g ♂♀ half and half. Shanyi Dongzhengzi No. 08-005, provided by the Experimental Animal Center of Xi'an Medical University.

实验室温:20-26℃   相对湿度:42-76%。Laboratory temperature: 20-26°C Relative humidity: 42-76%.

实验方法及结果Experimental method and results

取大鼠80只,雌雄各半,随机分为8组,每组10只。第一组为空白对照组,给等容积生理盐水;第二组为阳性对照组(强的松片8mg/kg);第3、4、5组为金嗓散结水提取物胶囊组(0.2142g、0.4284g、0.8568g/kg生药);第6、7、8组为金嗓散结水提醇沉提取物胶囊组(0.2142g、0.4284g、0.8568g/kg生药)。在乙醚浅麻下,剪毛消毒。无菌操作,于下腹部正中切开皮肤,将重50mg的灭菌棉球植入两侧腹股沟皮下,然后缝合皮肤,消毒,。从手术前3d开始ig给药,2ml/100g,1次/日,连续10d。d11处死大鼠,小心剥离取出棉球及包裹的肉芽组织,60℃干燥12h后称重,减去原棉球重量即为肉芽组织重量,以100g体重所含肉芽组织重量(双侧)表示。经t检验。结果见表15。80 rats, half male and half male, were randomly divided into 8 groups, 10 rats in each group. The first group is a blank control group, which gives equal volume of normal saline; the second group is a positive control group (prednisone tablet 8mg/kg); g, 0.4284g, 0.8568g/kg crude drug); the 6th, 7th, and 8th groups were Jinsang Sanjie water extraction and alcohol precipitation extract capsule group (0.2142g, 0.4284g, 0.8568g/kg crude drug). Under light anesthesia with ether, the shearing was disinfected. Aseptic operation, the skin was cut in the middle of the lower abdomen, and 50 mg sterile cotton balls were implanted under the skin of the groin on both sides, and then the skin was sutured and disinfected. From 3 days before the operation, ig administration was started, 2ml/100g, 1 time/day, for 10 consecutive days. Rats were sacrificed on day 11, the cotton balls and wrapped granulation tissue were carefully peeled off, dried at 60°C for 12 hours, and then weighed. Subtracting the weight of the original cotton balls was the weight of granulation tissue, expressed as the weight of granulation tissue contained in 100 g of body weight (both sides). Tested by t. The results are shown in Table 15.

表15 两种金嗓散结胶囊对大鼠慢性增生炎症的影响(X±S)Table 15 Effects of two kinds of Jinsang Sanjie Capsules on chronic hyperplasia and inflammation in rats (X±S)

与空白对照组比较*P<0.05  **P<0.01Compared with blank control group *P<0.05 **P<0.01

由表15可见,金嗓散结水提醇沉提取物胶囊和水提取物胶囊抑制大鼠棉球肉芽肿组织增生,减轻肉芽组织重量与空白对照组比较,均具有显著性差异(P<0.01);结果表明,两种不同工艺生产的金嗓散结胶囊对大鼠慢性棉球增生性炎症均有抑制作用,但金嗓散结水提醇沉提取物胶囊药效优于水提取物胶囊。It can be seen from Table 15 that Jinsang Sanjie Water Extraction and Precipitation Extract Capsules and Water Extract Capsules inhibit the hyperplasia of cotton ball granuloma tissue in rats, and reduce the weight of granulation tissue compared with the blank control group, there are significant differences (P<0.01 ); the results showed that Jinsang Sanjie Capsules produced by two different processes had inhibitory effect on chronic cotton ball proliferative inflammation in rats, but the efficacy of Jinsang Sanjie water-extracted and alcohol-precipitated capsules was better than that of water-extracted capsules .

实验例5 活血化瘀作用的研究Experimental Example 5 Study on the effect of promoting blood circulation and removing blood stasis

对急性血瘀证模型大鼠血液流变学的影响Effects on Hemorheology of Rats with Acute Blood Stasis Syndrome

受试药物:Test drug:

名称:金嗓散结胶囊Name: Jinsang Sanjie Capsules

性状:内容物为棕褐色的颗粒及粉末;气微,味微苦。Properties: The content is brown granule and powder; slight gas, slightly bitter taste.

提供单位:西安碑林中药厂Provider: Xi'an Beilin Traditional Chinese Medicine Factory

批号:水提醇沉提取物胶囊940303;水提取物胶囊940301Batch No.: Water Extraction and Alcohol Precipitation Extract Capsules 940303; Water Extract Capsules 940301

含量:水提醇沉提取物胶囊940303 0.4g/粒Content: water extraction and alcohol precipitation extract capsule 940303 0.4g/capsule

      水提取物胶囊940301 0.4g/粒  Water extract capsule 940301 0.4g/capsule

大鼠90只,雌雄各半,随机分为9组,每组10只。第一组为空白对照组,给等容积生理盐水;第二组为模型对照组,给等容积生理盐水;第三组为阳性对照组,给复方丹参片0.6g/kg;第4、5、6组为金嗓散结水提取物组(0.2142g、0.4284g、0.8568g/kg生药);第7、8、9组为金嗓散结水提醇沉提取物组(0.2142g、0.4284g、0.8568g/kg生药)。ig给药,等容量2ml/100g,1次/日,连续7d。试验d8除空白对照组外,其余各组均按文献方法复制急性血瘀证模型。每只大鼠Sc肾上腺素8μg/kg,2h后将大鼠浸入0℃冰水中5min,再过2h后第二次Sc等量肾上腺素。然后禁食,12h后乙醚麻醉下颈动脉采血,肝素抗凝,用于测定全血高切(200S-1)和低切粘度(40S-1)、血沉、红细胞压积并计算全血还原粘度;用热沉淀法测定血液纤维蛋白原含量;另取肝素抗凝血离心分离血浆,测定血浆粘度;再取枸橼酸钠抗凝血,用于测定血小板粘附率。经t检验。结果见表16、表17。90 rats, half male and half male, were randomly divided into 9 groups, 10 rats in each group. The first group is the blank control group, which is given equal volume of normal saline; the second group is the model control group, which is given equal volume of normal saline; Group 6 is Jinsang Sanjie water extract group (0.2142g, 0.4284g, 0.8568g/kg crude drug); Groups 7, 8, and 9 are Jinsang Sanjie water extraction and alcohol precipitation extract group (0.2142g, 0.4284g , 0.8568g/kg crude drug). Ig administration, equal volume 2ml/100g, 1 time/day, for 7 consecutive days. On test d8, except for the blank control group, the other groups copied the acute blood stasis model according to the literature method. Each rat Sc adrenaline 8 μg/kg, 2 hours later, the rats were immersed in ice water at 0°C for 5 minutes, and after another 2 hours, the same amount of adrenaline was Sc for the second time. After 12 hours of fasting, blood was collected from the carotid artery under ether anesthesia, anticoagulated with heparin, and used to measure high shear (200S -1 ) and low shear viscosity (40S -1 ), erythrocyte sedimentation rate, hematocrit and calculate whole blood reduced viscosity Determination of blood fibrinogen content by thermal precipitation method; take heparin anticoagulant blood and centrifuge plasma to measure plasma viscosity; take sodium citrate anticoagulant blood for determination of platelet adhesion rate. Tested by t. The results are shown in Table 16 and Table 17.

表16 两种金嗓散结胶囊对急性血瘀证大鼠血液粘度的影响(X±S)Table 16 Effects of two kinds of Jinsang Sanjie Capsules on blood viscosity of rats with acute blood stasis syndrome (X±S)

Figure C200610043108D00171
Figure C200610043108D00171

与正常对照组比较,**P<0.01;与模型对照组比较,*P<0.05,**P<0.01Compared with normal control group, **P<0.01; compared with model control group, *P<0.05, **P<0.01

表17 两种金嗓散结胶囊对急性血瘀证大鼠血纤维蛋白原含量、血沉、血小板粘附率及细胞压积的影响(X±S)Table 17 Effects of two kinds of Jinsang Sanjie Capsules on blood fibrinogen content, erythrocyte sedimentation rate, platelet adhesion rate and cell volume in acute blood stasis rats (X±S)

Figure C200610043108D00172
Figure C200610043108D00172

Figure C200610043108D00181
Figure C200610043108D00181

与正常对照组比较,**P<0.01;与模型对照组比较,*P<0.05,**P<0.01Compared with normal control group, **P<0.01; compared with model control group, *P<0.05, **P<0.01

由表16及表17可见,急性血瘀证模型大鼠全血高切变和低切变率粘度、血浆粘度和全血还原粘度明显增高,血液纤维蛋白原增多,血小板粘附率升高,与正常对照组比较,统计学有显著性差异(P<0.01)。与模型对照组比较,两种金嗓散结胶囊均降低急性血瘀证大鼠全血高切变和低切变率粘度、血浆粘度和全血还原粘度,降低血液纤维蛋白原含量,中、大剂量组具有显著性差异(P<0.05或P<0.01);且金嗓散结水提醇沉提取物胶囊优于水提取物胶囊。对血沉和红细胞压积则无明显影响。It can be seen from Table 16 and Table 17 that the whole blood high shear and low shear rate viscosity, plasma viscosity and whole blood reduced viscosity of acute blood stasis model rats were significantly increased, blood fibrinogen increased, platelet adhesion rate increased, Compared with the normal control group, there was statistically significant difference (P<0.01). Compared with the model control group, the two Jinsang Sanjie capsules both reduced the high-shear and low-shear rate viscosity, plasma viscosity and whole blood reduced viscosity of rats with acute blood stasis syndrome, and reduced the blood fibrinogen content. The high-dose group had significant difference (P<0.05 or P<0.01); and Jinsang Sanjie water-extracted alcohol-precipitated extract capsules were better than water-extracted capsules. There was no significant effect on erythrocyte sedimentation rate and hematocrit.

实验例6 金嗓散结胶囊治疗声带小结、声带息肉临床研究Experimental Example 6 Clinical Study of Jinsang Sanjie Capsules in Treating Vocal Cord Nodules and Vocal Cord Polyps

一、临床试验1. Clinical trials

试验方法experiment method

(一)实验设计(1) Experimental design

随机对照临床试验。试验组A组60例,B组60例,确定最佳的制备工艺。Randomized controlled clinical trials. The test group consists of 60 cases in group A and 60 cases in group B to determine the best preparation process.

(二)治疗方法(2) Treatment methods

A组:水提醇沉工艺生产金嗓散结胶囊,规格:每粒装0.4g,每粒含原生药量2.5g,用法用量:口服,一次3粒,一日2次。Group A: Jinsang Sanjie Capsules produced by water extraction and alcohol precipitation process, specifications: each capsule contains 0.4g, and each capsule contains 2.5g of raw medicine, usage and dosage: oral, 3 capsules at a time, twice a day.

B组:水提工艺生产金嗓散结胶囊,规格:每粒装0.4g,每粒含原生药量1.25g,用法用量:口服,一次6粒,一日2次。Group B: Jinsang Sanjie Capsules produced by water extraction process, specifications: each capsule contains 0.4g, each capsule contains 1.25g of crude drug, usage and dosage: oral, 6 capsules at a time, twice a day.

两组的日服用生药量均为15g,具有可比性。The daily dose of crude drug in the two groups was 15g, which was comparable.

疗程:一个月。Course of treatment: one month.

(三)观察方法(3) Observation method

在临床试验开始之前对参加试验的临床医师进行统一培训,使其对试验方案有充分的理解和统一认识,保证观测的各项指标的一致性。Before the start of the clinical trial, provide unified training to the clinicians participating in the trial, so that they can have a full understanding of the trial protocol and a unified understanding to ensure the consistency of the observed indicators.

1.门诊病历严格控制可变因素。1. Strict control of variable factors in outpatient medical records.

2.统一设计观察表格。2. Unified design of the observation form.

3.凡符合病历选择标准列为观察对象者,均按观察方案及观察表的要求填好症状及体征和有关各项检查结果。3. Anyone who meets the selection criteria of the medical records and is listed as the observation object shall fill in the symptoms and signs and relevant inspection results according to the requirements of the observation plan and observation form.

4.参加临床试验的医师必须向受试者提供有关临床试验的详细情况,包括试验目的,试验性质,可能的受益和危险,可供选用的其它治疗方及符合赫尔辛基宣言规定的受试者的权利和义务等,使受试者了解后表示同意。4. Physicians participating in the clinical trial must provide the subjects with detailed information about the clinical trial, including the purpose of the trial, the nature of the trial, possible benefits and risks, other treatments available and the conditions of the subjects who meet the requirements of the Declaration of Helsinki. Rights and obligations, etc., so that the subjects can express their consent after understanding.

观测指标:Observation indicators:

1.安全性观测:一般体格检查。1. Safety observation: general physical examination.

2.疗效性观察:相关症状及局部检查。2. Curative effect observation: related symptoms and local examination.

3.观测注意点:3. Observation points:

相关症状和体征:治疗后14天、30天各观察一次。Relevant symptoms and signs: observe once 14 days and 30 days after treatment.

疗效判定标准:Efficacy Judgment Criteria:

1.临床痊愈:声带小结、声带息肉消失,症状消失。1. Clinical recovery: vocal cord nodules, vocal cord polyps disappeared, and symptoms disappeared.

2.显效:声带小结、声带息肉、症状减少2/3以上者。2. Significant effect: Vocal cord nodules, vocal cord polyps, and symptoms are reduced by more than 2/3.

3.有效:声带小结、声带息肉、症状减少1/3以上者。3. Effective: Vocal cord nodules, vocal cord polyps, symptoms reduced by more than 1/3.

4.无效:声带小结、声带息肉、症状无改变或加重者。4. Ineffective: Vocal cord nodules, vocal cord polyps, no change or aggravation of symptoms.

安全性评价标准:Safety Evaluation Criteria:

1级:安全,无任何不良反应。Level 1: Safe, without any adverse reactions.

2级:比较安全,如有不良反应,不需做任何处理可继续给药。Level 2: It is relatively safe. If there is any adverse reaction, the drug can be continued without any treatment.

3级:有安全性问题,有中等程度的不良反应,做处理后可继续给药。Grade 3: There are safety problems and moderate adverse reactions, and the drug can be continued after treatment.

4级:因不良反应中止试验。Grade 4: The trial was discontinued due to adverse reactions.

二、病例资料2. Case information

性别:两组患者性别分布比较,见表1。Gender: The gender distribution of patients in the two groups is compared, see Table 1.

表1-1 两组声带小结患者性别分布比较Table 1-1 Comparison of gender distribution of patients with vocal cord nodules between the two groups

Figure C200610043108D00201
Figure C200610043108D00201

A组与B组比较:X2=0.625,P>0.05,无统计学意义。Comparison between group A and group B: X 2 =0.625, P>0.05, no statistical significance.

表1-2 两组声带息肉患者性别分布比较Table 1-2 Comparison of gender distribution of patients with vocal cord polyps in the two groups

Figure C200610043108D00202
Figure C200610043108D00202

A组与B组比较:X2=1.674,P>0.05,无统计学意义。Comparison between group A and group B: X 2 =1.674, P>0.05, no statistical significance.

年龄:两组患者年龄分布比较,见表2。Age: see Table 2 for comparison of the age distribution of the two groups of patients.

表2-1 两组声带小结患者年龄分布比较(岁)Table 2-1 Comparison of age distribution of patients with vocal cord nodules between the two groups (years)

Figure C200610043108D00203
Figure C200610043108D00203

A组与B组比较:X2=4.132,P>0.05,无统计学意义。Comparison between group A and group B: X2=4.132, P>0.05, no statistical significance.

表2-2 两组声带息肉患者年龄分布比较(岁)Table 2-2 Comparison of age distribution of patients with vocal cord polyps in the two groups (years)

Figure C200610043108D00204
Figure C200610043108D00204

A组与B组比较:X2=0.552,P>0.05,无统计学意义。Comparison between group A and group B: X 2 =0.552, P>0.05, no statistical significance.

病程:两组患者病程分布比较,见表3。Disease course: the comparison of the disease course distribution of the two groups is shown in Table 3.

表3-1 两组声带小结患者病程分布比较(月)Table 3-1 Comparison of disease course distribution of patients with vocal cord nodules between the two groups (months)

Figure C200610043108D00211
Figure C200610043108D00211

A组与B组比较:X2=0.119,P>0.05,无统计学意义。Comparison between group A and group B: X 2 =0.119, P>0.05, no statistical significance.

表3-2 两组声带息肉患者病程分布比较(月)Table 3-2 Comparison of disease course distribution in two groups of patients with vocal cord polyps (months)

A组与B组有比较:X2=3.005,P>0.05,无统计学意义。There is a comparison between group A and group B: X 2 =3.005, P>0.05, no statistical significance.

病情:两组患者病情比较,见表4。Conditions: The conditions of the two groups were compared, see Table 4.

表4-1 两组声带小结患者病情比较Table 4-1 Comparison of the condition of patients with vocal cord nodules between the two groups

A组与B组比较:X2=2.767,P>0.05,无统计学意义。Comparison between group A and group B: X 2 =2.767, P>0.05, no statistical significance.

表4-2 两组声带息肉患者病情比较Table 4-2 Comparison of the condition of patients with vocal cord polyps in the two groups

Figure C200610043108D00214
Figure C200610043108D00214

A组与B组比较:X2=4.571,P>0.05,无统计学意义。Comparison between group A and group B: X 2 =4.571, P>0.05, no statistical significance.

三、治疗结果3. Treatment results

两组患者临床疗效比较,见表5。The clinical curative effect comparison of the two groups of patients is shown in Table 5.

表5-1 两组声带小结患者临床疗效比较Table 5-1 Comparison of clinical curative effect of two groups of patients with vocal cord nodules

Figure C200610043108D00221
Figure C200610043108D00221

A组与B组比较:U=2.1317,P<0.01,有显著性差异。Compared with group A and group B: U=2.1317, P<0.01, there is a significant difference.

表5-2 两组声带息肉患者临床疗效比较Table 5-2 Comparison of clinical curative effect of two groups of patients with vocal cord polyps

Figure C200610043108D00222
Figure C200610043108D00222

A组与B组比较:U=2.5938,P<0.01,有显著性差异。Compared with group A and group B: U=2.5938, P<0.01, there is a significant difference.

两组患者治疗后各项症状疗效比较,见表6。The curative effect of each symptom after treatment in the two groups was compared, as shown in Table 6.

表6-1 两组声带小结患者治疗后各项症状疗效比较Table 6-1 Comparison of curative effects of various symptoms after treatment in patients with vocal cord nodules between the two groups

Figure C200610043108D00223
Figure C200610043108D00223

两组声带小结患者治疗后各项症状均有明显改善,组间比较,声音嘶哑、咽干为<0.05,有显著性差异;语言疲劳为P<0.01,有极显著性差,咽痒为P>0.05,无显著性差异。The symptoms of the two groups of patients with vocal cord nodules were significantly improved after treatment. Compared between the two groups, hoarseness and dry throat were <0.05, with a significant difference; language fatigue was P<0.01, with a very significant difference, and throat itching was P> 0.05, no significant difference.

表6-2 两组声带息肉患者治疗后各项症状疗效比较Table 6-2 Comparison of curative effects of various symptoms after treatment in two groups of patients with vocal cord polyps

Figure C200610043108D00231
Figure C200610043108D00231

两组声带息肉患者治疗后各项症状均有明显改善,组间比较,声音嘶哑、咽干为<0.05,有显著性差异;咽痒、语言疲劳为P>0.05,无显著性差异。不良反应:临床验证期间,无不良反应发生。All the symptoms of patients with vocal cord polyps in the two groups were significantly improved after treatment. Compared between the two groups, hoarseness and dry throat were <0.05, with significant differences; throat itching and speech fatigue were P>0.05, with no significant difference. Adverse reactions: During clinical verification, no adverse reactions occurred.

四、实验结论4. Experimental conclusion

金嗓散结胶囊治疗声带小结,声带息肉试验共观察病例120例,其中声带息肉60例,声带小结60例。临床观察结果:水提醇沉工艺生产的金嗓散结胶囊(A组)治疗声带小结,其中痊愈7例,显效12例,有效18例,无效3例,总有效率90.00%;水提工艺生产的金嗓散结胶囊(B组)治疗声带小结,其中痊愈3例,显效4例,有效10例,无效13例,总有效率56.67%。水提醇沉工艺生产的金嗓散结胶囊(A组)治疗声带息肉,其中痊愈3例,显效13例,有效10例,无效4例,总有效率86.67%,水提工艺生产的金嗓散结胶囊(B组)治疗声带息肉,其中痊愈0例,显效2例,有效9例,无效19例,总有效率36.67%。治疗前后各项中医症状均有明显改善。Jinsang Sanjie Capsules was used to treat vocal cord nodules, and a total of 120 cases of vocal cord polyps were observed, including 60 cases of vocal cord polyps and 60 cases of vocal cord nodules. Clinical observation results: Jinsang Sanjie Capsules (group A) produced by water extraction and alcohol precipitation process treated vocal cord nodules, among which 7 cases were cured, 12 cases were markedly effective, 18 cases were effective, and 3 cases were ineffective, with a total effective rate of 90.00%. The produced Jinsang Sanjie Capsules (group B) treated vocal cord nodules, among which 3 cases were cured, 4 cases were markedly effective, 10 cases were effective, and 13 cases were ineffective, with a total effective rate of 56.67%. Jinsang Sanjie Capsules (Group A) produced by water extraction and alcohol precipitation process treated vocal cord polyps, among which 3 cases were cured, 13 cases were markedly effective, 10 cases were effective, and 4 cases were ineffective, with a total effective rate of 86.67%. Sanjie Capsules (group B) treated vocal cord polyps, among which 0 cases were cured, 2 cases were markedly effective, 9 cases were effective, and 19 cases were ineffective, with a total effective rate of 36.67%. All TCM symptoms were significantly improved before and after treatment.

处方:马勃25g,莪术(醋炒)50g,金银花125g,桃仁50g,玄参125g,三棱(醋炒)50g,红花50g,丹参75g,板蓝根125g,麦冬100g,浙贝母75g,泽泻75g,蝉蜕75g,鸡内金(炒)50g,木蝴蝶75g,蒲公英125g;Prescription: Puffball 25g, Zedoary (stir-fried with vinegar) 50g, honeysuckle 125g, peach kernel 50g, Scrophulariaceae 125g, Sanleng (stir-fried with vinegar) 50g, safflower 50g, Salvia miltiorrhiza 75g, Radix Radix 125g, Ophiopogon japonicus 100g, Fritillaria 75g, Alisma 75g, cicada slough 75g, gallinaceous gold (fried) 50g, wood butterfly 75g, dandelion 125g;

具体实施例1  制备片剂的工艺步骤如下:Specific embodiment 1 The processing step of preparing tablet is as follows:

取处方量50%的金银花、浙贝母、红花,处方量2%的马勃,粉碎成细粉,过筛,混匀,备用;将莪术、桃仁、玄参、三棱、丹参、板蓝根、麦冬、泽泻、鸡内金、蝉蜕、木蝴蝶、蒲公英及金银花、浙贝母、红花、马勃四味药的粉碎后剩余量加加10倍、8倍水煎煮二次,每次2小时,合并煎液,滤过,滤液浓缩至相对密度为1.28~1.32(60℃)的稠膏,加95%乙醇使含醇量达60%,搅拌均匀,静置24小时,滤过,滤液回收乙醇,减压浓缩至相对密度为1.38~1.40(60℃)的清膏;加入制备的细粉及适量辅料混匀,压制成片,包薄膜衣,即得。Take 50% of the prescription amount of honeysuckle, Zhejiang Fritillaria, safflower, and 2% of the prescription amount of puffballs, crush them into fine powder, sieve, mix, and set aside; use curcuma, peach kernels, scrophulariaceae, trigonum, salvia miltiorrhiza, and isatis root , Ophiopogon japonicus, Alisma, gallinacea, cicada slough, wood butterfly, dandelion, honeysuckle, fritillaria, safflower, and puffball. After crushing, add 10 times and 8 times the remaining amount of water to decoct twice. Combine the decoctions for 2 hours each time, filter, concentrate the filtrate to a thick paste with a relative density of 1.28-1.32 (60°C), add 95% ethanol to make the alcohol content reach 60%, stir evenly, let stand for 24 hours, filter After filtration, the ethanol is recovered from the filtrate, concentrated under reduced pressure to a clear paste with a relative density of 1.38-1.40 (60°C); the prepared fine powder and appropriate amount of auxiliary materials are added, mixed evenly, compressed into tablets, and film-coated to obtain the product.

实施例2  制备胶囊剂的工艺步骤如下:Embodiment 2 The processing steps of preparing capsules are as follows:

取处方量50%的金银花、浙贝母、红花,处方量2%的马勃,粉碎成细粉,过筛,混匀,备用;将莪术、桃仁、玄参、三棱、丹参、板蓝根、麦冬、泽泻、鸡内金、蝉蜕、木蝴蝶、蒲公英及金银花、浙贝母、红花、马勃四味药的粉碎后剩余量加加10倍、8倍水煎煮二次,每次2小时,合并煎液,滤过,滤液浓缩至相对密度为1.28~1.32(60℃)的稠膏,加95%乙醇使含醇量达60%,搅拌均匀,静置24小时,滤过,滤液回收乙醇,减压浓缩至相对密度为1.38~1.40(60℃)的清膏;加入制备的细粉及适量辅料混匀,干燥,粉碎,制成细小颗粒,装入胶囊,即得。Take 50% of the prescription amount of honeysuckle, Zhejiang Fritillaria, safflower, and 2% of the prescription amount of puffballs, crush them into fine powder, sieve, mix, and set aside; use curcuma, peach kernels, scrophulariaceae, trigonum, salvia miltiorrhiza, and isatis root , Ophiopogon japonicus, Alisma, gallinacea, cicada slough, wood butterfly, dandelion, honeysuckle, fritillaria, safflower, and puffball. After crushing, add 10 times and 8 times the remaining amount of water to decoct twice. Combine the decoctions for 2 hours each time, filter, concentrate the filtrate to a thick paste with a relative density of 1.28-1.32 (60°C), add 95% ethanol to make the alcohol content reach 60%, stir evenly, let stand for 24 hours, filter After filtration, the filtrate recovered ethanol, concentrated under reduced pressure to a clear paste with a relative density of 1.38-1.40 (60°C); added the prepared fine powder and appropriate amount of auxiliary materials, mixed evenly, dried, crushed, made into fine particles, and packed into capsules to obtain .

实施例3  制备颗粒剂的工艺步骤如下:Embodiment 3 The processing steps of preparing granules are as follows:

取处方量50%的金银花、浙贝母、红花,处方量2%的马勃,粉碎成细粉,过筛,混匀,备用;将莪术、桃仁、玄参、三棱、丹参、板蓝根、麦冬、泽泻、鸡内金、蝉蜕、木蝴蝶、蒲公英及金银花、浙贝母、红花、马勃四味药的粉碎后剩余量加加10倍、8倍水煎煮二次,每次2小时,合并煎液,滤过,滤液浓缩至相对密度为1.28~1.32(60℃)的稠膏,加95%乙醇使含醇量达60%,搅拌均匀,静置24小时,滤过,滤液回收乙醇,减压浓缩至相对密度为1.38~1.40(60℃)的清膏;加入制备的细粉,混匀,干燥,粉碎,制成细小颗粒,包装即得。Take 50% of the prescription amount of honeysuckle, Zhejiang Fritillaria, safflower, and 2% of the prescription amount of puffballs, crush them into fine powder, sieve, mix, and set aside; use curcuma, peach kernels, scrophulariaceae, trigonum, salvia miltiorrhiza, and isatis root , Ophiopogon japonicus, Alisma, gallinacea, cicada slough, wood butterfly, dandelion, honeysuckle, fritillaria, safflower, and puffball. After crushing, add 10 times and 8 times the remaining amount of water to decoct twice. Combine the decoctions for 2 hours each time, filter, concentrate the filtrate to a thick paste with a relative density of 1.28-1.32 (60°C), add 95% ethanol to make the alcohol content reach 60%, stir evenly, let stand for 24 hours, filter After filtration, ethanol is recovered from the filtrate, concentrated under reduced pressure to a clear paste with a relative density of 1.38-1.40 (60°C); the prepared fine powder is added, mixed, dried, crushed, made into fine particles, and packaged.

实施例4  制备软胶囊剂的工艺步骤如下:Embodiment 4 The processing steps of preparing soft capsules are as follows:

取处方量50%的金银花、浙贝母、红花,处方量2%的马勃,粉碎成细粉,过筛,混匀,备用;将莪术、桃仁、玄参、三棱、丹参、板蓝根、麦冬、泽泻、鸡内金、蝉蜕、木蝴蝶、蒲公英及金银花、浙贝母、红花、马勃四味药的粉碎后剩余量加加10倍、8倍水煎煮二次,每次2小时,合并煎液,滤过,滤液浓缩至相对密度为1.28~1.32(60℃)的稠膏,加95%乙醇使含醇量达60%,搅拌均匀,静置24小时,滤过,滤液回收乙醇,减压浓缩至相对密度为1.38~1.40(60℃)的清膏;加入制备的细粉及适量辅料混匀,干燥,粉碎,制成细小颗粒,加入植物油,制成软胶囊,即得。Take 50% of the prescription amount of honeysuckle, Zhejiang Fritillaria, safflower, and 2% of the prescription amount of puffballs, crush them into fine powder, sieve, mix, and set aside; use curcuma, peach kernels, scrophulariaceae, trigonum, salvia miltiorrhiza, and isatis root , Ophiopogon japonicus, Alisma, gallinacea, cicada slough, wood butterfly, dandelion, honeysuckle, fritillaria, safflower, and puffball. After crushing, add 10 times and 8 times the remaining amount of water to decoct twice. Combine the decoctions for 2 hours each time, filter, concentrate the filtrate to a thick paste with a relative density of 1.28-1.32 (60°C), add 95% ethanol to make the alcohol content reach 60%, stir evenly, let stand for 24 hours, filter After filtering, the filtrate recovers ethanol, and concentrates under reduced pressure to a clear paste with a relative density of 1.38-1.40 (60°C); add the prepared fine powder and appropriate amount of auxiliary materials, mix evenly, dry, pulverize, make fine particles, add vegetable oil, and make a soft paste. capsules, ready to serve.

实施例5  该发明在治疗声带小结,声带息肉疾病的药物中的应用Example 5 Application of the invention in the treatment of vocal cord nodules and vocal cord polyposis

马勃25g,莪术(醋炒)50g,金银花125g,桃仁50g,玄参125g,三棱(醋炒)50g,红花50g,丹参75g,板蓝根125g,麦冬100g,浙贝母75g,泽泻75g,蝉蜕75g,鸡内金(炒)50g,木蝴蝶75g,蒲公英125g,制成1000粒,0.4g/粒,患声带小结,声带息肉的患者,口服,每次2-4粒,每日2次。25g of puffball, 50g of curcuma (stir-fried with vinegar), 125g of honeysuckle, 50g of peach kernel, 125g of scrophulariae, 50g of three-lens (stir-fried with vinegar), 50g of safflower, 75g of salvia miltiorrhiza, 125g of Radix Radix, 100g of Ophiopogon japonicus, 75g of fritillaria, Alisma 75g, cicada slough 75g, gallinaceous gold (fried) 50g, wood butterfly 75g, dandelion 125g, made into 1000 capsules, 0.4g/capsule, for patients with vocal cord nodules and vocal cord polyps, take orally, 2-4 capsules each time, daily 2 times.

Claims (4)

1, a kind of preparation technology who treats the Chinese medicine of vocal nodule, polyp of vocal cord symptom is characterized in that this preparation technology is:
The prescription: Lasiosphaera Seu Calvatia 25g, Rhizoma Curcumae 50g, Flos Lonicerae 125g, Semen Persicae 50g, Radix Scrophulariae 125g, rhizoma sparganic 50g, Flos Carthami 50g, Radix Salviae Miltiorrhizae 75g, Radix Isatidis 125g, Radix Ophiopogonis 100g, Bulbus Fritillariae Thunbergii 75g, Rhizoma Alismatis 75g, Periostracum Cicadae 75g, Endothelium Corneum Gigeriae Galli 50g, Semen Oroxyli 75g, Herba Taraxaci 125g;
Get Flos Lonicerae, Bulbus Fritillariae Thunbergii, the Flos Carthami of recipe quantity 40%-60%, the Lasiosphaera Seu Calvatia of recipe quantity 10%-30% is ground into fine powder, sieve, and mixing, standby; With Rhizoma Curcumae, Semen Persicae, Radix Scrophulariae, rhizoma sparganic, Radix Salviae Miltiorrhizae, Radix Isatidis, Radix Ophiopogonis, Rhizoma Alismatis, Endothelium Corneum Gigeriae Galli, Periostracum Cicadae, Semen Oroxyli, Herba Taraxaci and Flos Lonicerae, Bulbus Fritillariae Thunbergii, Flos Carthami, surplus adds 8-12 doubly after the pulverizing of Lasiosphaera Seu Calvatia four Chinese medicine, 6-10 times of decocting boils secondary, each 1-3 hour, collecting decoction, filter, in the time of 50-70 ℃, it is 1.28~1.32 thick paste that filtrate is concentrated into relative density, adding 90%-100% ethanol makes the alcohol amount of containing reach 50-70%, stir, left standstill 12-36 hour, and filtered filtrate recycling ethanol, in the time of 50-70 ℃, be evaporated to relative density and be 1.38~1.40 clear paste; The fine powder and the appropriate amount of auxiliary materials mixing that add preparation, drying is pulverized, and makes fine particle, promptly.
2, a kind of preparation technology who treats the Chinese medicine of vocal nodule, polyp of vocal cord symptom as claimed in claim 1 is characterized in that this preparation technology is:
The prescription: Lasiosphaera Seu Calvatia 25g, Rhizoma Curcumae 50g, Flos Lonicerae 125g, Semen Persicae 50g, Radix Scrophulariae 125g, rhizoma sparganic 50g, Flos Carthami 50g, Radix Salviae Miltiorrhizae 75g, Radix Isatidis 125g, Radix Ophiopogonis 100g, Bulbus Fritillariae Thunbergii 75g, Rhizoma Alismatis 75g, Periostracum Cicadae 75g, Endothelium Corneum Gigeriae Galli 50g, Semen Oroxyli 75g, Herba Taraxaci 125g;
Get Flos Lonicerae, Bulbus Fritillariae Thunbergii, the Flos Carthami of recipe quantity 50%, the Lasiosphaera Seu Calvatia of recipe quantity 20% is ground into fine powder, sieve, and mixing, standby; Surplus after the pulverizing of Rhizoma Curcumae, Semen Persicae, Radix Scrophulariae, rhizoma sparganic, Radix Salviae Miltiorrhizae, Radix Isatidis, Radix Ophiopogonis, Rhizoma Alismatis, Endothelium Corneum Gigeriae Galli, Periostracum Cicadae, Semen Oroxyli, Herba Taraxaci and Flos Lonicerae, Bulbus Fritillariae Thunbergii, Flos Carthami, Lasiosphaera Seu Calvatia four Chinese medicine is added 10 times, 8 times decoctings boil secondary, each 2 hours, collecting decoction, filter, in the time of 60 ℃, it is 1.28~1.32 thick paste that filtrate is concentrated into relative density, adding 95% ethanol makes and contains alcohol amount and reach 60%, stir, left standstill 24 hours, and filtered filtrate recycling ethanol, in the time of 60 ℃, be evaporated to relative density and be 1.38~1.40 clear paste; The fine powder and the appropriate amount of auxiliary materials mixing that add preparation, drying is pulverized, and makes fine particle, promptly.
3, Chinese medicine as claimed in claim 1 or 2 is in the application of the medicine of preparation treatment vocal nodule, polyp of vocal cord symptom, it is characterized in that: this medicine has the activating blood circulation to dissipate blood stasis function, can reduce whole blood viscosity, plasma viscosity, whole blood reduced viscosity, fibrinogen content and the attached rate of platelet; Inhibited to the chronic inflammatory disease granulation tissue hyperplasia.
4, Chinese medicine as claimed in claim 1 or 2 is characterized in that in the application of the medicine of preparation treatment vocal nodule, polyp of vocal cord symptom: this medicine is any in tablet, capsule, the granule.
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CN102363017B (en) * 2011-10-26 2013-04-03 西安碑林药业股份有限公司 Chinese medicinal composition having effects of clearing away heat and toxic materials, promoting blood circulation by removing blood stasis, removing dampness through diuresis and reducing phlegm and preparation method thereof
CN102363018B (en) * 2011-10-26 2013-04-03 西安碑林药业股份有限公司 Throat stagnation eliminating Chinese medicinal composition and preparation method thereof
CN108042698A (en) * 2018-01-19 2018-05-18 范鹏程 A kind of Chinese medicine composition for being used to treat polyp of vocal cord
CN109820988A (en) * 2019-04-03 2019-05-31 李瑞玉 It is a kind of to treat the swollen object Chinese medicine composition of vocal cords and preparation method

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金嗓散结丸药理研究、药效分析和临床观察. 傅彬.中国中西医结合耳鼻咽喉科杂志,第5卷第1期. 1997 *

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