TW457091B - A process for preparing Chinese herbs concentrate and the products thereof - Google Patents

Abstract

The products of preparing Chinese herbs concentrate are granulated by a fluid-bed process or using a high speed mixer. The dry extract of a formulated herbal drug that has been extracted with water is blent well with food grade surfactants which are dissolved in alcohol or water as a binder solution. These surfactants include sucrose fatty acid esters, sorbitan fatty acid esters, glycerin fatty acid esters and the mixture there of. By the process, the granules present a good stability, an easy flowability, and a relatively uniform particle size distribution. The granular products are much less hygroscopic and can disintegrated much easier compared to the original extracts. Using these processed granules to produce capsule or tablet products shows the same advantageous properties too.

Description

457 09 1 ′ Α7 Β7 V. Description of the invention () The invention is a dry extract obtained by extracting a traditional Chinese medicine formula with water, and using edible surfactants such as fatty acid sucrose esters or other polymer compounds in water, alcohol or The mixed solution is a binder, which is a concentrated Chinese medicine preparation obtained by mixing and granulating by spray drying or rapid rotation. The traditional Chinese medicine preparation has good fluidity, uniform particle distribution, and good moisture resistance after analysis of particle characteristics and stability tests Effect, good disintegration and dissolubility, and can be applied to capsule filling or direct ingot making. The moisture-proof effect and disintegration of the finished product are also #. The application of concentrated traditional Chinese medicine has gradually become Puyou, but because of the different ways of taking it, such as Shiqi Wan, San, Ointment, Dan and Tang, Jian, etc., Qunba Milu is very easy to absorb moisture, in the old process It is often necessary to add a high ratio of excipients -......... to maintain the stability of the formulation; but due to the complexity of the ingredients contained in natural products, it is likely to have an unexpected interaction with the added excipients It affects the absorption, metabolism, change of physicochemical properties and stability of active ingredients, etc., and further affects the pharmacological effect of the preparation and reduces the clinical treatment effect. Therefore, after extracting and drying the traditional Chinese medicinal materials with a solvent, adding a small amount or no excipients to make a stable and highly concentrated traditional Chinese medicinal form is the focus of the current need for improved technology. Although the concentration of traditional Chinese medicine is much lower than that of traditional Chinese medicine, compared with western medicine, the dose is still too large and inconvenient to swallow at once, which reduces the compliance of patients, reduces the willingness to use, and affects the treatment. Process and effect, reduce commodity prices. To solve this problem, the present invention uses the addition of edible surfactants, such as fatty acids (Sucrose fatty acid esters), fatty acid sorbitan (Sorbitan fatty acid esters), and fatty acid glycerides (glycerin fatty acid esters). Or other polymer compounds or without excipients, these edible surfactants can be used alone or in this way * 5. Use the "system", the grains are in or suspended in water, suitable essence or mixed solution to make 2 papers Zhang scale applies Chinese National Standard (CNS) Λϋ grid (21OX 297 mm)

457091 A7 _ 〆 B7 V. Description of the invention () Use. The granulation method is used to reduce the surface area of the traditional Chinese medicine dry extract in contact with the air to achieve the effect of preventing moisture. The stability of the finished product after testing and long-term observation is very high. The "prescription of Chinese medicine" referred to in the present invention is a prescription with a product name based on the original code, such as the excellent prescriptions of Yizong Jinjian, Yifang Jixie, Compendium of Materia Medica or Chinese Medical Dictionary, Chinese Pharmaceutical Dictionary, etc. The Department of Health of the hospital has published the traditional Chinese medicine benchmark party, which is authoritative and generally recognized as a traditional Chinese medicine preparation. The invention is to heat and boil the traditional Chinese medicine composition with 10 to 20 times the amount of pure water. After a certain period of time, the leaching solution obtained is concentrated under reduced pressure at 40 ° C to 65 ° C-to remove part of the water and dry it with air or spray. Obtain the dry extract; then mix the dry extract with a mobile layer spray dryer or a rapid mixing granulator, and then add fatty acid sucrose ester, fatty acid sorbose ester, fatty acid glycerol vinegar or a mixture thereof, the amount of which is used for dry extraction The weight of the paste is 1 to 15%, which is obtained by dissolving or suspending in water, alcohol or a mixed solution, and then kneading or granulating for several minutes and drying. In order to further explain the features and technical contents of the present invention, please refer to the following detailed description of the present invention. Example 1: Preparation method of Liuwei Dihuang Pill The composition of the medicinal materials used in this example is as follows: Rehmanniae Radix et Rhizomac 3200 g ★ Corni Fructus 1600 g D Dioscoreae Rhizoma 160G g% r. Aiismatis Rhizoma 1200 g 1 » * I peony skin Moutan Radicis Cortex 1200 g / λ <. Poria Hoelen 1200 g clothing paper scale applicable to Chinese national standard twin (CMS) A4 grid (210X297 mm) ^ j * Bundle :, order " '- J '(Please read the notes on the back before filling in this page) :.

V 45709 1 A7 B7 V. Description of the invention (The steps are as follows: 1) The above medicinal materials are shouted for 1G kg of paste G ~ pure water heated for several hours and then centrifuged for centrifugation. 2. Take the leachate obtained in step 1 above. After being concentrated under reduced pressure at 40 ° C ~ 65 ° C, it is dried by air drying or spraying to obtain a dry extract of about 2000 grams. About 2000 grams of more than 100 grams of raw medicinal materials are used to make dry extracts using fatty acid sucrose esters 3 .Extract about 2,000 grams of the dry extract from the crude drug obtained in the above step 2 into a rapid mixing granulator and mix for a few minutes. 4. Add 100 grams of fatty acid sucrose ester to mix appropriate alcohol, water or alcohol / water The mixed solution is dissolved or suspended, and sieved through the mesh of No. 100 or 200. 5 Slowly spray the solution obtained in the above step 4 into the dry extract obtained in the above step 3, and mix or granulate for several minutes. 6. Move to the flow The layer spray dryer is dried in hot air at 30 ° C ~ 75 ° C. 7. After sieving through No. 20 or No. 24 sieve, the finished product is obtained. Example 2: Preparation of Liuwei Dihuang Pills The medicinal materials used in this example The composition is as in Example 1. The steps are as follows: 1. The above medicinal materials are composed of 10 kg. 100 ~ 200 liters of pure water is heated and boiled for several hours after centrifugation; it is considered. Good paper scales are generally Chinese National Standard (CNS) A4 (21 ϋ X 297 mm) η Α7 Β7 Description of the invention (take the leaching solution obtained in step 1 above) After being concentrated under reduced pressure at 40 ° C ~ 65 ° C, it is dried by air drying or spraying to obtain a dry extract of about 2000 g. The above raw medicinal materials are used to make a dry extract of about 2000 g of fatty acid sucrose ester 100 g 3. Draw about 2,000 grams of the dry extract from the crude drug obtained in step 2 above and place it in a mobile layer spray dryer and mix for a few minutes. 4. 100 grams of fatty acid sucrose ester to mix appropriate alcohol, water or alcohol / water The mixed solution is dissolved or suspended, and sieved through a No. 100 or 200 sieve. 5. Slowly spray the solution obtained in step 4 into the dry extract obtained in step 3, and mix or mix the granules for several minutes. 6. Continue with 3G ° C ~ 75 ° C After hot air drying, the finished product is obtained by sieving through No. 20 or No. 24 sieve. Example 3: The method of making Shiquan Dabu Decoction, the composition of the medicinal materials used in this example is as follows: Poria Hoelen 1500 g Atractylodis Rhizoma W. 1500g Ginsen g Radix 1500 grams Rehmanniae Radix et Rhizomac 1500 grams (please read the note on the back before filling in this page) 丨 installed. The size of the paper waves applies the Chinese Garden Standard (CNS) Λ4ΛGrid (210X297mm4 5? Q v.〆A7 B7 5. Description of the invention (Paeoniae Lactiflorae Radix, Glycyrrhizae Radix (Mele), Pager, Astragail Radix, Cinnamomi Bark, Angelicae Sinensis Radix, Ligustici Wallichii Rhizoma, 1500 grams, Zingiberis Rhizoma Zizyphi Fructus 1000 grams is as follows: 1 · 17 ~ 5 kg of the above medicinal material composition is heated and boiled with 175 ~ 350 liters of pure water for several hours and centrifuged for filtration. 2. Take the leaching solution obtained in step 1 and concentrate it under reduced pressure at 40 ° C ~ 65 ° C, then dry it with air or spray to obtain about 3500 g of dry extract. 1500 grams 1500 grams 1500 grams 1500 grams 1500 grams {Please read the precautions on the back before filling in this page} 丨 Fill with a dry extract of more than 1T raw materials and use fatty acid sucrose esters about 3500 grams Π 5 grams of the crude drug obtained in step 2 above Draw out about 3500 grams of dry extract and put it into a rapid mixing granulator, mix for a few minutes. S Dissolve or suspend the fatty acid sucrose ester to dissolve or suspend the appropriate alcohol, water or alcohol / water mixture, and use 100 or 200 The sieve teacher sprays the solution obtained in step 4 above into the dry extract obtained in step 3 above, and mixes or granulates for several minutes. Move to the mobile layer spray dryer and dry it with 3 (rc: 75 " c hot air. -Vtf. -JM ·· 'ί: * f Wave ruler is applicable 1 ¾ Gujia standard Chinese (CNS) Λ 4 grid (plus X do not (Gongchu) 457 0 9 1 A7 _____B7 V. Description of the invention () 7 * After sieving through a No. 20 or No. 24 sieve, the finished product will be obtained. Example 4: Preparation method of Shiquan Dabu Decoction The medicinal materials used in this example The composition is as in Example 3. The steps are as follows: 1. The above-mentioned medicinal material composition 17.5 kg is heated and boiled for a few hours with 175 ~ 350 liters of pure water, and then centrifuged. 2 · Take the leaching solution obtained in the above step 1 at 40. 〇 ~ 65. ≪: After concentrating under reduced pressure, dry with air or spray to obtain about 3500 g of dry extract. About 3,500 g of dry extract made from the above raw medicinal materials, use 175 g of fatty acid sucrose ester 3 · Put about 3,500 grams of the raw medicine pomelo dry extract from step 2 into a fluidized layer spray-drying machine and mix for a few minutes. 4. Add 5 grams of fatty acid sucrose esters to prepare an appropriate alcohol, water or alcohol / water mixture Dissolve or suspend it and sieve through a No. 100 or 200 sieve. 5. Add the solution obtained in step 4 above to Xu Shi In the dry extract obtained in step 3, mix or granulate for several minutes. 6 · Continue drying with 3 (TC ~ 75 ° C hot air, and then sieve through a No. 20 or No. 24 sieve to obtain the finished product. Example 5: Jingfang How to make Baidusan ^ --- „---- i ------- Order (谙 Read the precautions on the back before filling in the 'Page) Dongweilang scale is applicable to Chinese national standard (〇 ^) 4 叱 grid (2 丨 0 \ 297 public release) 4 5 7 0 9 1 A7 B7 V. Description of the invention () The composition of the medicinal materials used in this example is as follows: Jing Fen Schizonepetae Herba 1500 g windproof Ledebouriellae Radix 1500 g live Notopterygii Rhizoma 1500 Gradual Angelicae Laxiflorae Radix 1500 Gram Bupleurum Bupleuri Radix 1500 Gram Pucedami Radix 1500 Gram Ligustici Wallichii Rhizoma 1500 Gram Aurantii Fructus 1500 Gram Platycode Radix 1500 Gram Hoelen 1500 Gram Radix Giza Giza Zingiberis Rhizoma 1500 grams of mint Menthae Herba 500 grams The steps are as follows: 1. 17.75 kg of the above medicinal materials are heated and boiled with 177 ~ 355 liters of pure water for several hours and centrifuged. 2. Take the leaching solution obtained in step 1 and concentrate it under reduced pressure at 40 ° C ~ 65 ° C, and then dry it with air or spray to obtain about 3550 g of dry extract. About 3550 grams of dry extracts made from the above raw medicinal materials are used. 180 grams of fatty acid sucrose esters are used. 3. About 3550 grams of the raw medicine grapefruit dry extracts obtained in the above step 2 are placed in fast-food paper. Present case (2) ϋΧ297 公 总) --r --- „----- ^ ------ ΐτ --------- swimming (please read the precautions on the back before filling this page) 457091 〆A7 _____ B7 V. Description of the invention () Speed mixing granulator, mixing for several minutes. 4 · Dissolve or suspend 18 g of fatty acid sucrose ester to dissolve or suspend the appropriate alcohol, water or alcohol / water mixture, and use No. 100 or No. 200 sieve. 5. Slowly spray the solution obtained in the above step 4 into the dry extract obtained in the above step 3, mix or granulate for several minutes. Β · Move to the mobile layer for spray drying The machine is dried with hot air at 30X ~ 75 ° C. 7. After sieving through No. 20 or No. 24 sieve, the finished product is obtained. Example 6: Preparation of Jingfang Baidu Powder The composition used in this example is as in Example 5. The steps are as follows: 1. The above-mentioned medicinal material composition 17.75 kg is heated and boiled for several hours with 177 ~ 355 liters of pure water, and then centrifuged for filtration. 2. Take step 1 The extract is concentrated under reduced pressure in 4 (rc ~ 65 < ic), and then dried by air drying or spraying to obtain a dry extract of about 3550 grams. About 3550 grams of 180 grams of raw medicinal materials are used to make dry extracts. Fatty acid sucrose esters -i--. Throw I: * v; *-^ J Μ 4 Put the raw _ material from the above step 2 into a mobile butcher salt dryer and mix for a few minutes. 180 grams of sweet and sour solution is dissolved or suspended with an appropriate fine / water mixture, and sieved with a sieve. Alcohol, water or wine No. 100 or 200

9 457091 A7 B7 V. Description of the invention (5) Slowly spray the solution obtained in the above step 4 into the dry extract obtained in step 3 'and mix or granulate for several minutes. 6 ‘continued with 30 ° C ~ 75 ° C hot air drying, then sieved through a No. 20 or No. 24 screen to obtain the finished product. In the above embodiment, the fatty acid sucrose ester can be replaced with a fatty acid sorbose ester or a fatty acid glyceride, and the effect is equivalent. Example 7 The traditional Chinese medicine preparations prepared in Examples 1 to 6 of the present invention were used to test the stability and moisture resistance of the accelerated stability test, thin-layer chromatographic analysis comparison and moisture content determination test. The test conditions were: The relative humidity is 75%, and the moisture content is determined under the conditions of 8 {rc, 30 minutes of drying and weight loss. The test results are shown in Tables 1 to 3. Table 1 shows the test results of Liuwei Dihuang Wan (Example 1 and Example 2). Table 2 shows the test results of Shiquan Dabu Decoction (Examples 3 and 4). Table 3 shows the test results of Jingfang Baidu San (Examples 5 and 6). From Tables 1 to 3, it can be seen that the traditional Chinese medicine preparation of the present invention has a long hygroscopic time and a low hygroscopic degree, that is, it has good moisture resistance and stability. i-I-II I 1 ...... 1 I 1 ^ 1 I ^^ 1 -------:: (Please read the notes on the back before copying the text «)

«Le scale general _ house quasi (cNS) A4 size (210X 297 mm) 457091 A >. B7 V. Description of the invention () Table 1 I Liuwei Dihuang Wan temperature (° C) time (days) dry extract Water content% Example 1 Water content% Example 2 Water content% Aluminum foil packet polyethylene bottle Aluminum foil packet polyethylene bottle Aluminum foil packet polyethylene bottle 25 15 5.11 5.12 2.51 2.32 3.00 3.22 25 30 5.20 5.41 2.71 2.42 3.51 3.70 25 60 6.28 6.99 2.72 2.90 3,52 3.82 25 90 6.42 7.62 2.51 2.88 3.72 3.83 40 15 5.41 5.61 2.72 2.79 2.90 3.01 40 30 5.62 6.29 2.81 3.01 3.84 3.97 40 60 6.69 7.91 2.79 3.58 3.79 4.08 40 90 6.81 8.31 2.88 3.62 3.89 4.19 50 15 4.91 6.40 3.07 3.51 3.89 3.99 50 30 5.99 7.39 3.18 3.61 4.11 4.21 50 60 7.59 8.68 3.52 4.42 4.32 4.53 50 90 8.11 9.29 4.10 4.62 4.48 4.97 | Control group * 1. 4 1. 51 1. 58 | Note: The control group is in accordance with the present invention The water content of the concentrated traditional Chinese medicine preparation before the test was%. 11 This paper is scaled to the Chinese National Standard (CNS) Λ4 specification (210X297 mm) --- J ---- 1¾ .------ 1T ------. ^ (Please read the Note: Please fill in this page again) 457091 A7 B7 V. Description of the invention () Table 2: Shiquan Dabu soup temperature time dry extract water content% Example III water content% Example IV water order% CC) (day) Aluminum foil packet polyethylene bottle Aluminum foil packet polyethylene bottle Chain box packet polyethylene inexpensive 25 15 4.12 4.29 1.99 2.01 2.08 2.40 25 30 4.27 5.06 2.23 2.13 2.84 2.48 25 60 4.82 5.84 2.43 2.39 2.90 3.02 25 90 5.33 6.07 2.52 2.38 3.01 3.22 40 15 4.34 4.61 2.19 1.98 2.11 2.12 40 30 4.53 5.28 2.70 2.79 2.97 3.01 40 60 4.67 5.82 2.68 3.18 3.12 3.12 40 90 5.01 7.47 2.51 2.49 3.24 3.41 50 15 4.93 5.37 2.07 2.50 2.68 2.61 50 30 5.97 6.40 3.17 2.63 3.43 2.44 50 60 6.45 7.11 3.31 3.37 3.53 2.99 50 90 6.94 8.87 3.26 3.57 3.69 4.29: 耝 0. 4 1. 01 1. 24 (Please read the precautions on the back before filling out this page)-Install '.14 rf: p ··' ^ 二. &Quot;! Τ '·' · ν '' Where the note: the control group is according to the present invention Method prepared concentrate formulation in medicine before the test% water content. '' The standard of Muling is applicable to the national standard of the country (210 × 29 " male tortoise) 457 09 1 A7 B7 V. Description of the invention (^ Table III: Temperature and time content of water resistance in dysentery) Example Three Water Content% Throughout Example 4; Content% CC) (days) Aluminum foil packet polyethylene bottle Aluminum foil packet polyethylene bottle @ foil packet polyethylene bottle 25 15 4.63 4.80 1.97 1.95 2.01 2.22 25 30 4.79 5.51 2.13 2.09 2.77 2.44 25 60 5.30 6.09 2.35 2.27 2.91 2 95 25 90 5.81 6.54 2.48 2.39 --- ~ 3.07 3.12 40 15 4.47 5.01 2.08 2.11 2 22 40 30 5.07 5.74 2.65 2.69 --- 2.87 2 90 40 60 5.26 6.06 2.74 3.08 3.01 3 〇9 40 90 5.63 6.37 2.75 3.28 3.22 50 15 5.43 5.88 2.12 2.44 2.48 / ----- 2 7R 50 30 6.42 6.96 2.59 2.52 2.53 50 60 6.95 7.60 3.01 3.47 2.94 50 90 7.42 9.00 3.17 3.44 ------ 3.21 A Cr \ Control group 1. 21 1. 38 ___ 1.50 Note *: The control group is the water content% of the concentrated traditional Chinese medicine preparation prepared according to the method of the present invention before testing. {Please read the notes on the back before filling this page]-^^ 1 · 1-»*; i ** — < ϋ-1 m! I-Order

: / · 'J Therefore, it is clear that the above-mentioned specific embodiments are used to describe the purpose, features, and effects of the present invention in detail. For those who are familiar with such techniques, according to the above description, there may be miscellaneous changes to this specific embodiment and Status, and it is out of the spirit of the present invention ... The scope of the patent of this invention is only by applying for a patent. For example, 13 winter paper-like materials_ $ 县 (CNS) A4 ^ r21〇X 297 ^

VI

Claims (1)

Attachment II & Month "ε; & Second! Patent No. 0851200244, please amend the scope of the patent (June 26, 89) 1. A method for preparing a concentrated Chinese medicine preparation, which includes the following steps: 1) The appropriate Chinese medicine formula is added with 10-20 times the amount of pure water and boiled together to obtain the concentrated extract, and the dry 'paste' obtained after vacuum drying or spray drying; 2) using a flow ^ spray dryer or rapid mixing to make After the granulator is mixed uniformly, add fatty acid sucrose ester, fatty acid sorbose ester, fatty acid glyceride or a mixture thereof, wherein the fatty acid part is selected from a group including hard fatty acid, oleic acid, palmitic acid and lauric acid, and the amount used is dry soaking The weight of the paste is 15%, which is dissolved or suspended in water, alcohol or a mixed solution thereof; and 3) It is made by mixing, granulating at a temperature of 30t: ~ 75 ° C, and sieving after drying. 2. According to the method for preparing a traditional Chinese medicine preparation according to the scope of patent application, the use amount of fatty acid sucrose ester, fatty acid sorbose ester, and fatty acid glyceride is equivalent to 4-10% of the dry extract is better. 457091 A5 B5 Four Chinese Abstracts (The name of the invention is a concentrated Chinese medicinal preparation and its preparation method amended in: This bucket of fat or glutamate disintegrates the disintegrating fat essence and dissolves it, and the K liquor production test loose fruit, and the synergistic collapse effect # 水 混 定, tide dipping formula Anguo's anti-dry ingredients and effects can be combined to analyze the tide, transform the ingredients, and prevent the quick speed of the extract. The points are quick and particularly good. Use high-quality or high-quality ingots to make the dry warp and beat. Prescription or aerosol, spraying uniformly, or medicinal medications are filled with active and middle cloth, and the capsules are seed capsules. The granule-granular mixture is used for food adhesion and can be used as medicine. Jiayingming and other liquids can be neutral. Hair esters dissolve and condense, and the sugar can be mixed together. It can also be mixed with sugar. The acid can be obtained. Mtil-Ming Mingming, Ben Wu: 4-.4 sticks whether The original substance of the change is printed in English by the Consumers Cooperative of the Central Bureau of quasi-bureau of the Ministry of Economics (the name of the invention: A Process for Preparing Chinese Herbs Concentrate and The Products there of The products of preparing Chinese herbs concentrate are granulated by a fluid-bed process or using a high speed nixer. The dry extract of a fo raulated herbal drug that has been extracted with water is blent well with food grade surfactants which are dissolved in alcohol or water as a binder solution. These surfactants include sucrose fatty acid esters, sorbitan fatty acid esters, glycerin fatty acid esters and the nixture there of . By the process, the granules present a good stability, an easy flowability, and a relatively uniform particle size distribution. The granular products are much less hygroscopic and can disintegrated much easier coopared to the original extracts'. Using these processed granules to produce capsule. or tablet products shows t; he same advantageous properties too. ------_------ ^ ------ tr ----- (Please read the precautions on the back before filling this page (Columns) This paper uses China's national kneading rate (CNS) A4 (210X297 mm). Attachment II: & Month "ε; & II! Patent No. 0851〇244〇, please amend the scope of the patent ( (June 26, 89) 1. A method for preparing a concentrated Chinese medicine preparation, which includes the following steps 1) Add 10-20 times the amount of pure Chinese medicine to the proper Chinese medicine formula and boil it together to obtain the concentrated extract, and dry it after vacuum drying or spray drying; 2) Use a flow ^ spray dryer or fast After the granulator is mixed uniformly, the fatty acid sucrose ester, fatty acid sorbose ester, fatty acid glyceride or mixture thereof is added, wherein the fatty acid part is selected from a group including hard fatty acid, oleic acid, palmitic acid and lauric acid, and the amount used is 15% by weight of dry extract, which is dissolved or suspended in water, alcohol or a mixed solution thereof; and 3) is then mixed, granulated at a temperature of 30t: ~ 75 ° C, and sieved after drying to make. 2. According to the method for preparing a traditional Chinese medicine preparation according to item 1 of the application, wherein the amount of fatty acid sucrose ester, fatty acid sorbose ester, and fatty acid glyceride equivalent to 4 to 10% of the dry extract is preferred. '