JPH0469608B2 - - Google Patents

Description

[Detailed description of the invention]

[Industrial Field of Application] The present invention relates to a method for producing a Chinese herbal medicine extract in the pharmaceutical industry. [Prior Art] Herbal medicines have been used as Chinese herbal medicines since ancient times, and their Chinese herbal prescriptions are described in many classics (Shokanron, Kinki Yoryo, etc.) as the accumulation of many years of experience. However, according to the classics, decoctions, in which the ingredients of Chinese herbal medicines are extracted by cutting the herbal medicines each time and boiling them with water, are not only difficult to take due to their unique medicinal odor and taste, but also require a lot of time and effort. And it takes time. Currently, in the field of medical drugs, Chinese herbal medicine extracts are being used, which do not require the above-mentioned work and are easy to take. It's very convenient. This herbal medicine extract is usually made by extracting the cut herbal medicine with water or alcohol, leaving the extract as it is or concentrating it, and drying it to make a herbal medicine extract powder, which is then added with an appropriate excipient (lactose, cornstarch, starch, etc.). Add and mix to prepare various dosage forms (tablets, capsules, powders, fine granules, granules, etc.)
It is obtained by a method of manufacturing. [Problems to be Solved by the Invention] As described above, in the production of Chinese herbal medicine extracts, steps such as concentration and drying are added to the above-mentioned extraction step. However, it has been reported that during this concentration, drying, etc. process, volatile components, which are part of the components of Chinese herbal medicine that should be contained in appropriate amounts in the extract, are dissipated together with water [ Akahori et al., Journal of Pharmaceutical Sciences, 32 , 24 (1978)]. In addition, it has been pointed out that in the case of Chinese herbal medicine extracts that concentrate multiple ingredients, the problem is that the ingredients must be kept stable for a long period of time [Toriizuka et al., Hospital Pharmacy,
Vol10, No.1 (1984), p.29-34]. The object of the present invention is to provide a method for producing a Chinese herbal medicine extract whose components are stable over a long period of time by supplementing the volatile components that are dissipated as described above in the Chinese herbal medicine extract. [Means for Solving the Problems] The present inventors have sought a method for producing a Chinese herbal medicine extract in which the volatile components that are dissipated as described above are supplemented with a Chinese herbal medicine extract, and the ingredients are stable over a long period of time. As a result of intensive research, we have found that we can extract Chinese herbal medicine with an extraction solvent, concentrate the extract, and dry it to obtain a Chinese herbal medicine extract powder. condensate, and use this condensate as it is or concentrate it,
Mix with one or more excipients selected from saccharides, starches, dextrins, silicic acid compounds, cellulose, gum tragacanth, and gum arabic, and mix the powder obtained by drying with the above herbal medicine extract powder. By doing so, they discovered that it was possible to obtain a Chinese herbal medicine extract that contained volatile components that would dissipate with the extraction solvent and whose components remained stable over a long period of time, and completed the present invention. The present invention will be explained in detail below. The herbal medicines used in the present invention include not only herbal medicines referred to in Chinese medicine, but also so-called herbal medicines or pharmaceutical preparations consisting of one type of herbal medicine or a mixture of two or more types of herbal medicines. Specific examples of Chinese herbal medicines are listed in the General Chinese Herbal Prescription Guide (supervised by the Pharmaceutical Affairs Bureau of the Ministry of Health and Welfare, published by Yakuji Jihosha, January 8, 1980, 4th edition, 6th printing) and Tsumura Medical Chinese Herbal Preparations [General Catalog]. Chinese herbal prescriptions are listed, and more specifically, kakkonto,
Kakkonto Kagawa = Shinyi, Keishikashakuyaku Daioto, Annachusan,
Hachimijiogan, Saiko Keishito, Saiko Keishi Kenkyoto, Goreisan, Keishikazutsuketo, Shoseiryuto, Tokishakuyakusan, Kamishoyosan, Keishibukureimaru, Keishikaryukotsu Oyster Hot water, Mao-to, Kibo-mi-to, Toki-shi-gyaku-kago-shu-ginger-to, Reiki-keishu-kan-to, Keishi-to, Juzen-tai-ho-to, Jingku-ren-kei-to, Tetsu-nin-to, Sokeikakketsu-to, Yokukan San, Kiyojobofuto, Keishikashakuyakuto, Tokokujokito, Bofutsushosan, Goshasan, Bokanzoto, Megamisan, Kososan, Keishininjinto, Yokukansankachenpihan Summer, healing bruises, Kokenchuyu, Tokiyu, Onkeito,
Examples include Gosha-Jinki-gan, Sairei-to, Shirei-to, Fukurei-drinkai Hanka Koboku-to, and Gorei-san. Specific examples of crude drugs include the Illustrated Encyclopedia of Japanese and Chinese Medicine in Primary Colors (Volumes 1 and 2, written by Tsuneo Namba, published by Yokusha Co., Ltd., April 1, 1982).
Examples include the herbal medicines listed in the Japanese Pharmacopoeia (Japan) and the 10th revised Japanese Pharmacopoeia [supervised by the Japan Compendium Association, published by Hirokawa Shoten (p.863-p.1278)]. Extraction solvents for Chinese herbal medicines include water, ethanol aqueous solution, acetic acid aqueous solution, etc., and hot extraction or cold extraction may be used, especially hot extraction using water at 90 to 100°C. is preferred. To concentrate the extract, vacuum concentration is generally used. Specifically, vacuum concentration is performed under conditions of a degree of vacuum of 30 to 70 mmHg and an evaporation temperature of 100°C or less, preferably 30 to 50°C. Next, this concentrated liquid is dried to obtain a Chinese herbal medicine extract powder using an appropriate drying method such as a commonly used spray drying method, vacuum drying method, or freeze drying method. As for specific drying conditions, for example, in the case of a spray drying method, a concentrated liquid is sprayed from an atomizer into a stream of hot air in a drying chamber kept at a high temperature of 60 to 300°C, and the solvent is instantaneously evaporated. In the case of the vacuum drying method, the concentrate that has been sufficiently concentrated under vacuum is dried for 5 minutes under a vacuum of 760 mmHg or less.
Dry at ~100℃. In the case of the freeze-drying method, the concentrate is cooled to -80 to 0°C to freeze, and the solvent is directly sublimated and dried in a vacuum of 1 mmHg or less. Volatile components are recovered by using a condenser to collect the extraction solvent vapor generated during extraction and/or concentration at a condensation temperature of 100°C or lower, preferably
This can be achieved by condensing at a temperature below 40℃. This condensate is in a state where the volatile components and extraction solvent are dispersed (some volatile components are dissolved in the extraction solvent), and even if it is moved to the next step of mixing with excipients. However, the condensate may be concentrated and then mixed with excipients. Examples of the concentration include a method of distillation using a distillation column, a method of freeze concentration, a method of membrane concentration, and the like. Next, when mixing the condensate and excipients, it is desirable to dissolve or disperse them more uniformly using a homogenizer, etc. The specific mixing ratio is based on the total weight of the condensate and excipients. Excipient weight 0.1-95
%, preferably 5 to 50%. Specific examples of sugar excipients include mannitol, sucrose, cerbitol, glucose, fructose, maltose, lactose, etc., and specific examples of starch excipients include corn starch, soluble starch, carboxymethyl starch, etc.
Specific examples of dextrin excipients include dextrin and cyclodextrin, specific examples of silicic acid compound excipients include porous silicic anhydride, ultrafine silicic anhydride, etc., and cellulose excipients. Specific examples of excipients include crystalline cellulose,
Examples include carboxymethylcellulose, caleboxymethylcellulose calcium salt, caleboxymethylcellulose sodium salt, etc., specific examples of gum tragacanth excipients include gum tragacanth, and specific examples of gum arabic excipients include gum arabic. . Furthermore, this condensate and excipient mixture is spray-dried,
Dry using an appropriate drying method such as vacuum drying or freeze drying. Specific drying conditions are the same as those described above. The thus obtained powder containing volatile components and the above-mentioned herbal medicine extract powder are mixed by ordinary powder mixing using, for example, a mixer.
The specific mixing ratio is 10 to 90% of the powder containing volatile components to the total weight of the powder containing volatile components and the herbal medicine extract powder, and if necessary, the powder containing volatile components may be added to the powder that does not retain anything. Excipients may also be added. In the present invention, it is important to mix the powder containing volatile components obtained as described above with the herbal medicine extract powder. In other words, if a method is adopted in producing a Chinese herbal medicine extract, volatile components dissipated during extraction and/or concentration are recovered and added at any step during the manufacturing process of the Chinese herbal medicine extract. It is possible that volatile components are retained in the
Mixing the powder containing the volatile component with the herbal medicine extract powder as in the present invention,
This is because it is particularly superior in terms of long-term stability of the contained components compared to other cases. For example, as an example of a method in which the recovered volatile components are added at any step during the manufacturing process of a herbal medicine extract, the herbal medicine is extracted with an extraction solvent, the extract is concentrated to obtain a concentrated liquid, and at the same time, the extraction The extraction solvent vapor containing volatile components generated during extraction and/or concentration is condensed, and the condensed liquid is added to the above concentrated liquid as it is or concentrated, and further dried to obtain a Chinese herbal medicine extract powder. A method of adding appropriate excipients (lactose, corn starch, starch, etc.) to the final product and mixing them to form various dosage forms (tablets, capsules, powders, fine granules, granules, etc.) (hereinafter referred to as the comparative method) ) can be mentioned. However, the long-term stability of the components contained in the herbal medicine extract obtained by the present invention is far superior to that of the herbal medicine extract prepared by the comparative method, as shown in the experimental examples described later. Next, the mixture of the volatile component-containing powder obtained above and the herbal medicine extract powder is subjected to operations such as granulation, sizing, and tableting as necessary to form granules, fine granules, and powders. , made into capsules, tablets, etc.
Make it into a Chinese herbal medicine extract. Granulation methods include a general dry granulation method and a wet granulation method, with the dry granulation method being preferred. [Effects of the Invention] The effects of the present invention include the following points. The components contained in the Chinese herbal medicine extract obtained by the present invention are stable over a long period of time. Experimental examples in which the Chinese herbal medicine extract obtained according to the present invention exhibits excellent stability over a long period of time are as follows. In addition, as an example of a comparative control, a Chinese herbal medicine extract prepared by the above-mentioned comparative method was used. Experimental Example 1 Sample: Sample 1A: 10 g of Goreisan extract granules produced as described in Example 1 below. Sample 2A: 10 g of Juzentaihoto extract fine granules produced as described in Example 2 below. Sample 1B: Prescription crude drug Goreisan (Example 1 described below)
(described in Example 1 below), put 10 kg into the same extractor as described in Example 1 below, add 100 kg of water, heat and extract in the same manner as in Example 1 below, and after the extraction is completed, perform solid-liquid separation during hot extraction. A liquid was obtained, concentrated to about 1/4 at 40°C using a vacuum concentrator, and added to this concentrated liquid in the same manner as in Example 1 below.
After adding about 3 of the steam condensate obtained during the above heating extraction and mixing well, spray drying (air blowing at 150℃,
Exhaust air at 90°C) to obtain a dry extract powder. To 100g of this dry extract powder, add 400g of dextrin [manufactured by Matsutani Chemical Industry Co., Ltd.] and mix well.
10g of Goreisan extract granules compressed into 12 to 32 mesh granules. Sample 2B: Put 10kg of the prescribed crude drug Juzentaihoto (described in Example 2 below) into the same extractor as described in Example 1 below, and add 20% ethanol aqueous solution.
100 was added and extracted by heating in the same manner as in Example 2 below. After the extraction was completed, solid-liquid separation was performed during heating to obtain an extract, which was concentrated to about 1/4 at 40°C using a vacuum concentrator. , To this concentrated liquid, in the same manner as in Example 1 described later, about 3 steam condensate obtained during the heating extraction was added and mixed well, and then spray-dried (blow air 150 ° C, exhaust air 90 ° C), As a dry extract powder, among this dry extract powder
After adding 150g of dextrin to 100g and mixing well, compression molding is performed to obtain 10g of Juzen Taihoto Extract fine granules with a size of 32 to 150 mesh. Accelerated Test Conditions Each sample was placed in a glass container and left to stand for 6 months at 40°C and 75% RH using a constant temperature and humidity machine (manufactured by Tabai Seisakusho). High-performance liquid chromatography measurement Take 2 g of each of samples 1A, 1B, 2A, and 2B immediately after production, extract with 30 ml of ethyl acetate,
Waters High Performance Liquid Chromatography [Model 590, Column: Reversed phase packing material (250 mm x
4.6 mm), mobile phase: mixed solution of acetonitrile, water, and oxalic acid, flow rate: 1 ml/min, detection wavelength:
280 nm] to measure the analytical pattern. Six months after the accelerated test, 2 g of each sample was taken from Samples 1A, 1B, 2A, and 2B, and the analysis pattern was measured using the same method as described above. Results The high performance liquid chromatography analysis patterns of the sample before and after the 6-month accelerated test are shown in Figure 1 for Sample 1A, Figure 2 for Sample 1B, Figure 3 for Sample 2A, and Figure 4 for Sample 2B. As shown in the figure. In FIGS. 1 to 4, a shows the analysis pattern before the accelerated test, and b shows the analysis pattern after the accelerated test. As is clear from the results shown in Figures 1 to 4, samples 1A and 2A according to the present invention show almost no change in the peaks marked with 〓 even after 6 months, but samples 1B and 2B show 〓 A clear decrease in the peaks indicated by marks indicates that the stability of the components contained in Samples 1A and 2A according to the present invention is extremely excellent. Experimental Example 2 Samples: Sample 3A: 10 g of Keishibukuryogan extract granules produced as described in Example 4 below. Sample 4A: 10 g of Keishibukuryogan extract granules produced as described in Example 5 below. Sample 5A: 10 g of Keishibukuryogan extract granules produced as described in Example 7 below. Sample 6A: 10 g of Keishibukuryogan extract granules produced as described in Example 8 below. Sample 3B: Put 10 kg of Keishibukuryogan prescription herbal medicine (described in Example 3 below) into the same extractor as described in Example 1 below, add 100% water, and heat in the same manner as in Example 3 below. After the extraction is completed, solid-liquid separation is carried out under heat to obtain an extract, which is concentrated to about 1/4 at 40°C using a vacuum concentrator. After adding about 15% of the steam condensate obtained during the heating extraction process and mixing well, spray drying (air blowing)
150℃, exhaust air 90℃), add 400g of dextrin [manufactured by Matsutani Chemical Industry Co., Ltd.] to 100g of the dry extract powder and mix well.
3. 10 g of Keishibukuryogan extract granules compressed into 12 to 32 mesh granules. Sample 4B: 10 g of Keishibukuryogan extract granules produced in the same manner as Sample 3B above, except that cyclodextrin [trade name: Dexipearl, manufactured by Shiomiko Seito Co., Ltd.] was used instead of dextrin. Sample 5B: Put 10 kg of Keishibukuryogan prescription herbal medicine (described in Example 6 below) into the same extractor as described in Example 1 below, add 100 g of water, and heat in the same manner as in Example 6 below. After the extraction is completed, solid-liquid separation is carried out under heat to obtain an extract, which is concentrated to about 1/4 at 40°C using a vacuum concentrator. After adding about 15% of the vapor condensate obtained during the above heating extraction and mixing well, freeze-dry (freezing temperature -40°C, degree of vacuum 0.1 mmHg, shelf temperature 20°C),
It was further crushed to obtain a dry extract powder of 80 mesh or less, and 400 g of dextrin [manufactured by Matsutani Chemical Industry Co., Ltd.] was added to 100 g of this dry extract powder, mixed well, and compression molded to form granules of 12 to 32 mesh. Keishibukuregan extract granules 10g. Sample 6B: 10 g of Keishibukuryogan extract granules produced in the same manner as Sample 5B above, except that cyclodextrin [trade name: Dexipearl, manufactured by Shiomiko Seito Co., Ltd.] was used instead of dextrin. Accelerated Test Conditions Each sample was placed in a glass container and left to stand for 6 months at 40°C and 75% RH using a constant temperature and humidity machine (manufactured by Tabai Seisakusho). High performance liquid chromatography measurement At the start of accelerated testing for each sample, 1
After 2 months, 2 months, 3 months, and 6 months, 2 g each was collected, extracted with 30 ml of 50% methanol, and an analysis pattern was measured using high performance liquid chromatography manufactured by JASCO Corporation. column:
Reversed phase packing (250mm x 4.6mm) Mobile phase: Acetonitrile/acetic acid/water mixed solution, flow rate: 1ml/
min, detection wavelength: 280 nm, the peak area at the start of the accelerated test is set as 100 for component P1 detected around the retention time of about 17 minutes, and one month later,
The peak area for P1 was determined after 2 months, 3 months, and 6 months, and the residual rate of P1 was determined from the ratio to the peak area at the start of the test. Results The results are shown in Table 1.

[Table] From Table 1, samples 3A, 4A, 5A according to the present invention,
It can be seen that the long-term stability of component P1 contained in 6A is extremely excellent. Experimental Example 3 Samples: Sample 7A: 35 Goreisan extract tablets manufactured as described in Example 9 below. Sample 8A: 35 Goreisan extract tablets manufactured as described in Example 10 below. Sample 9A: 35 Goreisan extract tablets manufactured as described in Example 11 below. Sample 10A: 35 Goreisan extract tablets manufactured as described in Example 12 below. Sample 7B: Prescription crude drug Goreisan (Example 9 below)
10 kg) was placed in the same extractor as described in Example 1 below, 100 kg of water was added and extracted by heating in the same manner as in Example 9 below. After the extraction was completed, solid-liquid separation was performed during heating for extraction. A liquid was obtained, concentrated to about 1/4 at 40°C using a vacuum concentrator, and added to this concentrated liquid in the same manner as in Example 1 below.
About 15% of the vapor condensate obtained during the above heating extraction was concentrated to 5% using a tray distillation column in the same manner as in Example 9 described below. 90℃) and
Mannitol is added to 100g of this dry extract powder [manufactured by Towa Kasei Kogyo Co., Ltd.]
Add 400g, mix well, compress and mold into plain tablets, 35 Goreisan extract tablets. Sample 8B: Goreisan extract tablet manufactured in the same manner as Sample 7B above, except that cornstarch [manufactured by Matsutani Chemical Industry Co., Ltd.] was used instead of mannitol.
35 tablets. Sample 9B: Goreisan extract tablet 35 manufactured in the same manner as Sample 7B above, except that dextrin [manufactured by Matsutani Chemical Industry Co., Ltd.] was used instead of mannitol.
Tablet. Sample 10B: Crystalline cellulose instead of mannitol [Product name: Avicel, Asahi Kasei Corporation
35 Goreisan extract tablets manufactured in the same manner as Sample 7B above, except that the same method as Sample 7B was used. Accelerated Test Conditions Each sample was placed in a glass container and left to stand for 6 months at 40°C and 75% RH using a constant temperature and humidity machine (manufactured by Tabai Seisakusho). High performance liquid chromatography measurement At the start of accelerated testing for each sample, 1
After 2 months, 2 months, 3 months, and 6 months, 2 tablets each were collected, crushed, extracted with 30 ml of 50% methanol, and the analysis pattern was measured using high performance liquid chromatography manufactured by JASCO Corporation. .
Column: Reversed phase packing material (250mm x 4.6mm), Mobile phase: Mixed solution of acetonitrile, acetic acid, and water, Flow rate: 1ml/min, Detection wavelength: 280nm. Detected at a retention time of approximately 17 minutes. For component P2, the peak area at the start of the accelerated test is set to 100,
1 month later, 2 months later, 3 months later, 6 months later
The peak area for P2 was determined, and the residual rate of P2 was determined from the ratio to the peak area at the start of the test. Results The results are shown in Table 2.

[Table] From Table 2, samples 7A, 8A, 9A, according to the present invention,
It can be seen that the long-term stability of component P2 contained in 10A is significantly superior. Experimental Example 4 Samples: Sample 11A: 10 g of Annakasan extract powder prepared as described in Example 13 below. Sample 12A: 10 g of Annakasan extract powder prepared as described in Example 14 below. Sample 11B: Annachusan prescription herbal medicine (Example 13 below)
(described in Example 1 below), put 10Kg into the same extractor as described in Example 1 below, add 100kg of water, and prepare in Example 1 below.
Extraction was carried out by heating in the same manner as in step 13. After the extraction was completed, solid-liquid separation was performed during heating to obtain an extract, which was concentrated to about 1/4 at 40°C using a vacuum concentrator. In the same manner as in Example 1,
After adding about 15% of the steam condensate obtained during the above heating extraction and mixing well, spray drying (blow air at 150℃,
Exhaust air at 90℃) to dry extract powder, add 100g of this dry extract powder to 400g of porous silicic anhydride [Product name: Cyroid 266, manufactured by Fuji Co., Ltd.]
10g of Annakasan extract powder. Sample 12B: Soluble starch with 0.5% sucrose fatty acid ester added instead of porous silicic anhydride [sucrose fatty acid ester; trade name: Shugar Ester, manufactured by Hishito Co., Ltd., soluble starch; trade name: Stabilose, Matsutani Chemical Anchusan extract powder manufactured in the same manner as Sample 11B above except for using [manufactured by Kogyo Co., Ltd.]
10g. Accelerated Test Conditions Each sample was placed in a glass container and left to stand for 6 months at 40°C and 75% RH using a constant temperature and humidity machine (manufactured by Tabai Seisakusho). High performance liquid chromatography measurement At the start of accelerated testing for each sample, 1
After 2 months, 2 months, 3 months, and 6 months, 2 g each was collected, extracted with 30 ml of 50% methanol, and an analysis pattern was measured using high performance liquid chromatography manufactured by JASCO Corporation. column:
Reversed phase packing (250mm x 4.6mm), mobile phase: acetonitrile/acetic acid/water mixed solution, flow rate: 1
ml/min, detection wavelength: 280 nm measurement condition, the peak area of component P3 detected around the retention time of about 17 minutes is set to 100 at the start of the accelerated test, and after 1 month, 2 months, 3 months, and 6 months. The subsequent peak area for P3 was determined, and the residual rate of P3 was determined from the ratio to the peak area at the start of the test. Results The results are shown in Table 3.

[Table] From Table 3, it can be seen that the long-term stability of component P3 contained in Samples 11A and 12A according to the present invention is extremely excellent. Experimental Example 5 Samples: Sample 13A: 10 g of Hankakobokuto extract granules produced as described in Example 15 below. Sample 14A: 10 g of Hankakobokuto extract granules produced as described in Example 16 below. Sample 15A: 10 g of Hankakobokuto extract granules produced as described in Example 17 below. Sample 13B: Put 10kg of Hanka Kobokuto prescription herbal medicine (described in Example 15 below) into the same extractor as described in Example 1 below, add 100% water, and heat extraction in the same manner as in Example 15 below. After the extraction was completed, solid-liquid separation was performed during heating to obtain an extract, which was concentrated to about 1/4 at 40°C using a vacuum concentrator. After adding about 15% of the steam condensate obtained during the heating extraction process and mixing well, spray drying (air blowing)
150℃, exhaust air 90℃), dry extract powder,
100g of this dry extract powder contains soluble starch [Product name: Stabilose, Matsutani Chemical Industry Co., Ltd.]
Add 400g of product], mix well, and compression mold.
10g of Hankakobokuto extract granules with 32 pieces of granules. Sample 14B: Carboxymethyl cellulose calcium salt (trade name:
10 g of Hankakobokuto extract granules manufactured in the same manner as Sample 13B above except that ECG505, manufactured by Gotoku Yakuhin Kogyo LLC] was used. Sample 15B: 10 g of Hankakobokuto extract granules produced in the same manner as Sample 13B above, except that gum arabic powder [manufactured by Sankyo Foods Co., Ltd.] was used instead of soluble starch. Severity test conditions Each sample was left standing at 50°C for one week using a constant temperature and humidity machine. Thin layer chromatography measurement 2g of each sample was collected at the start of the severe test and one week later, extracted with 30ml of hexane, the extract was spotted on a silica plate, and a mixed solution of hexane, benzene, and ethyl acetate was extracted. Among the absorbance analysis patterns obtained by Shimadzu thin-layer densitometry (detection wavelength: 365 nm), the peak area at the start of the severe test was calculated for component P4, whose Rf value was detected around 0.5. 100 and P4 after another week
The peak area of P4 was determined, and the residual rate of P4 was determined from the ratio to the peak area at the start of the test. Results The results are shown in Table 4.

[Table] From Table 4, samples 13A, 14A, and
It can be seen that the stability of component P4 contained in 15A is significantly superior. [Examples] Hereinafter, the present invention will be explained in more detail with reference to Examples, but the present invention is not limited thereto. Example 1 Goreisan (Takshiya 3.94 parts, Seujiyutsu 3.02 parts,
Chiyorei 3.02 parts, Bukuriyo 3.02 parts, Keihi 1.50
Put 10 kg of prescribed herbal medicine (consisting of
100% of water was added and extracted by heating at 100°C. After the extraction was completed, solid-liquid separation was performed while hot to obtain an extract. Further, the extraction solvent vapor generated during the heating extraction was condensed in a shell and tube condenser (condensation temperature 40°C) to obtain a vapor condensate of approx. The extract was concentrated to about 1/4 using a vacuum concentrator at 40°C, and then spray-dried (blow air at 150°C, exhaust air at 90°C) to obtain a dry extract powder. On the other hand, 1.0 kg of dextrin [manufactured by Matsutani Chemical Industry Co., Ltd.] was added to the total amount of the vapor condensate obtained during the above heating extraction, and after uniformly dispersing and mixing using a homogenizer, spray drying (air blowing at 150°C, Exhaust air 90
℃) to obtain a dry dextrin powder containing volatile components. To 100 g of the dry extract powder obtained as above, 50 g of the above volatile component-containing dry dextrin powder and 350 g of dextrin powder were added, mixed well, and then compression molded to form granules of 12 to 32 meshes. Extract granules were obtained. Example 2 Juzentaihoto (3.0 parts of Aspergillus japonica, 3.0 parts of Keihi, 3.0 parts of Japanese sardine, 3.0 parts of Shayakuyaku, 3.0 parts of Senkiyu, 3.0 parts of Soujiyutsu, 3.0 parts of Japanese acanthus, 3.0 parts of carrot,
10 kg of the prescribed herbal medicine (consisting of 3.0 parts of Bukuriyo and 1.5 parts of Licorice) was placed in the same extractor as described in Example 1, and 80 kg of 20% ethanol aqueous solution was added.
Extraction was carried out by heating at ℃, and after the extraction was completed, solid-liquid separation was carried out during heating to obtain an extract. In addition, in the same manner as in Example 1, a steam condensate of about 30% by heat extraction was obtained. The extract was concentrated to about 1/4 at 40°C using a vacuum concentrator, and then spray-dried (blow air at 150°C, exhaust air).
90°C) and made into a dry extract powder. On the other hand, the total amount of the steam condensate obtained during the above heating extraction is
After adding 1.0 kg of dextrin [manufactured by Matsutani Chemical Industry Co., Ltd.] and uniformly dispersing and mixing using a homogenizer, the mixture was spray-dried (blow air at 150°C, exhaust air at 90°C) to obtain a dry dextrin powder containing volatile components. To 100 g of the dry extract powder obtained as above, 50 g of the volatile component-containing dry dextrin powder and 350 g of dextrin powder were added, mixed well, and compression molded to form granules of 32 to 150 mesh. Houto extract fine granules were obtained. Example 3 Keishibukuregan (keihi 3.0 parts, shiyakuyaku 3.0 parts,
Put 10kg of the prescribed herbal medicine (consisting of 3.0 parts of tonin, 3.0 parts of bukuriyo, and 3.0 parts of botanpi) into the same extractor as described in Example 1, add 100% of water, and heat extraction at 100℃. Solid-liquid separation was then performed to obtain an extract. Further, in the same manner as in Example 1, about 15% of steam condensate was obtained during heating extraction. The extract was concentrated to about 1/4 at 40°C using a vacuum concentrator, and then spray-dried (blow air at 150°C, exhaust air at 90°C).
℃) and made into a dry extract powder. On the other hand, the steam condensate obtained during the above heating extraction 15
7.5 kg of lactose (manufactured by Megre) was added to the mixture, and after uniformly dispersing and mixing using a homogenizer, the mixture was spray-dried (blow air at 150°C, exhaust air at 90°C) to obtain a dry lactose powder containing volatile components. After adding 50 g of the volatile component-containing dry lactose powder and 350 g of lactose powder to 100 g of the dry extract powder obtained as above and mixing well,
The mixture was compression molded into granules of 12 to 32 meshes to obtain Keishibukuryogan extract granules. Example 4 Dextrin [Matsuya Chemical Industry Co., Ltd.] instead of lactose
Keishibukuryogan extract granules were obtained in the same manner as described in Example 3, except that the same method was used as described in Example 3. Example 5 Cyclodextrin [trade name:
Keishibukuryogan extract granules were obtained in the same manner as described in Example 3, except that Dexipearl, manufactured by Shiosui Minato Seito Co., Ltd.] was used. Example 6 Keishibukuregan (keihi 3.0 parts, shiyakuyaku 3.0 parts,
Put 10kg of the prescribed herbal medicine (consisting of 3.0 parts of tonin, 3.0 parts of bukuriyo, and 3.0 parts of botanpi) into the same extractor as described in Example 1, add 100% of water, and heat extraction at 100℃. Solid-liquid separation was then performed to obtain an extract. Further, in the same manner as in Example 1, about 15% of steam condensate was obtained during heating extraction. The extract was concentrated to about 1/4 at 40°C using a vacuum concentrator, and then freeze-dried (freezing temperature -40°C, degree of vacuum 0.1 mmHg, shelf temperature 20°C) to form a dry extract powder. did. On the other hand, the steam condensate obtained during the above heating extraction 15
Add 7.5 kg of lactose (manufactured by Maigret Co., Ltd.) to the mixture, disperse and mix uniformly using a homogenizer, and then freeze-dry (freezing temperature -40℃, degree of vacuum 0.1mmHg, shelf temperature
20°C) and further crushed to obtain a dry lactose powder containing volatile components with a mesh temperature of 80°C or less. For 100g of the dry extract powder obtained as above, 50g of dry lactose powder containing volatile components is added.
g and 350 g of lactose powder were added and mixed well, and then compression molded into 12 to 32 mesh granules to obtain Keishibukuryogan extract granules. Example 7 Dextrin [Matsuya Chemical Industry Co., Ltd.] instead of lactose
Keishibukuryogan extract granules were obtained in the same manner as described in Example 6, except that the same method was used as described in Example 6. Example 8 Cyclodextrin [trade name:
Keishibukuryogan extract granules were obtained in the same manner as described in Example 6, except that Dexipearl, manufactured by Shiomiko Seito Co., Ltd.] was used. Example 9 Goreisan (3.94 parts of Chikushiya, 3.02 parts of Soujiyutsu,
Chiyorei 3.02 parts, Bukuriyo 3.02 parts, Keihi 1.50
10kg of the prescribed herbal medicine (consisting of 10 parts) was placed in the same extractor as described in Example 1, 100% of water was added, and the mixture was heated to 100°C.
After the extraction was completed, solid-liquid separation was performed during heating to obtain an extract. Further, in the same manner as in Example 1, a vapor condensate of about 15% was obtained during heating extraction, and concentrated to 5% using a tray distillation column. After concentrating the extract to about 1/4 at 40°C using a vacuum concentrator,
This was further spray-dried (blow air at 150°C, exhaust air at 90°C) to obtain a dry extract powder. On the other hand, mannitol [manufactured by Towa Chemical Industry Co., Ltd.]
After adding 2.5 and uniformly dispersing and mixing using a homogenizer, spray dry (ventilation 150℃, exhaust air 90℃)
Then, a dry mannitol powder containing volatile components was obtained. To 100g of the dry extract powder obtained as above, 50g of the volatile component-containing dry mannitol powder and 350g of mannitol powder were added, mixed well, and then compression molded into goreisan extract tablets (each weighing approximately 300mg). I got it. Example 10 Goreisan extract tablets (each weighing approx.
300mg) was obtained. Example 11 In the same manner as described in Example 9 except that dextrin [manufactured by Matsutani Chemical Industry Co., Ltd.] was used instead of mannitol, goreisan extract tablets (each weighing approximately 300 ml) were prepared in the same manner as described in Example 9.
mg) was obtained. Example 12 Goreisan extract tablets (each weighing approximately 300 mg) were prepared in the same manner as described in Example 9, except that crystalline cellulose [trade name: Avicel, manufactured by Asahi Kasei Industries, Ltd.] was used instead of mannitol. Obtained. Example 13 10 kg of the prescribed herbal medicine of Annachusan (consisting of 4.0 parts of Keihi, 3.0 parts of Quercus chinensis, 3.0 parts of Borei, 1.5 parts of Keihi, 1.0 part of Licorice, 1.0 part of Shiyukusha, and 0.5 parts of Riyokiyo) was described in Example 1. Put it in the same extractor, add 100% water, heat and extract at 100℃,
After the extraction was completed, solid-liquid separation was performed while hot to obtain an extract.
Further, in the same manner as in Example 1, about 15% of steam condensate was obtained during heating extraction. The extract was concentrated to about 1/4 at 40°C using a vacuum concentrator, and then spray-dried (blow air at 150°C, exhaust air at 90°C) to obtain a dry extract powder. On the other hand, the steam condensate obtained during the above heating extraction contained 7.5 kg of porous silicic anhydride [trade name:
Cyroid 266, manufactured by Fuji Co., Ltd.] was added and mixed uniformly using a homogenizer, and then spray-dried (blow air at 150°C, exhaust air at 90°C) to obtain a dry porous silicic acid anhydride powder containing volatile components. To 100 g of the dry extract powder obtained as above, 50 g of the volatile component-containing dry porous silicic anhydride powder and 350 g of porous silicic anhydride powder were added and mixed well to obtain Anchusan extract powder. Ta. Example 14 Soluble starch with 0.5% sucrose fatty acid ester added instead of porous silicic anhydride [sucrose fatty acid ester; trade name: Shugar ester, Ryoto Co., Ltd.
Anchu-san extract powder was obtained in the same manner as described in Example 13, except that soluble starch (trade name: Stabilose, manufactured by Matsutani Kagaku Kogyo Co., Ltd.) was used. Example 15 Hankakobokuto (keihi 6.0 parts, bukuriyou 5.0 parts,
Put 10kg of the prescribed herbal medicine (consisting of 3.0 parts of Kouboku, 2.0 parts of Soyou, and 10 parts of Shiyoukiyo) into the same extractor as described in Example 1, add 100% of water, and heat extraction at 100℃. Solid-liquid separation was then performed to obtain an extract. In addition, in the same manner as in Example 1, a steam condensate of about 15% by heat extraction was obtained. The extract was concentrated to about 1/4 at 40°C using a vacuum concentrator, and then spray-dried (blow air at 150°C, exhaust air at 90°C).
℃) and made into a dry extract powder. On the other hand, 7.5 kg of soluble starch [trade name: Stabilose, manufactured by Matsutani Chemical Industry Co., Ltd.] was added to the total amount of the steam condensate obtained during the above heating extraction, and after uniformly dispersing and mixing using a homogenizer, it was sprayed. It was dried (blow air at 150°C, exhaust air at 90°C) to obtain a dry soluble starch powder containing volatile components. To 100 g of the dry extract powder obtained as above, 50 g of the above dry soluble starch powder containing volatile components and 350 g of soluble starch powder were added, mixed well, and then compression molded to form granules of 12 to 32 meshes. Natsukobokuto extract granules were obtained. Example 16 Hankakobokuto extract granules were obtained in the same manner as described in Example 15, except that carboxymethyl cellulose calcium salt (trade name: ECG505, manufactured by Gotoku Pharmaceutical Co., Ltd.) was used instead of soluble starch. Example 17 Hankakobokuto extract granules were obtained in the same manner as described in Example 15, except that gum arabic powder (manufactured by Sankyo Foods Co., Ltd.) was used instead of soluble starch.

[Brief explanation of the drawing]

The drawings show the high performance liquid chromatography analysis patterns before and after the accelerated test in Experimental Example 1, and Figure 1 shows the analysis pattern of Sample 1A.
Figure 2 shows the analysis pattern of sample 1B, Figure 3
The figure shows the analysis pattern of sample 2A, and FIG. 4 shows the analysis pattern of sample 2B.

Claims (1)

[Claims] 1. Extract the herbal medicine with an extraction solvent, concentrate the extract, and dry it to obtain the herbal medicine extract powder, and condense the extraction solvent vapor containing volatile components generated during extraction and/or concentration, and extract this condensate. 1 selected from sugars, starches, dextrins, silicic acid compounds, celluloses, gum tragacanth, and gum arabic, either as is or in concentrated form.
A method for producing a Chinese herbal medicine extract, which comprises mixing the powder obtained by mixing with one or more excipients and drying the powder and the above Chinese medicine extract powder.