Method for preparing granules or pills containing extracts in high concentration

Abstract

The present invention relates to a method for preparing a granule or a pill containing a plant, medicinal herb or traditional oriental medicine decoction extract, having the steps of: (a) injecting a powdered plant, medicinal herb or traditional oriental medicine decoction extract into a fluidized-bed device and spraying purified water or a solution of the same type of extract as the extract powder at the extract powder while fluidizing the same, thereby generating microgranules of the extract powder; and (b) injecting the microgranules generated at step (a) as seeds into the fluidized-bed device and spraying a solution of the extract while fluidizing the same, thereby growing the microgranules to a predetermined size of granule or pill. According to the present invention, it is possible to prepare a granule or a pill containing an extract in a high concentration.

Claims

1. Granules or pills containing an extract of a plant, herbal medicine, or medicinal herb decoction, which are prepared by a method comprising: (a) feeding an extract powder of a plant, medicinal herb, or medicinal herb decoction into a fluidized-bed device to fluidize the extract powder, and spraying purified water onto the fluidized extract powder, thereby generating micro granules of the extract powder, the microgranules having a diameter of 1-150 μm; and (b) feeding the microgranules generated in step (a) as seeds into a fluidized-bed device to fluidize the microgranules, and spraying a solution of the same kind of extract as the extract powder onto the microgranules, thereby growing the microgranules into granules having a diameter of 1-3 mm or pills having a diameter of 4-10 mm, wherein the extract is contained in up to 100 wt% with respect to the granule or pill.

2. The granules or pills of claim 1 wherein the method further comprising, before step (a), preparing the extract powder of a plant, medicinal herb, or medicinal herb decoction in a spray dryer.

3. The granules or pills of claim 1, wherein in step (a), the purified water is sprayed from the top of the fluidized-bed device in a top-spray manner.

4. The granules or pills of claim 3, wherein in step (b), the solution of the extract is sprayed from the bottom of the fluidized-bed device in a bottom-spray manner.

5. The granules or pills of claim 1, wherein the method further comprising: (c-1), after step (b), feeding the granules generated in step (b) as seeds into a rotor of a fluidized-bed device to fluidize the granules, and spraying the solution of the extract onto the fluidized granules while the microgranules generated in step (a) are transferred into the rotor, thereby obtaining granules or pills growing to a predetermined size.

6. The granules or pills of claim 1, wherein the method further comprising: (c-2), after step (b), surface-coating the granules or pills generated in step (b) with a moisture-proofing material.

7. The granules or pills of claim 6, wherein the moisture-proofing material is selected from the group consisting of hydroxypropyl methylcellulose, hydroxypropyl cellulose, ethyl cellulose, methyl cellulose, titanium dioxide, polyethylene glycol, triethyl citrate, triacetin, dibutyl sebacate, polymethacrylate, cellulose acetate phthalate, carnauba wax, candelila wax, petroleum wax, beeswax, and palm oil.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

(1) FIG. 1 schematically illustrates a whole flow chart showing a preparing method of the present invention.

(2) FIG. 2 shows actual images of granules and pills prepared by processes in example 3. (a) Sipjeondaebotang granules; (b) Red ginseng concentrate pills; and (c) Acanthopanax senticosus granules

(3) FIG. 3 shows an actual image of Sipjeondaebotang pills prepared by a process in example 4. Dark regions indicate granules with a diameter of 3 mm in the image.

(4) FIG. 4 shows images of final products produced according to the preparing method of the present invention. {circle around (1)} Acanthopanax senticosus; {circle around (2)} Astragalus membranaceus; {circle around (3)} Banhasihamtang; {circle around (4)} Sipjeondaebotang; {circle around (5)} Cheongseoikgitang (rectangular preparation: coated with green color); {circle around (6)} Rehmannia glutinosa (Circular and rectangular preparations); {circle around (7)} Angelica gigas+Allium victorialis (rectangular preparation); {circle around (8)} Hovenia dulcis; and {circle around (9)} red ginseng.

MODE FOR CARRYING OUT THE INVENTION

(5) The present invention will now be described in further detail by examples. It would be obvious to those skilled in the art that these examples are intended to be more concretely illustrative and the scope of the present invention as set forth in the appended claims is not limited to or by the examples.

EXAMPLES

Example 1

Preparation of Extract Powder Through Spray Drying

(6) In the present example, Acanthopanax senticosus, Astragali Radix, Angelicae gigantis Radix and Allii Bulbus, Hovenia dulcis, and six-year old red ginseng were used as sources for herbal medicine extract samples. For medicinal herb decoctions, decoctions composed of less than 10 species, 10 species, and more than 10 species of raw materials were selected, and corresponding standard decoctions were Banhasihamtang (Pinelliae Rhizoma, Scutellariae Radix, Zingiberis Rhizoma, Adenophorae Radix, Glycyrrhizae Radix, Jujubae Fructus, and Coptidis Rhizoma; seven species), Sipjeondaebotang (Jujubae Fructus, Cinnamomi Ramulus, Angelicae gigantis Radix, Adenophorae Radix, Paeoniae Radix Alba, Astragali Radix, Cnidii Rhizoma, Rehmanniae Radix Preparat, Atractylodis Rhizoma, and Atractylodis macrocephalae Rhizoma; 10 species); and Cheongseoikgitang (Puerariae Radix, Jujubae Fructus, Angelicae gigantis Radix, Liriopis Tuber, Adenophorae Radix, Atractylodis macrocephalae Rhizoma, Cimicifugae Rhizoma, Massa Medicata Fermentata, Phellodendri Cortex, Astragali Radix, Alismatis Rhizoma, Citri reticulatae viride Pericarpium, Atractylodis Rhizoma, Fraxini Cortex, and Schizandrae Fructus: 15 species).

(7) {circle around (1)} Preparation of Acanthopanax senticosus Powder

(8) 5 kg of Acanthopanax senticosus and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 150° C., an outlet temperature of 85° C., and an extract spray rate of 500 ml/h. Approximately 900 g of dried powder was prepared per batch of the extract.

(9) {circle around (2)} Preparation of Astragali Radix Powder

(10) 5 kg of Astragali Radix and 50 kg of purified water were fed into an herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 160° C., an outlet temperature of 95° C., and an extract spray rate of 1000 ml/h. Approximately 500 g of dried powder was prepared per batch of the extract.

(11) {circle around (3)} Preparation of Banhasihamtang Powder

(12) 5 kg of Banhasihamtang prescription raw materials, which were prepared by an oriental medicine clinic, and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 145° C., an outlet temperature of 80° C., and an extract spray rate of 800 ml/h. Approximately 1,050 g of dried powder was prepared per batch of the extract.

(13) {circle around (4)} Preparation of Sipjeondaebotang Powder

(14) 5 kg of Sipjeondaebotang prescription raw materials, which were prepared by an oriental medicine clinic, and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 145° C., an outlet temperature of 80° C., and an extract spray rate of 800 ml/h. Approximately 1,250 g of dried powder was prepared per batch of the extract.

(15) {circle around (5)} Preparation of Cheongseoikgitang Powder

(16) 5 kg of Cheongseoikgitang prescription raw materials, which were prepared by an oriental medicine clinic, and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 145° C., an outlet temperature of 80° C., and an extract spray rate of 800 ml/h. Approximately 950 g of dried powder was prepared per batch of the extract.

(17) {circle around (6)} Preparation of Rehmanniae Radix Preparat Powder

(18) 5 kg of Rehmanniae Radix Preparat which was purchased from a herbal medicine shop and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 145° C., an outlet temperature of 80° C., and an extract spray rate of 700 ml/h. Approximately 2,250 g of dried powder was prepared per batch of the extract.

(19) {circle around (7)} Preparation of Angelicae gigantis Radix and Allii Bulbus Powder

(20) 5 kg of Angelicae gigantis Radix and Allii Bulbus, which are mixed at a ratio of 20:80 based on a weight ratio obtained by converting the moisture content of a raw material into 10%, and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 145° C., an outlet temperature of 80° C., and an extract spray rate of 800 ml/h. Approximately 2,050 g of dried powder was prepared per batch of the extract.

(21) {circle around (8)} Preparation of Hovenia dulcis Powder

(22) 5 kg of Hovenia dulcis and dried fruits thereof and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 145° C., an outlet temperature of 80° C., and an extract spray rate of 800 ml/h. Approximately 1,350 g of dried powder was prepared per batch of the extract.

(23) {circle around (9)} Preparation of Red Ginseng Powder

(24) 5 kg of 6-year old red ginseng and 50 kg of purified water were fed into a herbal extractor, allowed to steep for 2 hours at room temperature, and then extracted for 3 hours at 95° C., followed by filtration. The extract was spray-dried using a spray dryer (SD-1000, Eyela) having an inlet temperature of 145° C., an outlet temperature of 80° C., and an extract spray rate of 800 ml/h. Approximately 2,600 g of dried powder was prepared per batch of the extract.

Example 2

Preparation of Microgranules in Top-Spray Manner by Fluidized-Bed Device

(25) Microgranules were prepared from each of the dried powders prepared in example 1 using a top-spray system of a fluidized-bed device (FBGC-3, Chungjin Tech Korea) provided with the top-spray system, a bottom-spray system, and a tangential rotor system. When the microgranules were prepared in a top spray manner, an extract corresponding to each of the dried powders or purified water was used as a binder. When the extract was used, the fluidizing room temperature was set to 65-70° C., the extract feeding rate to 150-200 ml/h, and the spray pressure to 1 kg/cm.sup.2, and the spray pressure was increased to a range of 1.5-3.5 kg/cm.sup.2 while observing the fluidized state. When the purified water was used, the fluidizing room temperature was set to 70-75° C., the extract feeding rate to 180-250 ml/h, and the spray pressure to 1 kg/cm.sup.2, and the spray pressure was increased to a range of 1.5-3.5 kg/cm.sup.2 while observing the fluidized state. In addition, when the extract was used, 600-1000 g of the corresponding dried powder was fed as a base seed, and when the purified water was used, 1200-1500 g of the corresponding dried powder was fed. For a binder, 1500 g of the corresponding extract was sprayed, and 2000 g of purified water was sprayed in the Banhasihamtang, Angelicae gigantis Radix and Allii Bulbus, and Hovenia dulcis. The results of preparing microgranules by the methods were tabulated in table 1. Samples coated with shellac or ethyl cellulose, shown in table 1, were prepared for tableting in example 5 below, and the sizes of granules and pills were measured after additional processes in the examples below.

(26) TABLE-US-00001 TABLE 1 Results of preparing microgranules in top-spray manner and final products thereof Top-spray process Average Comparison Base Microgranule particle (final Sample Seed production size product No. Sample Name (g) Binder (g) (g) (μm) content %) {circle around (1)} Acanthopanax 600 Corresponding 900 100 Up to 4 mm- senticosus extract 1500 sized granules (100%) {circle around (2)} Astragali Radix 1000 Corresponding 1150 100 Up to 2.3 mm- extract 1500 sized granules (100%) {circle around (3)} Banhasihamtang 1500 Purified 1470 80 Up to 2.3 mm- water 2000 sized granules (100%) {circle around (4)} Sipjeondaebotang 1000 Corresponding 1370 100 Up to 8 mm- extract 1500 sized pills (98.52%) {circle around (5)} Cheongseoikgitang 800 Corresponding 1080 100 Coated extract 1500 with 1% shellac and then tableted (86.36%) {circle around (6)} Rehmanniae Radix 1000 Corresponding 1650 100 Coated Preparat extract 1500 with 1% ethyle cellulose and then tableted (98%) {circle around (7)} Angelicae 1500 Purified 1480 80 Coated gigantis Radix water 2000 with 2% and Allii Bulbus ethyle cellulose and then tableted (85%) {circle around (8)} Hovenia dulcis 1200 Purified 1170 80 2 mm-sized water 2000 granules containing capsule (100%) {circle around (9)} Six-year old red 1000 Corresponding 1750 100 2 mm-sized ginseng extract 1500 granules and 8 mm- sized pills (100%)

Example 3

Preparation of Granules and Pills in Bottom-Spray Manner by Fluidized-Bed Device

(27) The microgranules prepared in example 2 above were fed as base seeds for fluidized-bed formation into the bottom-spray system of the fluidized-bed device (FBGC-3, Chungjin Tech Korea), thereby preparing circular granules and pills. More specifically, 1000 g of microgranules of each of Astragali Radix, Banhasihamtang, and Hovenia dulcis prepared in example 2 above were fed as base seeds for fluidized-bed formation. The fluidizing room temperature was set to 65-70° C., and the extract feeding rate was increased from 120 ml/h to 200 ml/h. The spray pressure was gradually increased from 1 kg/cm.sup.2 at an initial state to a range of 1.5-2.0 kg/cm.sup.2 while observing the fluidized state. Also, 750 g of microgranules of each of Acanthopanax senticosus, Sipjeondaebotang, and red ginseng were fed as base seeds for fluidized-bed formation, to grow the particle size to 3-4 mm. For Sipjeondaebotang and red ginseng, this procedure was repeated one more time, and the spray pressure was increased to 5 kg/cm.sup.2 at the maximum limit. In the present process, in order to increase the growing rate of the particle size, the initial solid content (concentration of 5-20%) of the corresponding extract was concentrated to 30-40%. Through this process, Astragali Radix, Banhasihamtang, and Hovenia dulcis pills were prepared to have a diameter of 2.3 mm, Acanthopanax senticosus and Sipjeondaebotang pills were prepared to have a diameter of 3-4 mm, and Sipjeondaebotang and red ginseng pills were prepared to have a diameter of 8 mm (FIG. 2).

Example 4

Preparation of Granules and Pills Using Rotor System of Fluidized-Bed Device

(28) In the preparation of pills using a tangential rotor system of a fluidized-bed device (FBGC-3, Chungjin Tech Korea), Sipjeondaebotang granules with a diameter of about 3 mm prepared in example 3 were used. With respect to the powder constantly fed into the inside of the rotor from the outside, the microgranules prepared in example 2, which was coated with a 1.5% solution in which ethyl cellulose corresponding to 2% based on 1500 g of the microgranules was dissolved in ethyl alcohol, were fed into the rotor at a constant rate using a feeder. That is, 500 g of the granules with a size (diameter) of 3 mm, which was previously prepared in example 3, were fed as seeds into a fluidized-bed rotor system provided with a rotating circular disk, and then the microgranule powder coated with ethyl cellulose was fed into a granulator at a rate of 10 g/min while the rotor system is rotated at 250 rpm. While the internal temperature of the rotor is maintained at 25° C., a Sipjeondaebotang extract prepared in example 1 was sprayed as a binder at a rate of 10 ml/min, thereby growing the microgranules into pills with a size of 8 mm. FIG. 3 shows an image of Sipjeondaebotang pills that have been prepared, and it can be confirmed from FIG. 3 that the microgranule powder is coated in layers on the surface of the Sipjeondaebotang granule with a size of 3 mm (FIG. 3).

Example 5

Preparation of Circular and Rectangular Tablets Using Tableting Machine

(29) In the last step of the micro-granulating procedure in example 2, the dried powder of each of Cheongseoikgitang, Rehmanniae Radix Preparat, and Angelicae gigantis Radix and Allii Bulbus was surface-coated with a shellac or ethyl cellulose solution, thereby allowing the powder to have improved fluidity in a tableting procedure. Then, raw materials shown in table 2 below were mixed to prepare rectangular and circular tablets. Models KISAN KP-410 and KISAN KF-S50 were used for a tableting machine and a capsule filling machine, respectively. As shown in FIG. 4, it was confirmed that the fluidity was favorable without tangle (cementation) of powder raw materials mixed before tableting, and there were no problems in the moldability for being manufactured into products, binding force, and stability after being manufactured into products.

(30) TABLE-US-00002 TABLE 2 Mixing ratio of raw materials for tableting (%) Angelicae Rehmanniae gigantis Radix + Raw material Cheongseoikgitang Radix Allii Bulbus Microgranule 95 98 85 powder Avi-cell 2.5 1.0 5.0 Saccharose- 0.5 0.5 2.0 fatty acid ester stearic acid — — 5.0 magnesium HPMC 2.0 0.5 3.0 total, % 100 100 100 Note Coated with — — gardenia green.sup.a Final content 86.36% 98% 85% (%) .sup.aThe tablet was externally coated with a 5% solution in which, based on 100 g of a tablet, 5.5% TiO.sub.2, 2.5% hydroxypropyl methylcellulose (HPMC), and 2.0% gardenia green are dissolved in 70% ethyl alcohol was prepared, using a sugar coated tablet coater.

(31) Having described a preferred embodiment of the present invention, it is to be understood that variants and modifications thereof falling within the spirit of the invention may become apparent to those skilled in this art, and the scope of this invention is to be determined by appended claims and their equivalents.