Summary of the invention
Goal of the invention is in order to overcome above the deficiencies in the prior art, the invention provides a kind of preparation method of JINDAN PIAN, when medicinal material extract, Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati are used water extraction after with 60% ethanol extraction again, extract with the full composition that reaches these three kinds of medical materials, take full advantage of the effective ingredient in the medical material, improve curative effect.
To achieve these goals, the present invention is by the following technical solutions:
A kind of preparation technology of Chinese medicine JINDAN PIAN may further comprise the steps:
(1) medicinal material extract: Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati are used respectively ethanol extraction three times, Fel Sus domestica unguentum with ethanol extraction once, the alcoholic solution that merges backflow and Fel Sus domestica unguentum, medical material residue after the extraction decocts with water twice again, filter, concentrated, alcohol extract and water extraction concentrated solution are merged, be condensed into extractum;
(2) drying: extractum is formed fine powder by spray drying;
(3) granulate: fine powder is made by granulator can be for the granule of tabletting;
(4) tabletting: granule is added direct compression behind the lubricant, obtain plain sheet;
(5) coating: the JINDAN PIAN element sheet that presses is placed in the high-efficiency coating pot, film coating, the coating gain in weight is 2%-5%, and get final product.
The weight of the used ethanol of medicinal material extract in the step (1) is respectively 5-10 times of corresponding medical material Herba Lysimachiae weight, and the 3-7 of Radix Gentianae weight times, the 3-7 of Rhizoma Polygoni Cuspidati weight times, the 2-3 of Fel Sus domestica unguentum weight doubly.
Used ethanol is the ethanol of content 60%, and extracting mode is reflux, extract,, and wherein for the first time extraction time is 2-3 hour, and second, third time extraction time is 1-2 hour, has extracted rear merging backflow and Fel Sus domestica unguentum alcohol extract, obtains alcohol extract; In the above-mentioned steps, alcohol extract is Recycled ethanol further also.
The preparation technology of described Chinese medicine JINDAN PIAN, the medical material residue decocts with water 5-8 that twice used water yield be respectively the medical material amount doubly and 4-6 times.
The preparation technology of described Chinese medicine JINDAN PIAN after wherein decocting boils filters medicinal liquid, and being concentrated into Baume degrees is 5-8 ° of Be, and temperature is 60-80 ℃.
The preparation technology of described Chinese medicine JINDAN PIAN, it is 12-18 ° of Be that alcohol extract and water extraction concentrated solution are incorporated into Baume degrees, temperature is 60-80 ℃.
The preparation technology of described Chinese medicine JINDAN PIAN, spray dryer inlet temperature are 180~220 ℃, and outlet temperature is 90~110 ℃.
The preparation technology of described Chinese medicine JINDAN PIAN, granulator inlet temperature are 60~110 ℃, and the transfusion frequency values is 35~50HZ.
Beneficial effect
In extraction step, Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati are used water extraction after with ethanol extraction again, the full composition that reaches these three kinds of medical material effective ingredient extracts, so that the effective ingredient in the medical material is fully used, the JINDAN PIAN of using the present invention to make is compared with the JINDAN PIAN that traditional method makes, the total content of Quercetin and kaempferide has improved more than 60%, Determination of Polydatin has improved 42.8%, and the content of Radix Gentianae hardship also is significantly improved.
The specific embodiment:
Embodiment 1
The preparation method of JINDAN PIAN may further comprise the steps:
(1) medicinal material extract: by weight, with 60 parts of Herba Lysimachiaes, 10 parts of Radix Gentianaes, 20 parts of usefulness of Rhizoma Polygoni Cuspidati, 60% alcohol reflux three times (add amount of alcohol and be about respectively 5 times, 3 times, 3 times of medical material amount), 3 hours for the first time, second and third time each 2 hours, alcoholic solution (1 part of the Fel Sus domestica unguentum that merges backflow and Fel Sus domestica unguentum, add 2 times of extractions of ethanol), Recycled ethanol obtains alcohol extract.Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati residue are decocted with water secondary (amount of water is about respectively 5 times of medical material amounts, 4 times of amounts), each 2 hours, medicinal liquid filters, be concentrated into Baume degrees and be about 5 ° of Be, temperature 60 C, precipitation is more than 24 hours, and the mixed liquor of leaching supernatant and alcohol extract merging is concentrated into Baume degrees and is about 12 ° Be(60 ℃) extractum.
(2) drying: clear paste is spray dried to fine powder.The spray dryer inlet temperature is 180 ℃, and outlet temperature is 90 ℃.
(3) granulate: but the magnesium stearate of fine powder and 1% is directly made the granule of tabletting with one-step-granulating method.The one-step-granulating method inlet temperature is 90 ℃, and the transfusion frequency values is 35HZ.
(4) tabletting: with the granule tabletting, punch die φ 10mm scrobicula checks that every 15 minutes average sheet is heavy once, checks hardness, outward appearance etc. simultaneously in the tabletting process.
(5) coating: get qualified JINDAN PIAN element sheet, set high in the effect coating pan, start seed-coating machine, exhaust blower and hot-air blower, elder generation's blowing hot-air pre-phlogiston sheet to 40 ℃, then start spraying system, film-coat liquid is sprayed onto the tablet surface equably, the coating temperature is 50~60 ℃, until sprayed till whole thin film dress materials, the coating weightening finish is 2%.
Embodiment 2
The preparation method of JINDAN PIAN may further comprise the steps:
(1) medicinal material extract: with 60 parts of Herba Lysimachiaes, 10 parts of Radix Gentianaes, 20 parts of usefulness of Rhizoma Polygoni Cuspidati, 60% alcohol reflux three times (add amount of alcohol and be about respectively 6 times, 4 times, 4 times of medical material amount), 3 hours for the first time, second and third time each 1 hour, alcoholic solution (1 part of the Fel Sus domestica unguentum that merges backflow and Fel Sus domestica unguentum, add 3 times of extractions of ethanol), Recycled ethanol.Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati residue are decocted with water secondary (amount of water is about respectively 6 times of medical material amounts, 5 times of amounts), each 2 hours, medicinal liquid filters, be concentrated into Baume degrees and be about 6 ° Be(60 ℃), precipitation is more than 24 hours, the mixed liquor of leaching supernatant and alcohol extract merges, and is concentrated into Baume degrees and is about 14 ° Be(60 ℃) clear paste.
(2) drying: clear paste is spray dried to fine powder.The spray dryer inlet temperature is 190 ℃, and outlet temperature is 100 ℃.
(3) granulate: but the magnesium stearate of fine powder and 1% is directly made the granule of tabletting with one-step-granulating method.The one-step-granulating method inlet temperature is 100 ℃, and the transfusion frequency values is 40HZ.
(4) tabletting: with the granule tabletting, punch die φ 10mm scrobicula checks that every 15 minutes average sheet is heavy once, checks hardness, outward appearance etc. simultaneously in the tabletting process.
(5) coating: get qualified JINDAN PIAN element sheet, set high in the effect coating pan, start seed-coating machine, exhaust blower and hot-air blower, elder generation's blowing hot-air pre-phlogiston sheet to 40 ℃, then start spraying system, film-coat liquid is sprayed onto the tablet surface equably, the coating temperature is 50~60 ℃, until sprayed till whole thin film dress materials, the coating weightening finish is 3%.
Embodiment 3
The preparation method of JINDAN PIAN may further comprise the steps:
(1) medicinal material extract: with 50 parts of Herba Lysimachiaes, 8 parts of Radix Gentianaes, 15 parts of usefulness of Rhizoma Polygoni Cuspidati, 60% alcohol reflux three times (add amount of alcohol and be about respectively 7 times, 5 times, 5 times of medical material amount), 2 hours for the first time, second and third time each 1 hour, alcoholic solution (1 part of the Fel Sus domestica unguentum that merges backflow and Fel Sus domestica unguentum, add 2 times of extractions of ethanol), Recycled ethanol.Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati residue are decocted with water secondary (amount of water is about respectively 6 times of medical material amounts, 5 times of amounts), each 2 hours, medicinal liquid filters, be concentrated into Baume degrees and be about 6 ° Be(80 ℃), precipitation is more than 24 hours, the mixed liquor of leaching supernatant and alcohol extract merges, and is concentrated into Baume degrees and is about 15 ° Be(80 ℃) clear paste.
(2) drying: clear paste is spray dried to fine powder.The spray dryer inlet temperature is 210 ℃, and outlet temperature is 95 ℃.
(3) granulate: but the magnesium stearate of fine powder and 1% is directly made the granule of tabletting with one-step-granulating method.The one-step-granulating method inlet temperature is 85 ℃, and the transfusion frequency values is 50HZ.
(4) tabletting: with the granule tabletting, punch die φ 10mm scrobicula checks that every 15 minutes average sheet is heavy once, checks hardness, outward appearance etc. simultaneously in the tabletting process.
(5) coating: get qualified JINDAN PIAN element sheet, set high in the effect coating pan, start seed-coating machine, exhaust blower and hot-air blower, elder generation's blowing hot-air pre-phlogiston sheet to 40 ℃, then start spraying system, film-coat liquid is sprayed onto the tablet surface equably, the coating temperature is 50~60 ℃, until sprayed till whole thin film dress materials, the coating weightening finish is 3%.
Embodiment 4
The preparation method of JINDAN PIAN may further comprise the steps:
(1) medicinal material extract: with 70 parts of Herba Lysimachiaes, 10 parts of Radix Gentianaes, 25 parts of usefulness of Rhizoma Polygoni Cuspidati, 60% alcohol reflux three times (add amount of alcohol and be about respectively 7 times, 5 times, 5 times of medical material amount), 2 hours for the first time, second and third time each 1 hour, alcoholic solution (1 part of the Fel Sus domestica unguentum that merges backflow and Fel Sus domestica unguentum, add 3 times of extractions of ethanol), Recycled ethanol.Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati residue are decocted with water secondary (amount of water is about respectively 6 times of medical material amounts, 5 times of amounts), each 2 hours, medicinal liquid filters, be concentrated into Baume degrees and be about 7 ° Be(80 ℃), precipitation is more than 24 hours, the mixed liquor of leaching supernatant and alcohol extract merges, and is concentrated into Baume degrees and is about 17 ° Be(80 ℃) clear paste.
(2) drying: clear paste is spray dried to fine powder.The spray dryer inlet temperature is 200 ℃, and outlet temperature is 95 ℃.
(3) granulate: but the magnesium stearate of fine powder and 1% is directly made the granule of tabletting with one-step-granulating method.The one-step-granulating method inlet temperature is 75 ℃, and the transfusion frequency values is 40HZ.
(4) tabletting: with the granule tabletting, punch die φ 10mm scrobicula checks that every 15 minutes average sheet is heavy once, checks hardness, outward appearance etc. simultaneously in the tabletting process.
(5) coating: get qualified JINDAN PIAN element sheet, set high in the effect coating pan, start seed-coating machine, exhaust blower and hot-air blower, elder generation's blowing hot-air pre-phlogiston sheet to 40 ℃, then start spraying system, film-coat liquid is sprayed onto the tablet surface equably, the coating temperature is 50~60 ℃, until sprayed till whole thin film dress materials, the coating weightening finish is 4%.
Embodiment 5
The preparation method of JINDAN PIAN may further comprise the steps:
(1) medicinal material extract: with 60 parts of Herba Lysimachiaes, 10 parts of Radix Gentianaes, 20 parts of usefulness of Rhizoma Polygoni Cuspidati, 60% alcohol reflux three times (add amount of alcohol and be about respectively 10 times, 7 times, 7 times of medical material amount), 2 hours for the first time, second and third time each 1 hour, alcoholic solution (1 part of the Fel Sus domestica unguentum that merges backflow and Fel Sus domestica unguentum, add 3 times of extractions of ethanol), Recycled ethanol.Herba Lysimachiae, Radix Gentianae, Rhizoma Polygoni Cuspidati residue are decocted with water secondary (amount of water is about respectively 8 times of medical material amounts, 6 times of amounts), each 2 hours, medicinal liquid filters, be concentrated into Baume degrees and be about 8 ° Be(70 ℃), precipitation is more than 24 hours, the mixed liquor of leaching supernatant and alcohol extract merges, and is concentrated into Baume degrees and is about 18 ° Be(70 ℃) clear paste.
(2) drying: clear paste is spray dried to fine powder.The spray dryer inlet temperature is 220 ℃, and outlet temperature is 90 ℃.
(3) granulate: but the magnesium stearate of fine powder and 1% is directly made the granule of tabletting with one-step-granulating method.The one-step-granulating method inlet temperature is 110 ℃, and the transfusion frequency values is 50HZ.
(4) tabletting: with the granule tabletting, punch die φ 10mm scrobicula checks that every 15 minutes average sheet is heavy once, checks hardness, outward appearance etc. simultaneously in the tabletting process.
(5) coating: get qualified JINDAN PIAN element sheet, set high in the effect coating pan, start seed-coating machine, exhaust blower and hot-air blower, elder generation's blowing hot-air pre-phlogiston sheet to 40 ℃, then start spraying system, film-coat liquid is sprayed onto the tablet surface equably, the coating temperature is 50~60 ℃, until sprayed till whole thin film dress materials, the coating weightening finish is 5%.
Get extracting method of the present invention and make the JINDAN PIAN effective substance content that JINDAN PIAN and existing traditional method make and compare test, concrete data see Table 1.Detection method is referring to research " Shandong medicine thing " the 29th volume the 3rd phase author Chen Xiaofeng, Yang Yanfei in 2010 of JINDAN capsule quality standard.
Table 1 JINDAN PIAN of the present invention and traditional method make the contrast of JINDAN PIAN active constituent content
Can be found out by above test data, the JINDAN PIAN of using the present invention to make is compared with the JINDAN PIAN that traditional method makes, the total content of Quercetin and kaempferide has improved more than 60%, Determination of Polydatin has improved 42.8%, and the content of Radix Gentianae hardship also is significantly improved, therefore the present invention's technique of preparing JINDAN PIAN can effectively utilize raw material, improves curative effect, has reduced accordingly cost.