CN106031763A

CN106031763A - Improved preparation method of notoginseng root capsules for dysmenorrhoea

Info

Publication number: CN106031763A
Application number: CN201510123311.1A
Authority: CN
Inventors: 黄辉球
Original assignee: HUIZHOU JIUHUI PHARMACEUTICAL CO Ltd
Current assignee: HUIZHOU JIUHUI PHARMACEUTICAL CO Ltd
Priority date: 2015-03-20
Filing date: 2015-03-20
Publication date: 2016-10-19

Abstract

The invention relates to the field of a preparation method and technology of Chinese patent medicines. The invention provides an improved preparation method of notoginseng root capsules for dysmenorrhoea. The preparation method comprises the following steps: (1) individual ultra-fine pulverization is carried out for notoginseng roots, flying squirrel feces, typha pollen, corydalis tubers, Szechuan lovage rhizomes, common aucklandia roots, fennel, and borneol, in order to obtain fine powder, and the powder is uniformly mixed for standby; (2) medicinal powder obtained in the step (1) and a filler are uniformly mixed according to a weight ratio 0.5-1.5:0.5, a wetting agent is added, and granulation is carried out by extrusion with a wet method; (3) particles obtained in the step (2) are dried in a baking oven at 60 DEG C for 60 minutes, dried particles are obtained, particles are arranged and contained in capsules, and the capsules are obtained. The filler comprises starch, dextrin and lactose according to a weight proportion 7:1:1. The wetting agent comprises an ethanol alcohol whose weight percentage is 70% and a povidone solution whose weight percentage is 3%. The preparation method improves fluidity of products, solves the sticking problem, shortens disintegration time limit, and improves bioavailability.

Description

A kind of preparation method of the TIANQI TONGJING JIAONANG of improvement

Technical field

The present invention relates to Chinese patent medicine preparation method technical field.

Background technology

TIANQI TONGJING JIAONANG is recorded in Drug Standard of Ministry of Public Health of the Peoples Republic of China Traditional Chinese medicine historical preparation the 10th.Finding through inspection information, this prescription is to be developed by ancient prescription " SHIXIAO SAN ".Prescription is made up of Radix Notoginseng, Oletum Trogopterori, Pollen Typhae, Rhizoma Corydalis, Rhizoma Chuanxiong, the Radix Aucklandiae, Fructus Foeniculi, Borneolum Syntheticum.Radix Notoginseng merit arrogates to oneself removing stasis to stop bleeding, analgesic therapy of invigorating blood circulation, and can stop blooding, again can dissipating blood stasis, have hemostasis and do not hinder positive feature, for monarch drug.Rhizoma Chuanxiong, Rhizoma Corydalis blood-activating and qi-promoting pain relieving；Oletum Trogopterori, Pollen Typhae removing stasis to stop bleeding, promoting blood circulation and stopping pain.Radix Aucklandiae promoting the circulation of QI to relieve pain, are ministerial drug altogether.The pungent temperature of Fructus Foeniculi, warming liver and expelling cold, antalgic, for adjuvant drug.Borneolum Syntheticum clearing away heat to alleviate pain, fragrance is walked to alter, for making medicine.All medicines share, and play promoting blood circulation and hemostasis, the merit of circulation of qi promoting dispersing cold for relieving pain altogether.

TIANQI TONGJING JIAONANG is to be the hard capsule that raw material is prepared from by Radix Notoginseng, Oletum Trogopterori, Pollen Typhae, Rhizoma Corydalis, Rhizoma Chuanxiong, the Radix Aucklandiae, Fructus Foeniculi, Borneolum Syntheticum, has logical QI and blood regulating, effect of pain relieving regulating menstruation.Cure mainly abdominal pain in menstruation and because of cold caused menoxenia.But sticking phenomenon the most easily occurs in this product, mobility is poor, thus affects capsule content uniformity；After storing a period of time, disintegration can extend, and bioavailability reduces.

Summary of the invention

The technical problem to be solved is to provide the preparation method of the new TIANQI TONGJING JIAONANG of a kind of improvement, and this method can improve the mobility of this product, solves sticking problem, shortens disintegration, improves bioavailability.

The technical problem to be solved is achieved by the following technical programs:

A kind of preparation method of the TIANQI TONGJING JIAONANG of improvement, preparation process is:

(1) the independent micronizing of Radix Notoginseng, Oletum Trogopterori, Pollen Typhae, Rhizoma Corydalis, Rhizoma Chuanxiong, the Radix Aucklandiae, Fructus Foeniculi, Borneolum Syntheticum powder are broken into fine powder, mix standby；

(2) after step (1) gained medicated powder and filler weight proportion are 0.5 ~ 1.5:0.5 mixing, adding wetting agent, wet-method extrusion is pelletized；

(3) step (2) gained granule oven drying about 60min at 60 DEG C, obtains dry granule, and granulate is encapsulated, to obtain final product.

Further, described filler be part by weight be the starch of 7:1:1, dextrin and lactose.

Further, described wetting agent be weight percentage 70% ethanol solution and percentage by weight be 3% povidone solution.

There is advantages that

The present invention is in the research of preparation technology, for improving the drug dissolution of monarch drug, first by independent for Radix Notoginseng micronizing, has more been ground into the seven flavor medicine material mixing of fine powder with other；Use the mixed accessories that comprehensive scoring method screening is suitable；And carry out preferably, determining optimal molding technique parameter to medicine and adjuvant optimum proportioning, wetting agent, particle drying technique, provide theoretical foundation for specification industrialized production.

Detailed description of the invention

Below in conjunction with embodiment, the present invention will be described in detail, and embodiment is only the preferred embodiment of the present invention, is not limitation of the invention.

Embodiment 1

(2) after step (1) gained medicated powder and filler weight proportion are 1:0.5 mixing, adding wetting agent, wet-method extrusion is pelletized；Described filler be part by weight be the starch of 7:1:1, dextrin and lactose.Described wetting agent be weight percentage 70% ethanol solution and percentage by weight be 3% povidone solution.

The present invention, under the guidance of Chinese medical theory, applies modern pharmaceutical technology, improves the preparation technology of preparation, to improving the mobility of this product, solves sticking problem, shortens disintegration, improves bioavailability.Inventor this carried out substantial amounts of experiment.In experiment, instrument is electric drying oven with forced convection (DHG-9240A, upper Nereid grand experimental facilities company limited), electronic balance (JD1000-2, Longteng Electronic Weighing Instrument Co., Ltd., Shenyang), electronic analytical balance (AUW200, Shimadzu company limited of Japan), in reagent used, lactose, mannitol, soluble starch, dextrin, microcrystalline Cellulose are medicinal rank；Other reagent are analytical pure.

(1) screening of adjuvant

1 The prescreening of single adjuvant

The protogenic medicinal powder of TIANQI TONGJING JIAONANG is amorphous powder, there is hygroscopicity, poor fluidity, is difficult to make granule, in order to make granule have relatively small hygroscopicity and relatively good mobility, granulation adjuvant is screened by spy, select starch, Icing Sugar, dextrin, four kinds of adjuvant alternately excipient of microcrystalline Cellulose, medicated powder is mixed in the ratio of 1:1 with adjuvant, sieves, 60 DEG C of dry 0.5h, to obtain final product.The investigation of situation, mobility and mouldability that prepared granule is sieved.Data are shown in Table 1-1 and table 1-2.

Table 1-1 medicated powder and ratio of adjuvant

Sieve situation, angle of repose and mouldability of table 1-2 is investigated

Use single adjuvant granulation can the group's of generation phenomenon, additionally, mobility is the best, mouldability is respectively less than 85%.Therefore intend filtering out preferably mixed accessories from above 4 kinds of adjuvants.

The screening of mixed accessories

Take five parts of same amount of medicated powder adjuvants different with proportioning respectively, sieve, mix homogeneously, 60 DEG C of dry 0.5h, with 80% appropriate ethanol soft material, cross 16 mesh sieves and pelletize, 60 DEG C of drying, granulate, to obtain final product^[68-72].It is shown in Table 1-3.

Table 1-3 medicated powder and ratio of adjuvant

The investigation of 2.1 Moisture percentage

By five parts of particle dryings to constant weight, the weighing botle of own constant weight is put into the granule of thick about 2mm, weighing botle is opened wide after putting into the drying tower filling sodium chloride supersaturated solution standing 1h, 3h, 8h, 24h, 48h, 72h, 96h, again weigh.Shared by the difference of twice weighing, the percent of granular mass is the Moisture percentage of granule.It is shown in Table 1-4.

The hydroscopicity table of five kinds of granules of table 1-4

2.2 critical relative humiditys measure

Take 5 kinds of granules being dried to constant weight respectively to be placed in the weighing botle of own labelling constant weight, tiling thickness about 2mm, uncovered weighing botle is respectively placed in the exsiccator of the supersaturated solution filling the sulfuric acid solution of 7 kinds of different sulfuric acid concentrations and salt, 48h is kept in 25 DEG C of constant incubators, then weigh, by calculating hydroscopicity the critical relative humidity of 5 kinds of freshly prepared granules of observation of mapping, it is shown in Table 1-5.

The critical relative humidity of five kinds of granules of table 1-5 measures table

The critical humidity of 5 kinds of granules is 73%, 78%, 78%, 81%, 73% respectively.

The mensuration of 2.3 mobility

Use fixed funnel method, 3 funnels connects and is fixed on height (H) place certain on the pan paper of horizontal positioned, carefully granule is poured in the funnel gone up most along hopper walls until the granule cone tips of formation touches bell mouth on pan paper.The diameter (2R) of conical base is measured, by angle of repose: tan α=2H/d calculates and get final product with slide gauge.It is shown in Table 1-6.

The mensuration of table 1-6 five kinds granule angle of repose

2.4 mouldabilities are investigated

Specify by under Chinese Pharmacopoeia 2010 version one (annex IC), use double sieve method.Take test sample l0g, weighed weight, put in a sieve (10 mesh), transfer on No. five sieves (80 mesh).Keeping level to sieve, left and right comes and goes, and sieves while tapping 3 minutes.Take and can not calculate percentage by a sieve and granules and powder that No. five sieves can be passed through, weighed weight.15% must not be crossed.Ratio of briquetting (%)=by No. 1 sieve and particle weight/granule gross weight × 100% not passing through No. 5 sieves.It is shown in Table 1-7.

The ratio of briquetting investigation table of five kinds of granules of table 1-7

2.5 overall merit

Use the comprehensive scoring method five groups of granule hygroscopicity to making, mobility, the integrated survey of mouldability, determine optimal experimental group, so that it is determined that optimal mixed accessories.It is shown in Table 1-8.

The comprehensive evaluation form of five kinds of granules of table 1-8

Note: S=(Xmin/X) * 20+(Ymin/Y) * 30+(Z/Zmax) * 30+(H/Hmax) * 20

By testing above it can be seen that No. 2 experiments are the most relatively superior to other prescriptions number at aspects such as hydroscopicity, mobility, mouldabilities, therefore experiment plan employing mixed accessories soluble starch: dextrin: lactose=7:1:1.

(2) medicated powder is investigated with the proportion compatibility of mixed accessories

By medicated powder and adjuvant respectively with 2:1, the ratio of 0.5:1,1:0.5,1:1,1:2 adds, sieves, mix homogeneously, 60 DEG C of dry half an hour, with appropriate ethanol soft material, and mistake 16 mesh sieves granulation, 60 DEG C of drying, granulate and get final product.And then determine the optimum proportioning of medicated powder and excipient.It is shown in Table 1-9.

The proportion compatibility of table 1-9 medicated powder and mixed accessories is investigated

When medicated powder and mixed accessories proportioning are 1:1 and 1:0.5 when, granulating efficiency is all preferable, but for reducing the adjuvant content in capsule 's content and preparation cost, so the medicated powder ratio of adjuvant granulating efficiency of selection 1:0.5 is best.

(3) wetting agent screening

Getting it filled after powder and the mixing of suitable adjuvant, be divided into 5 parts, select 20% ethanol, 60% ethanol, 70% ethanol, 70%+3% polyvidone respectively, 85% ethanol is wetting agent, pelletizes, compare the different wetting agent impact on granulating efficiency after making soft material.Choose the wetting agent that effect is best.It is shown in Table 1-10.

Table 1-10 wetting agent screens

Select 70% ethanol+3% polyvidone preferable as the wetting agent of granule as seen from the above table.

(4) particle drying technical study

Using far infrared constant temperature evaporation tank (baking oven) to be dried, the baking temperature more different by single factor exploration method and drying time are to ginsenoside Rg in finished particle₁Content and the impact of apparent mass of the content of moisture and granule^[70,71,73], thus screen optimum drying technique.

Taking 3 crowdes of each 50g of wet granular prepared through same process condition, rigid condition is to be dried 30min, 60min and 90min at 60 DEG C, and inspection target is ginsenoside Rg in granule₁With content and the apparent particle quality of moisture, the results are shown in Table 1-11.

Investigation tables drying time different during table 1-11 60 DEG C

By experimental result understand when baking temperature be 60 DEG C, drying time be 60min time, drying effect is best.When rigid condition is 60min, investigate different baking temperature 60 DEG C, 80 DEG C, 90 DEG C to inspection target: ginsenoside Rg₁With content and the impact of apparent particle quality of moisture, the results are shown in Table 1-12.

Baking temperature investigation tables different during table 1-12 60min drying time

Being understood in drying time by experimental data is under 60min, baking temperature is bigger to granule index composition influence, the change of other factors is inconspicuous, to sum up told, the drying process of this experiment selects baking temperature to be 60 DEG C, drying time is 60min, can prepare index component content high, the measured granule of matter.

Claims

1. the preparation method of the TIANQI TONGJING JIAONANG improved, it is characterised in that:

The preparation method of the TIANQI TONGJING JIAONANG of improvement the most according to claim 1, it is characterised in that: described filler be part by weight be the starch of 7:1:1, dextrin and lactose.

The preparation method of the TIANQI TONGJING JIAONANG of improvement the most according to claim 1, it is characterised in that: described wetting agent be weight percentage 70% ethanol solution and percentage by weight be 3% povidone solution.

The preparation method of the TIANQI TONGJING JIAONANG of improvement the most according to claim 1, it is characterised in that: step (2) described medicated powder and filler weight proportion are 1:0.5.