CN102824457A - Eight-treasure motherwort active site and preparation process of capsules - Google Patents
Eight-treasure motherwort active site and preparation process of capsules Download PDFInfo
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Abstract
The invention provides a novel preparation method for preparing an eight-treasure motherwort active site and a preparation process of eight-treasure capsules. An SFC-CO2 method is adopted to extract volatile constituents in a prescription, and a microwave-assisted extraction method is used for extracting active constituents in the prescription. The preparation process is low in energy dissipation, short in time consumption, is complete in active constituent extraction in the obtained active site and high in content, and has good therapeutic effects.
Description
Technical field
The present invention relates to a kind of BAZHEN YIMU JIAONANG preparation technology, belong to the pharmaceutical technology (tcd) technical field.
Background technology
The eight delicacies with motherwort pill capsule comes from Jing-Yue Complete Works; Existing for " Chinese pharmacopoeia version in 2005 is recorded, and prescription consists of Herba Leonuri, Radix Codonopsis, Radix Rehmanniae Preparata, Rhizoma Atractylodis Macrocephalae (parched), Poria, Radix Angelicae Sinensis, Radix Paeoniae Alba, Rhizoma Chuanxiong and Radix Glycyrrhizae, has the effect that fills blood, transfers menstruation; The clinical plain body of women that is used for loses after empty or the serious disease prolonged illness or Qi and blood deficiency due to the severe loss of blood; Irregular menstruation loses the first-selected prescription of menoxenia for QI and blood is two.But honeyed pill is directly beaten powder with whole crude drug and is used as medicine, and dose is big, takes inconvenience, so the pharmaceuticals researcher develops the BAZHEN YIMU JIAONANG agent that makes things convenient for the patient to take.
Stachydrine is one of effective ingredient of Herba Leonuri, is the quality control index of Herba Leonuri, and Herba Leonuri is the monarch drug of BAZHEN YIMU JIAONANG, and is therefore to the assay of stachydrine, significant to the quality of control BAZHEN YIMU JIAONANG.
Traditional handicraft to the extraction process of BAZHEN YIMU JIAONANG is: volatile ingredient adopts water to steam the distillation mode and extracts, and the medicinal residues after extracting mix with other medicines again, obtain active site with water boiling and extraction.In the technology, during the vapor extraction volatile ingredient, composition extracts not exclusively; Loss of volatile oil is bigger, and extraction ratio is low, and adopts the decocting mode of boiling to extract the stachydrine in the Herba Leonuri; Extraction ratio is extremely low; The alkaloid in the Herba Leonuri can not be fully extracted,, the curative effect that Herba Leonuri is enriched blood and invigorated blood circulation in the prescription can not be given full play to such as the stachydrine constituents.And, adopt the water boiling and extraction mode, power consumption is high, length consuming time.
Therefore, need carry out certain improvement, to reach the higher purpose lower when the consumption energy consumption of extraction ratio to the technology of traditional BAZHEN YIMU JIAONANG.
Summary of the invention
The object of the present invention is to provide a kind of technology of active site of new preparation eight delicacies with motherwort Chinese prescription, technology of the present invention is consuming time few, and it is low to consume energy, and extraction efficiency is higher, and loss of effective components is littler, gained active site better efficacy.
Among the present invention, the prescription of said eight delicacies with motherwort Chinese prescription mainly is made up of following bulk drugs: the Herba Leonuri of 250-300 weight portion, the Radix Codonopsis of 60-80 weight portion; The Rhizoma Atractylodis Macrocephalae of 60-80 weight portion, the Poria of 60-80 weight portion, the Radix Glycyrrhizae of 30-40 weight portion; The Radix Angelicae Sinensis of 130-160 weight portion; The Radix Paeoniae Alba of 60-80 weight portion, the Rhizoma Chuanxiong of 60-80 weight portion, the Radix Rehmanniae Preparata of 130-160 weight portion.
Particularly, the preparation technology of the active site of eight delicacies with motherwort Chinese prescription according to the invention comprises the steps:
(1) respectively get the Radix Paeoniae Alba of 1/3 deal Poria and recipe quantity, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae of recipe quantity, be ground into coarse powder, with supercritical CO
2Extraction extracts volatile oil, collects volatile oil, and is subsequent use;
(3) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae medicinal residues and Herba Leonuri, Radix Codonopsis, Radix Rehmanniae Preparata, and the Poria that remains 2/3 deal are ground into coarse powder; Add 5 ~ 40 times of weight extraction solvents, soaked 2 ~ 8 hours, put in the microwave extraction tank; Carry out microwave extracting, isolated by filtration gets extract;
(4) microwave extracting gained extract being evaporated to relative density is 1.15 ~ 1.35 (60 ℃), gets extractum, adds the fine powder of gained in the step (1), mixing, and drying gets medicated powder.
Gained volatile oil and medicated powder are the active site of eight delicacies with motherwort Chinese prescription, or are called active component.
Among the present invention, supercritical CO
2In the extraction step, extraction temperature is 35 ~ 45 ℃, and extracting pressure is 15 ~ 45Mpa, and the extraction time is 1 ~ 2 hour, and more particularly, extraction temperature is 40 ℃, and extracting pressure is 20Mpa, and the extraction time is 1 hour.
Among the present invention; Used extraction solvent is preferably water or ethanol in the step (3); The ethanol of 50% ~ 80% (V/V) more preferably, the amount of used extraction solvent is the amount (V/W) of 5 ~ 40 times of medical materials, is preferably the ethanol extraction solvent (V/W) of 50% ~ 80% (V/V) of 20 ~ 30 times of amounts; That is, solid-liquid ratio of the present invention is 1:5 ~ 40 (W/V), is preferably 1:20 ~ 30 (W/V).Before the microwave extraction, spice earlier through 2 ~ 8 hours, be preferably 2 ~ 5 hours extraction solvent and soak after, be transferred to and carry out microwave extraction in the microwave extracting jar.
During microwave extraction, the power of used microwave extracting is 400 ~ 500W, 10 ~ 40 minutes microwave extracting time.Further, the medicinal liquid of the present invention after microwave extraction can be removed impurity such as some phlegmatic temperaments, tannic acid, inorganic elements through a column chromatography purification step, obtains purer active site, and the gained active site is prepared into capsule, and taking dose is littler.Particularly, said method is:
(1) respectively get the Radix Paeoniae Alba of 1/3 deal Poria and recipe quantity, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae of recipe quantity, be ground into coarse powder, with supercritical CO
2Extraction extracts volatile oil, collects volatile oil, and is subsequent use;
(3) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae medicinal residues and Herba Leonuri, Radix Codonopsis, Radix Rehmanniae Preparata, and the Poria that remains 2/3 deal are ground into coarse powder; Add 5 ~ 40 times of weight extraction solvents, soaked 2 ~ 8 hours, put in the microwave extraction tank; Carry out microwave extracting, isolated by filtration gets extract;
(4) the gained extract is added in the macroporous adsorptive resins of having handled well, uses earlier the distilled water eluting,, use 3 ~ 8 column volumes of ethanol elution of 60% ~ 80% (V/V) instead, collect ethanol elution to the water lotion clarification, subsequent use;
(5) cross ethanol elution behind the post, being evaporated to relative density is 1.15 ~ 1.35 (60 ℃), extractum, add the fine powder of gained in the step (1), mixing, drying, medicated powder.
Gained volatile oil and medicated powder are the active site of eight delicacies with motherwort Chinese prescription.
Wherein, used macroporous adsorbent resin, used macroporous resin filler is a D-101 type macroporous resin, during ethanol-eluting resin column, the consumption of eluent is 6 ~ 8 column volumes.
A purpose more of the present invention is to provide a kind of technology for preparing BAZHEN YIMU JIAONANG, and said technology comprises; Will above the active medicated powder of resulting eight delicacies with motherwort, add a certain amount of starch, be binding agent with the ethanol of 90% (V/V); The system soft material, sieves at granulation, drying, granulate, sprays into said volatile oil; Sealing incapsulates, and has both got capsule.
The advantage of technology of the present invention and traditional handicraft shows as: (1) extraction time shortens greatly, and power consumption is few; (2) active component volatile oil extraction yield is higher; (3) extraction of alkaloids composition is more complete in the Herba Leonuri, and stachydrine content is higher in the gained extractum; (4) compare with traditional handicraft, when changing into the crude drug dosage that gives equal parts, have good therapeutical effect.
Description of drawings:
Fig. 1-1 stachydrine hydrochloride reference substance chromatogram (concentration 0.512mg/ml).
Fig. 1-2 stachydrine hydrochloride reference substance chromatogram (concentration 1.024mg/ml).
The sample chromatogram figure of Fig. 1-3 method 1 preparation, 1 position, peak is a stachydrine hydrochloride.
The sample chromatogram figure of Fig. 1-4 method 2 preparations, 1 position, peak is a stachydrine hydrochloride.
The sample chromatogram figure of Fig. 1-5 method 3 preparations, 1 position, peak is a stachydrine hydrochloride.
The specific embodiment:
The present invention further illustrates through following embodiment, but any embodiment or its combination is not to be understood that and is the restriction to scope of the present invention or embodiment.Scope of the present invention is limited appended claims, and in conjunction with this description and the general general knowledge in this area, those of ordinary skills can clearly understand claims institute restricted portion.Under prerequisite without departing from the spirit and scope of the present invention, those skilled in the art can carry out any modification or change to technical scheme of the present invention, and this modification and change are also contained in the scope of the present invention.
Embodiment 1 traditional handicraft prepares the active medicated powder of gained BAZHEN YIMU JIAONANG
Herba Leonuri 273g, Radix Codonopsis 68g, Radix Rehmanniae Preparata 137g, Rhizoma Atractylodis Macrocephalae (parched) 68g, Poria 68g, Radix Angelicae Sinensis 137g, Radix Paeoniae Alba 68g, Rhizoma Chuanxiong 68g, Radix Glycyrrhizae 34g
Get the Poria (22g) of 1/3rd weight portions and the Radix Paeoniae Alba (68g) of said weight portion, be ground into fine powder, cross 60 mesh sieves, subsequent use; The Radix Angelicae Sinensis of said weight portion, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae (parched) distillating extracting oil, the aqueous solution after the distillation in addition device are collected, the Radix Codonopsis of medicinal residues and said weight portion, Radix Rehmanniae Preparata, Herba Leonuri, Radix Glycyrrhizae and remain the Poria decocte with water secondary of 2/3rds weight portions, 2 hours first time; 1.5 hours second time, decoction liquor is filtered, and filtrating merges, with the aqueous solution merging after the distillation; Relative density is 1.20 extractum when being concentrated into 60 ℃, adds said fine powder, stirs, the dry medicated powder that gets; Medicated powder adds appropriate amount of starch, and the ethanol with 90% is binding agent system soft material, granulation, drying, sprays into said volatile oil; Sealing incapsulates, every dress 0.28g; Promptly get, this is counted as crude drug the content of every gained BAZHEN YIMU JIAONANG, is equivalent to 0.921g.
The active site and the capsule thereof of embodiment 2 prepared eight delicacies with motherwort Chinese prescriptions of the present invention
Herba Leonuri 273g, Radix Codonopsis 68g, Radix Rehmanniae Preparata 137g, Rhizoma Atractylodis Macrocephalae (parched) 68g, Poria 68g, Radix Angelicae Sinensis 137g, Radix Paeoniae Alba 68g, Rhizoma Chuanxiong 68g, Radix Glycyrrhizae 34g
(1) get the Poria (22g) of 1/3rd weight portions and the Radix Paeoniae Alba (68g) of said weight portion, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae (parched) of said weight portion, be ground into coarse powder, extract with supercritical CO 2 extraction carrying out volatile ingredient; The supercritical carbon dioxide extraction condition is that extraction temperature is 40 ℃, and extracting pressure is 20Mpa, and the extraction time is 1 hour; Collect gained volatile oil, subsequent use; Medicinal residues after extracting are subsequent use;
(3) Radix Codonopsis of medicinal residues and said weight portion, Radix Rehmanniae Preparata, Herba Leonuri, Radix Glycyrrhizae and remain the Poria of 2/3rds weight portions; Be ground into coarse powder with 20 times of amount 60% ethanol (v/w); Soak after 3 hours, put in the microwave extraction device, carry out microwave extracting; The condition of microwave extracting is: microwave power 450W, 30 minutes extraction time.Behind microwave extracting, the gained extract filters, and collects filtrating, and filtrate decompression is concentrated into relative density and is about 1.30 (60 ℃), adds the fine powder in the above-mentioned steps (1), stirring and evenly mixing, and vacuum drying, pulverizing get medicated powder, and be subsequent use.
Above-mentioned medicated powder for preparing and volatile ingredient are the BAZHEN YIMU JIAONANG active site.
The BAZHEN YIMU JIAONANG preparation: the medicated powder with step in the above-mentioned steps (3) gained, add a spot of starch, the ethanol with 90% is binding agent system soft material, granulation, drying; Spray into said volatile oil, sealing incapsulates; Every dress 0.28g; Promptly get, this is counted as crude drug the content of every gained BAZHEN YIMU JIAONANG, is equivalent to 0.921g.
The active site and the capsule thereof of embodiment 3 prepared eight delicacies with motherwort Chinese prescriptions of the present invention
Herba Leonuri 273g, Radix Codonopsis 68g, Radix Rehmanniae Preparata 137g, Rhizoma Atractylodis Macrocephalae (parched) 68g, Poria 68g, Radix Angelicae Sinensis 137g, Radix Paeoniae Alba 68g, Rhizoma Chuanxiong 68g, Radix Glycyrrhizae 34g
(1) get the Poria (22g) of 1/3rd weight portions and the Radix Paeoniae Alba (68g) of said weight portion, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae (parched) of said weight portion, be ground into coarse powder, extract with supercritical CO 2 extraction carrying out volatile ingredient; The supercritical carbon dioxide extraction condition is that extraction temperature is 40 ℃, and extracting pressure is 20Mpa, and the extraction time is 1 hour; Collect gained volatile oil, subsequent use; Medicinal residues after extracting are subsequent use;
(3) Radix Codonopsis of medicinal residues and said weight portion, Radix Rehmanniae Preparata, Herba Leonuri, Radix Glycyrrhizae and remain the Poria of 2/3rds weight portions; Be ground into coarse powder with 20 times of amount 60% ethanol (v/w); Soak after 3 hours, put in the microwave extraction device, carry out microwave extracting; The condition of microwave extracting is: microwave power 450W, 30 minutes extraction time.Behind microwave extracting, the gained extract filters, and is subsequent use;
(4) gained filtrating behind the microwave extracting, on the D-101 type macroporous adsorptive resins handled well, use earlier the distilled water eluting; Be clarification to eluent, use 6 column volume amounts of ethanol elution of 75% instead, collect ethanol elution; Be evaporated to relative density and be 1.30 extractum (60 ℃), add the fine powder in the above-mentioned steps (1), stirring and evenly mixing; Vacuum drying, pulverizing get medicated powder, and be subsequent use.
Above-mentioned medicated powder for preparing and volatile ingredient are the BAZHEN YIMU JIAONANG active site.
The BAZHEN YIMU JIAONANG preparation: the medicated powder with step in the above-mentioned steps (4) gained, add a spot of starch, the ethanol with 90% is binding agent system soft material, granulation, drying; Spray into said volatile oil, sealing incapsulates; Every dress 0.20g; Promptly get, this is counted as crude drug the content of every gained BAZHEN YIMU JIAONANG, is equivalent to 0.921g.
The active site of embodiment 4 prepared eight delicacies with motherwort Chinese prescriptions of the present invention
Herba Leonuri 250g, Radix Codonopsis 60g, Radix Rehmanniae Preparata 130g, Rhizoma Atractylodis Macrocephalae (parched) 60g, Poria 60g, Radix Angelicae Sinensis 130g, Radix Paeoniae Alba 60g, Rhizoma Chuanxiong 60g, Radix Glycyrrhizae 30g
(1) get the Poria (20g) of 1/3rd weight portions and the Radix Paeoniae Alba (60g) of said weight portion, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae (parched) of said weight portion, be ground into coarse powder, extract with supercritical CO 2 extraction carrying out volatile ingredient; The supercritical carbon dioxide extraction condition is that extraction temperature is 35 ℃, and extracting pressure is 15Mpa, and the extraction time is 1 hour; Collect gained volatile oil, subsequent use; Medicinal residues after extracting are subsequent use;
(3) Radix Codonopsis of medicinal residues and said weight portion, Radix Rehmanniae Preparata, Herba Leonuri, Radix Glycyrrhizae and remain the Poria of 2/3rds weight portions; Be ground into coarse powder with 20 times of amount 50% ethanol (v/w); Soak after 2 hours, put in the microwave extraction device, carry out microwave extracting; The condition of microwave extracting is: microwave power 400W, 10 minutes extraction time.Behind microwave extracting, the gained extract filters, and collects filtrating, and filtrate decompression is concentrated into relative density and is about 1.15 (60 ℃), adds the fine powder in the above-mentioned steps (1), stirring and evenly mixing, and vacuum drying, pulverizing get medicated powder, and be subsequent use.
Above-mentioned medicated powder for preparing and volatile ingredient are the BAZHEN YIMU JIAONANG active site
The active site of embodiment 5 prepared eight delicacies with motherwort Chinese prescriptions of the present invention
Herba Leonuri 300g, Radix Codonopsis 80g, Radix Rehmanniae Preparata 160g, Rhizoma Atractylodis Macrocephalae (parched) 80g, Poria 80g, Radix Angelicae Sinensis 160g, Radix Paeoniae Alba 80g, Rhizoma Chuanxiong 80g, Radix Glycyrrhizae 40g
(1) get the Poria (27g) of 1/3rd weight portions and the Radix Paeoniae Alba (80g) of said weight portion, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae (parched) of said weight portion, be ground into coarse powder, extract with supercritical CO 2 extraction carrying out volatile ingredient; The supercritical carbon dioxide extraction condition is that extraction temperature is 45 ℃, and extracting pressure is 45Mpa, and the extraction time is 2 hours; Collect gained volatile oil, subsequent use; Medicinal residues after extracting are subsequent use;
(3) Radix Codonopsis of medicinal residues and said weight portion, Radix Rehmanniae Preparata, Herba Leonuri, Radix Glycyrrhizae and remain the Poria of 2/3rds weight portions; Be ground into coarse powder with 30 times of amount 80% ethanol (v/w); Soak after 5 hours, put in the microwave extraction device, carry out microwave extracting; The condition of microwave extracting is: microwave power 500W, 30 minutes extraction time.Behind microwave extracting, the gained extract filters, and collects filtrate for later use;
(4) gained filtrating behind the microwave extracting, on the D-101 type macroporous adsorptive resins handled well, use earlier the distilled water eluting; Be clarification to eluent, use 5 column volume amounts of ethanol elution of 70% instead, collect ethanol elution; Be evaporated to relative density and be 1.30 extractum (60 ℃), add the fine powder in the above-mentioned steps (1), stirring and evenly mixing; Vacuum drying, pulverizing get medicated powder, and be subsequent use;
Above-mentioned medicated powder for preparing and volatile ingredient are the BAZHEN YIMU JIAONANG active site.
Embodiment 6 vapor distillations and SFC-CO
2Extract the volatile oil yield relatively
In embodiment 1 and embodiment 2 methods, the volatile oil extraction ratio is relatively seen table 1
Table 1 distinct methods to volatile ingredient extraction ratio in the prescription relatively
From table 1, can find out, adopt SFC-CO
2Mode extracts the volatile oil in Radix Angelicae Sinensis, Rhizoma Chuanxiong and the Rhizoma Atractylodis Macrocephalae in the BAZHEN YIMU JIAONANG, and its volatile oil yield is higher, extracts more complete.
The prescription that takes by weighing same amount is formed (with the Poria and the Radix Paeoniae Alba of recipe quantity of removing 1/3rd amounts, residue prescription medical material total amount is that 100g counts), presses the method for embodiment 1,2 and 3; After carrying out the volatile ingredient extraction; Extract other effective ingredient again, after the method for embodiment 1 is boiled to decocting, all aqueous extracts; Concentrating under reduced pressure, dry, pulverize medicated powder I; Embodiment 2 arrives the microwave extraction liquid after the step 3, and directly concentrate drying, pulverizing gets medicated powder II; Embodiment 3 to step 4 cross that the gained alcohol eluen directly concentrates behind the post, dry, pulverize medicated powder III; Compare Determination of Contents of Hydrochloric Stachydrine among medicated powder I, medicated powder II and the medicated powder III; Determination of Contents of Hydrochloric Stachydrine is measured and is adopted HPLC, sees table 2 and reference substance Fig. 1-1,1-2 and sample drawing 1-3,1-4,1-5.
Table 2 distinct methods extracts gained medicated powder Determination of Contents of Hydrochloric Stachydrine relatively
From table 2, can find out, adopt the microwave extracting method, the prescription yield of extract improves; And Determination of Contents of Hydrochloric Stachydrine obviously will be higher than and uses boiling water extraction method in the extractum, and the extraction rate of transform of total stachydrine hydrochloride obviously raises; After macroporous adsorbent resin was further refining, extractum content reduced, and Determination of Contents of Hydrochloric Stachydrine raises; But the amount of total stachydrine hydrochloride only has the minimizing of very small amount, and refining effect is more satisfactory.
Experiment medicine: (1) embodiment 1 prepared gained BAZHEN YIMU JIAONANG; (2) BAZHEN YIMU JIAONANG that obtains of embodiment 2 prepared; (3) BAZHEN YIMU JIAONANG that obtains of embodiment 3 prepared; (4) synestrin tablets: south China pharmaceutical factory produces, and is made into the suspension of desired concn in the experiment with distilled water.
Experiment reagent: (1) estradiol radioimmunological kit: Depew, Tianjin company limited; (2) progesterone radioimmunological kit: China Atomic Energy Science Research Institute.
Experimental technique: get body weight and be 70 of the female immaturity SD rats of 80-100g, be divided into blank group, positive controls, traditional handicraft BAZHEN YIMU JIAONANG group at random, and the high, medium and low dose groups of the embodiment of the invention 3 technology gained BAZHEN YIMU JIAONANGs; The embodiment of the invention 2 technology gained BAZHEN YIMU JIAONANG groups, totally 7 groups, each group is by every 100g body weight 1ml medicine liquid irrigation stomach; The blank group gives the normal saline of equivalent, and positive controls gives the diethylstilbestrol of 0.018mg/kg, and BAZHEN YIMU JIAONANG gives 0.84g crude drug/kg female Mus for commercially available group; Technology of the present invention (embodiment 3 technologies) gained BAZHEN YIMU JIAONANG group gives 0.84g crude drug/kg, 0.56g crude drug/kg, 0.28g crude drug/kg, and the embodiment of the invention 2 technology gained BAZHEN YIMU JIAONANG groups give 0.84g crude drug/kg rat, once a day; Successive administration 10 days, 1h after the last administration, blood sampling after each Mus is weighed; Get serum and measure the content of serum estradiol (E2) and progesterone (P) with radioimmunoassay method; And get uterus, ovary, and weigh with torsion balance, calculate the corresponding organs coefficient; Compare each group difference with the t check, the result sees table 3 and table 4.
Each group of table 3 is to female young Mus sexual organ's influence (x ± s)
Compare * P with the blank group<0.05, * * P<0.01; Compare with traditional handicraft gained BAZHEN YIMU JIAONANG,
#P<0.05
Can know that by table 3 positive controls, traditional handicraft group gained BAZHEN YIMU JIAONANG group, technology of the present invention are respectively organized female young Mus uterus organ coefficient and all increased than the blank group, t checks has significant difference (P 0.05, P 0.01).Compare with traditional handicraft gained BAZHEN YIMU JIAONANG group; The prepared BAZHEN YIMU JIAONANG that obtains of technology of the present invention; Under the situation that is equal to crude drug dosage, (all give 0.084g crude drug/100g Mus); Technology group of the present invention is more obvious to the raising of the uterus organ coefficient of female young Mus, and wherein embodiment 3 technology group high dose differences have significance (P < 0.05), and dose groups and low dose group and traditional handicraft gained BAZHEN YIMU JIAONANG group among the present invention; The uterus organ coefficient is increased quite, and difference does not have significance to each other.The above results proves, adopts the BAZHEN YIMU JIAONANG of technology gained of the present invention, the BAZHEN YIMU JIAONANG for preparing with traditional handicraft; Under the situation that is equal to crude drug dosage; It is more obvious on female young Mus uterus organ coefficient is increased, better effects if, and embodiment 2 is suitable with embodiment 3 effects; Just the total dose that extracts of each capsule of embodiment 3 still less can be still less when taking.
Each group of table 4 is to the influence of female young Mus gonadal hormone (x ± s)
Compare * P with the blank group<0.05, * * P<0.01; Compare with traditional handicraft gained BAZHEN YIMU JIAONANG,
#P<0.05
Can know that from table 4 result the level of the female young Mus serum estradiol of each drug group all obviously increases than the blank group, and all significant differences is arranged (P 0.01); Compare with the BAZHEN YIMU JIAONANG that traditional handicraft prepares, the prepared BAZHEN YIMU JIAONANG that obtains of technology of the present invention is equal under the situation of dosage (amounting to the crude drug that becomes to be equal to is as the criterion); The prepared capsule that obtains of technology of the present invention; It is more obvious that female young Mus serum estradiol level is raise, but in the embodiment of the invention 3 technologies between dose groups, low dose group and traditional handicraft group, to the rising of estradiol level; Difference is not obvious; During with dosage, difference is also not obvious, but all will obviously be better than the traditional handicraft group with 3 two technologies of embodiment for embodiment 2.Explain, adopt technology gained BAZHEN YIMU JIAONANG of the present invention, be equal under the dosage, in the rising to the female mice serum estradiol, have more remarkable advantages.
Each administration group is to also all reducing the level of female young Mus serum progesterone, and each administration group difference is not obvious.
The experiment medicine: (1) traditional handicraft prepares the gained BAZHEN YIMU JIAONANG; (2) technology gained BAZHEN YIMU JIAONANG of the present invention, embodiment 2 and embodiment 3 technologies.
Laboratory animal: Kunming mouse, female, body weight 18 ~ 22g, the Jiangxi College of Traditional Chinese Medicine laboratory animal department of the Chinese Academy of Sciences provides.
Experimental technique: 60 mices are divided into 6 groups at random, 10 every group, are respectively model of blood dificiency group, traditional handicraft gained BAZHEN YIMU JIAONANG group, the high, medium and low dose groups of the embodiment of the invention 3 technology gained BAZHEN YIMU JIAONANGs, 2 groups of the embodiment of the invention.Each organizes the equal eye socket blood sampling of mice 0.5ml, surveys hemoglobin (Hb) and erythrocyte (RBC) counting simultaneously, gets blood behind the 24h that loses blood again and surveys Hb and RBC; And administration every day, the traditional handicraft BAZHEN YIMU JIAONANG gives 1.68g crude drug/kg mice, and the embodiment of the invention 3 technology groups give 1.68,1.12,0.56g crude drug/kg mice; The embodiment of the invention 2 technology groups give 1.68 g crude drug/kg mice, gastric infusion once a day, capacity is the 0.2ml/10g body weight; The model of blood dificiency group gives the normal saline of equivalent, and successive administration 7 days was got blood and surveyed Hb and RBC on the 8th; Adopt relatively each group difference situation of t check, the result sees table 5 and table 6.
The influence of table 5 pair losing blood property blood deficiency mice hemoglobin
Compare * P with the model of blood dificiency group<0.05, * * P<0.01; Compare with traditional handicraft gained BAZHEN YIMU JIAONANG,
#P<0.05
The influence of table 6 pair losing blood property blood deficiency mouse red blood cell counting
Compare * P with the model of blood dificiency group<0.05, * * P<0.01; Compare with traditional handicraft gained BAZHEN YIMU JIAONANG,
#P<0.05
Can know by table 5,6, before losing blood property mice Hb and RBC counting all is starkly lower than and loses blood, successive administration respectively organize after 7 days mice Hb and RBC counting all apparently higher than the model of blood dificiency group (P 0.05 or P 0.01), show that BAZHEN YIMU JIAONANG has blood tonification effect.Technology gained BAZHEN YIMU JIAONANG group of the present invention prepares gained BAZHEN YIMU JIAONANG group (commercially available BAZHEN YIMU JIAONANG) with traditional handicraft and compares; Technology high dose group of the present invention is (after amounting to into crude drug; Dosage is equal to the traditional handicraft group) will be to the rising of mice Hb and the RBC counting of losing blood apparently higher than the traditional handicraft group, difference has significance (P < 0.05), between other each group; Difference is not obvious; No significance shows that technology group of the present invention is being equal under the situation of dosage, the blood tonification effect of losing blood property mice is better than traditional handicraft prepares resultant BAZHEN YIMU JIAONANG; The effect of the embodiment of the invention 3 technology groups will be better than embodiment 2 technology groups a little, but difference does not have significance between the two.
Claims (10)
1. the method for preparing of an eight delicacies with motherwort Chinese prescription active site, the crude drug of wherein said eight delicacies with motherwort Chinese prescription comprises: the Herba Leonuri of 250-300 weight portion, the Radix Codonopsis of 60-80 weight portion; The Rhizoma Atractylodis Macrocephalae of 60-80 weight portion, the Poria of 60-80 weight portion, the Radix Glycyrrhizae of 30-40 weight portion; The Radix Angelicae Sinensis of 130-160 weight portion; The Radix Paeoniae Alba of 60-80 weight portion, the Rhizoma Chuanxiong of 60-80 weight portion, the Radix Rehmanniae Preparata of 130-160 weight portion; It is characterized in that said method for preparing comprises the steps:
(1) respectively get the Radix Paeoniae Alba of 1/3 deal Poria and recipe quantity, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae of recipe quantity, be ground into coarse powder, with supercritical CO
2Extraction extracts volatile oil, collects volatile oil, and is subsequent use;
(3) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae medicinal residues and Herba Leonuri, Radix Codonopsis, Radix Rehmanniae Preparata, and the Poria that remains 2/3 deal are ground into coarse powder; Add 5 ~ 40 times of amount extraction solvents (V/W), soaked 2 ~ 8 hours, put in the microwave extraction tank; Carry out microwave extracting, isolated by filtration gets extract;
(4) microwave extracting gained extract being evaporated to relative density is 1.15 ~ 1.35 (60 ℃), gets extractum, adds the fine powder of gained in the step (1), mixing, and drying gets medicated powder;
(5) gained volatile oil and the middle gained medicated powder of step (4) in the step (2) are the active site of eight delicacies with motherwort Chinese prescription.
2. method for preparing according to claim 1, wherein supercritical CO described in the step (2)
2The extraction temperature of extraction is 35 ~ 45 ℃, and extracting pressure is 15 ~ 45MPa, and the extraction time is 1 ~ 2 hour.
3. method for preparing according to claim 1, wherein supercritical CO described in the step (2)
2The extraction temperature of extraction is 40 ℃, and extracting pressure is 20MPa, and the extraction time is 1 hour.
4. method for preparing according to claim 1, wherein the solvent of extraction described in the step (3) is the ethanol of water or 50% ~ 80% (V/V).
5. method for preparing according to claim 4, wherein said extraction solvent are the ethanol of 50% ~ 80% (V/V), and the addition of extraction solvent is 20 ~ 30 times of amounts (V/W), and soak time is 2 ~ 5 hours.
6. method for preparing according to claim 1, wherein, the power of said microwave extracting is 400 ~ 500W, the microwave extracting time is 10 ~ 40 minutes.
7. method for preparing according to claim 6, wherein, the power of said microwave extracting is 450W, the microwave extracting time is 30 minutes.
8. according to any described method for preparing of claim in the claim 1 ~ 7, it is characterized in that said method for preparing comprises the steps:
(1) respectively get the Radix Paeoniae Alba of 1/3 deal Poria and recipe quantity, be ground into fine powder, cross 60 mesh sieves, subsequent use;
(2) get Radix Angelicae Sinensis, Rhizoma Chuanxiong, the Rhizoma Atractylodis Macrocephalae of recipe quantity, be ground into coarse powder, with supercritical CO
2Extraction extracts volatile oil, collects volatile oil, and is subsequent use;
(3) Radix Angelicae Sinensis, Rhizoma Chuanxiong, Rhizoma Atractylodis Macrocephalae medicinal residues and Herba Leonuri, Radix Codonopsis, Radix Rehmanniae Preparata, and the Poria that remains 2/3 deal are ground into coarse powder; Add 5 ~ 40 times of weight extraction solvents, soaked 2 ~ 8 hours, put in the microwave extraction tank; Carry out microwave extracting, isolated by filtration gets extract;
(4) the gained extract is added in the macroporous adsorptive resins of having handled well, uses earlier the distilled water eluting,, use 3 ~ 8 column volumes of ethanol elution of 60% ~ 80% (V/V) instead, collect ethanol elution to the water lotion clarification, subsequent use;
(5) cross ethanol elution behind the post, being evaporated to relative density is 1.15 ~ 1.35 (60 ℃), extractum, add the fine powder of gained in the step (1), mixing, drying, medicated powder;
(6) gained volatile oil and the middle gained medicated powder of step (5) in the step (2) are the active site of eight delicacies with motherwort Chinese prescription.
9. preparation technology according to claim 8, the alcoholic acid elution volume of wherein said 60% ~ 80% (V/V) is 6 ~ 8 column volumes.
10. a method for preparing BAZHEN YIMU JIAONANG is characterized in that, with the medicated powder of step (5) gained any among the medicated powder of step any among the claim 1-7 (4) gained or the claim 8-10; Add starch; Ethanol with 90% (V/V) is binding agent, makes soft material, granulation, drying, granulate, sieves, and gets granule; In incapsulating, promptly get capsule.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104474113A (en) * | 2014-11-27 | 2015-04-01 | 江西百神药业股份有限公司 | Preparation method of Bazhen Yimu pill composition |
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| CN1456206A (en) * | 2003-01-03 | 2003-11-19 | 江西南昌桑海制药厂 | Qi-blood tonifying capsule |
| CN1712060A (en) * | 2005-06-23 | 2005-12-28 | 修涞贵 | Preparation of Chinese medicinal mixture for treating gynecologic menstrual disease |
| CN101874852A (en) * | 2010-04-28 | 2010-11-03 | 江西南昌桑海制药厂 | Quality detecting method of restorex plus extract capsule |
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| JPH04288016A (en) * | 1991-03-14 | 1992-10-13 | Tokai Capsule Kk | Production of soft capsule agent of active type vitamin d3s |
| CN1364514A (en) * | 2001-01-16 | 2002-08-21 | 杨孟君 | Nano eight ingredient motherwort medicine and its preparing method |
| CN1456206A (en) * | 2003-01-03 | 2003-11-19 | 江西南昌桑海制药厂 | Qi-blood tonifying capsule |
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| CN104474113B (en) * | 2014-11-27 | 2016-08-24 | 江西百神药业股份有限公司 | A kind of preparation method of bazhen yimu pills, bazhen yimu wan compositions |
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Application publication date: 20121219 |