CN105300907A - Method for detecting intermediate products for pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center - Google Patents
Method for detecting intermediate products for pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center Download PDFInfo
- Publication number
- CN105300907A CN105300907A CN201510764205.1A CN201510764205A CN105300907A CN 105300907 A CN105300907 A CN 105300907A CN 201510764205 A CN201510764205 A CN 201510764205A CN 105300907 A CN105300907 A CN 105300907A
- Authority
- CN
- China
- Prior art keywords
- pharmaceutical preparation
- ethanol
- middle product
- weight portion
- add
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the field of traditional Chinese medicine preparation detection and particularly relates to a method for detecting intermediate products for a pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center. According to the method for detecting the intermediate products for the pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center, by selecting extract solvents, extract solvent amount and extraction methods and the like, atractylode total flavonoids in the intermediate products for the pharmaceutical preparation is extracted to the largest extent, and accordingly the content of atractylode total flavonoids is measured accurately. Experiments show that according to the detection method, not only can the content of atractylode total flavonoids in the intermediate products for the pharmaceutical preparation be measured accurately, but also the detection time is short, the quality difference and stability of the intermediate products of each batch can be evaluated quickly, and the method is favorable for effectively controlling medicine quality and improving medicine use safety and stability.
Description
Technical field
The invention belongs to Chinese medicine preparation detection field, be specifically related to a kind of detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect.
Background technology
HUOXIANG ZHENGQI JIAONANG forms by by Chinese medicines such as Pogostemon cablin, the bighead atractylodes rhizome (stir-fry), the bark of official magnolia (ginger system), rhizoma pinellinae praeparata, perilla leaf, the root of Dahurain angelica, dried orange peel, Poria cocos, balloonflower root, Radix Glycyrrhizae, date, the shell of areca nut, gingers, have induce sweat dampness dissipating, QI regulating and in effect, clinically for catching cold, internal injury humidity hysteresis, headache dusk the disease such as weight, abdominal distention, vomiting diarrhea.Wherein bark of official magnolia clearing damp disappears stagnant, and the root of Dahurain angelica induces sweat loose cold, and dampness elimination of holding concurrently is stagnant, and the bighead atractylodes rhizome replenishes qi to invigorate the spleen, and to help transporting, above-mentioned three taste medicinal materials all play a significant role in prescription.In the preparation technology of HUOXIANG ZHENGQI JIAONANG, the root of Dahurain angelica, rhizoma atractylodis macrocephalae and the ginger bark of official magnolia are mixed, adopt alcohol extracting method effective component extracting.At present, for the bighead atractylodes rhizome, mainly through atractylodes lactone constituents, it is differentiated and quality control, but the method is difficult to use in the quick detection of the middle product of HUOXIANG ZHENGQI JIAONANG.
" bighead atractylodes rhizome general flavone is differentiated and assay " (Hunan Normal University's journal (medicine), 2008, 5 (1), 16-19) disclose bighead atractylodes rhizome Determination Method of Flavone Content to comprise the following steps: accurately take a certain amount of sample, in Soxhlet extractor through petroleum ether degreasing to colourless, sherwood oil is produced after letting cool, add 95% ethanol, by the solid-to-liquid ratio of 16:1, refluxing extraction 2h at 80 DEG C, filter, reduced pressure concentration, dissolve with 95% ethanol, be settled to 100mL, accurate absorption constant volume liquid 8mL is in the volumetric flask of 25mL, measure its absorbance as follows, finally be calculated as follows out the content (g/g) of flavone compound in sample, rutin is dried to constant weight at 120 DEG C, accurately takes 0.0228g rutin standard items, the ethanol with 30% dissolves, and is settled to 50mL.Get above-mentioned rutin standard solution 1mL, 2mL, 3mL, 4mL, 5mL respectively in 5 25mL measuring bottles, add the ethanol of appropriate 30%, then add the NaNO of 0.7mL5%
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, the NaOH adding 5mL4% after 6min shakes up, and with the ethanol constant volume of 30%, measure in wavelength 510nm place after 10min, reagent is blank reference; Precision measures sample solution 3mL, by the method operation in the making of rutin standard curve, and the absorbance log that METHOD FOR CONTINUOUS DETERMINATION sample is 5 times.
Because the middle product of HUOXIANG ZHENGQI JIAONANG are made up of the root of Dahurain angelica, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia, connect each other between each Chinese medicine, interact, influence each other, the separating effect of other chemical compositions of the middle product of bighead atractylodes rhizome general flavone and HUOXIANG ZHENGQI JIAONANG is poor, thus causes carrying out assay.Therefore, " bighead atractylodes rhizome general flavone differentiate and assay " method and be not suitable for the assay of bighead atractylodes rhizome general flavone in the middle product of HUOXIANG ZHENGQI JIAONANG.
Therefore, set up a kind of detection method with bighead atractylodes rhizome general flavone in the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect, it is significant that the quality for HUOXIANG ZHENGQI JIAONANG carries out control comprehensively.
Summary of the invention
For this reason, to be solved by this invention is do not have the content assaying method of bighead atractylodes rhizome general flavone in the middle product of HUOXIANG ZHENGQI JIAONANG in prior art, cause the technical matters that can not control the quality of the bighead atractylodes rhizome in the middle product of HUOXIANG ZHENGQI JIAONANG, thus proposes a kind of detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect.
For solving the problems of the technologies described above, the present invention is achieved through the following technical solutions:
The invention provides a kind of detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect,
The bulk drug of the middle product of described pharmaceutical preparation consists of: the root of Dahurain angelica, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia;
This detection method comprises the following assay step to bighead atractylodes rhizome general flavone:
(1) preparation of need testing solution: the middle product getting pharmaceutical preparation to be measured, accurately weighed, porphyrize, get 0.4-0.6 weight portion, accurately weighed, in 250 parts by volume conical flasks, precision adds 60%-90% ethanol 40-60 parts by volume, weighed weight, and 85 DEG C add hot reflux 25-35min, let cool, supply the weight of less loss with 60%-90% ethanol, shake up, filter, get subsequent filtrate, as need testing solution;
(2) preparation of standard solution: precision takes 0.015-0.025 weight portion rutin standard items, dissolves with 25%-35% ethanol, and is settled to 50 parts by volume, as standard solution;
(3) measure: accurate absorption need testing solution and standard solution 1.0mL respectively, first adds 25%-35% ethanol 10mL, then add 0.7mL5%NaNO
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, add 5mL4%NaOH after placing 6min, shake up, with 25%-35% ethanol constant volume, after placing 10min, measure absorbance in wavelength 510nm place;
The pass of described weight portion and parts by volume is g/mL.
Preferably, the above-mentioned detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect of the present invention,
This detection method comprises the following assay step to bighead atractylodes rhizome general flavone:
(1) preparation of need testing solution: the middle product getting pharmaceutical preparation to be measured, accurately weighed, porphyrize, get 0.5 weight portion, accurately weighed, in 250 parts by volume conical flasks, precision adds 80% ethanol 50 parts by volume, weighed weight, and 85 DEG C add hot reflux 30min, let cool, supply the weight of less loss with 80% ethanol, shake up, filter, get subsequent filtrate, as need testing solution;
(2) preparation of standard solution: precision takes 0.020 weight portion rutin standard items, dissolves with 30% ethanol, and is settled to 50 parts by volume, as standard solution;
(3) measure: accurate absorption need testing solution and standard solution 1.0mL respectively, first adds 30% ethanol 10mL, then add 0.7mL5%NaNO
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, add 5mL4%NaOH after placing 6min, shake up, with 30% ethanol constant volume, after placing 10min, measure absorbance in wavelength 510nm place.
Further preferably, the above-mentioned detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect of the present invention, the bulk drug of the middle product of described pharmaceutical preparation consists of:
Root of Dahurain angelica 50-80 weight portion, rhizoma atractylodis macrocephalae 115-145 weight portion, ginger bark of official magnolia 115-145 weight portion.
Further preferably, the above-mentioned detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect of the present invention, the bulk drug of the middle product of described pharmaceutical preparation consists of:
The root of Dahurain angelica 65 weight portion, rhizoma atractylodis macrocephalae 130 weight portion, the ginger bark of official magnolia 130 weight portion.
Further preferably, the above-mentioned detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect of the present invention,
Described pharmaceutical preparation is tablet, capsule, pill, granule, honey refining pill, sustained release preparation, quick releasing formulation, controlled release preparation, oral liquid or ejection preparation.
Further preferably, the above-mentioned detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect of the present invention, the middle product of described pharmaceutical preparation are prepared by following methods:
Get the root of Dahurain angelica of selected weight portion, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia, with the general assembly (TW) of the potpourri of the root of Dahurain angelica, rhizoma atractylodis macrocephalae and the ginger bark of official magnolia for benchmark, add the 60%-80% ethanol of 3-7 weight times amount, soak at least 24h, forced circulation 2-5h, filter, it is 1.00-1.10 that filtrate is concentrated into 80 DEG C of relative densities, obtains the middle product of described pharmaceutical preparation.
Further preferably, the above-mentioned detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect of the present invention, the middle product of described pharmaceutical preparation are prepared by following methods:
Get the root of Dahurain angelica of selected weight portion, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia, with the general assembly (TW) of the potpourri of the root of Dahurain angelica, rhizoma atractylodis macrocephalae and the ginger bark of official magnolia for benchmark, add 70% ethanol of 5 weight times amount, soak at least 24h, forced circulation 3.5h, filter, it is 1.05 that filtrate is concentrated into 80 DEG C of relative densities, obtains the middle product of described pharmaceutical preparation.
Technique scheme of the present invention has the following advantages compared to existing technology:
The present invention has the detection method of the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect, by selective extraction solvent, Extraction solvent amount, extracting method etc., bighead atractylodes rhizome general flavone in the middle product of this pharmaceutical preparation is farthest extracted, thus exactly its content is measured.Experiment shows, this detection method not only can measure the content of the bighead atractylodes rhizome general flavone in the middle product of this pharmaceutical preparation exactly, and detection time is short, can the mass discrepancy of product and stability in the middle of each batch of Fast Evaluation, be conducive to controling effectively to the quality of this medicine, contribute to the safety and stability improving this drug use.
Accompanying drawing explanation
In order to make content of the present invention be more likely to be clearly understood, below according to a particular embodiment of the invention and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein:
Fig. 1 is the canonical plotting in experimental example of the present invention.
Embodiment
experimental example
1, the investigation of empirical factor
1.1 Extraction solvent are investigated
The middle product of pharmaceutical preparation prepared by Example 1, accurately weighed, porphyrize, gets in 1g to 100mL volumetric flask, add ethanol (40%, 50%, 70%, 80%, 95%, the 100%) 80mL of variable concentrations, ultrasonic 30min, lets cool, constant volume, shakes up, and waits to develop the color.
Specific experiment the results are shown in Table 1.
Table 1 Extraction solvent investigation table
As shown in Table 1, the content of 80% alcohol extract gained bighead atractylodes rhizome general flavone is the highest.Therefore, 80% alcohol extract is chosen.
1.2 extracting modes are investigated
(1) the middle product of the pharmaceutical preparation of Example 1 preparation, accurately weighed, porphyrize, gets in 1g to 100mL volumetric flask, adds 80% ethanol 80mL, and ultrasonic different time (0min, 15min, 30min), lets cool, constant volume, shake up, and waits to develop the color.
(2) the middle product of the pharmaceutical preparation of Example 1 preparation, accurately weighed, porphyrize, gets in 0.5g to 250mL conical flask, add 80% ethanol 50mL, weighed weight, adds hot reflux different time (30min, 1h, 2h) in 85 DEG C, lets cool, supply weight, shake up, filter, wait to develop the color.
Specific experiment the results are shown in Table 2.
Table 2 extracting method and extraction time are investigated
As shown in Table 2, the content of refluxing extraction 30min gained bighead atractylodes rhizome general flavone is the highest.Therefore, the extracting method of backflow 30min is chosen.
The investigation of 1.3 Extraction solvent amounts
The middle product of pharmaceutical preparation prepared by Example 1, accurately weighed, porphyrize, gets in 0.5g to 250mL conical flask, add 80% ethanol (25mL, 50mL) of different amount respectively, weighed weight, adds hot reflux 30min in 85 DEG C, lets cool, supply weight, shake up, filter, wait to develop the color.
Specific experiment the results are shown in Table 3.
The investigation of table 3 different solvents amount
As shown in Table 3, the content of the solvent extraction gained bighead atractylodes rhizome general flavone of 50mL is higher.Therefore, 50mL solvent extraction is chosen.
2, the detection method finally determined
The middle product of the pharmaceutical preparation of [preparation of sample] Example 1 preparation, accurately weighed, porphyrize, gets 0.5g, in 250mL conical flask, add 80% ethanol 50mL, weighed weight, add hot reflux 30min in 85 DEG C, let cool, supply weight, shake up, filter, measure its absorbance as follows.
[drafting of typical curve] accurately takes 20mg rutin standard items, and the ethanol with 30% dissolves, and is settled to 50mL.Get above-mentioned rutin standard solution 1mL, 2mL, 3mL, 4mL, 5mL respectively in 5 25mL measuring bottles, add the ethanol 10mL of 30%, then add the NaNO of 0.7mL5%
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, the NaOH adding 5mL4% after 6min shakes up, and with the ethanol constant volume of 30%, measure in wavelength 510nm place after 10min, reagent is blank reference.
[mensuration] precision draws testing sample solution 1.0mL, and the method under sighting target directrix curve item, from " adding the ethanol 10mL of 30% ", measures absorbance in accordance with the law.
3, methodological study
(1) investigation of the range of linearity
The accurate rutin standard solution (concentration is respectively 0.4505mg, 0.9010mg, 1.3514mg, 1.8019mg, 2.2524mg) drawing different volumes carries out ultraviolet determination respectively, absorbance is measured by said determination condition, and with absorbance (Y), rutin content (X) is returned, obtain canonical plotting, as shown in Figure 1.
(2) Precision Experiment
Get 1 part of need testing solution duplicate measurements 6 times, specific experiment the results are shown in Table 4.
Table 4 Precision Experiment result
As shown in Table 4, the RSD of the assay result that same need testing solution duplicate measurements is 6 times is 0.11%, shows that this detection method precision is good.
(3) stability experiment
Get same need testing solution, measure 7 times as stated above, specific experiment the results are shown in Table 5.
Table 5 stability experiment result
As shown in Table 5, need testing solution RSD in 2h is 3.02%, shows that this detection method is substantially comparatively stable.
(4) repeated experiment
By above assay method, prepare 6 parts of need testing solutions respectively to the middle product of pharmaceutical preparation prepared by embodiment 1, record absorbance and calculate content, specific experiment the results are shown in Table 6.
Table 6 repeated experiment result
As shown in Table 6, the RSD<2% of 6 parts of need testing solutions, shows this detection method repeatability better.
(5) average recovery experiment
Middle the product of pharmaceutical preparation prepared by the embodiment 1 of getting known content, precision adds a certain amount of rutin standard items respectively, and by test sample preparation and assay method, parallelly do 12 groups, specific experiment the results are shown in Table 7-1 and shows 7-2.
The experiment of table 7-1 average recovery
The experiment of table 7-2 average recovery
From table 7-1 and table 7-1, average recovery mean value is between 95.0% ~ 110.0%, and each RSD≤5%, meets the requirements, and shows that this detection method is feasible.
(6) sample size measures
Get the middle product of pharmaceutical preparation prepared by the 3 batches of embodiments 1, with final defining method, i.e. legal system available test sample solution carry out assay below " 2 " item, specific experiment the results are shown in Table 8.
Table 8 assay result
As shown in Table 8, the RSD of the assay result of the middle product of the pharmaceutical preparation of three batches of embodiment 1 preparations is all less than 2%, and in the middle of these three batches, the quality of product is ideal.
4, conclusion
In sum, the detection method that the present invention has middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect can detect the content of bighead atractylodes rhizome general flavone in the middle product of pharmaceutical preparation prepared by embodiment 1 exactly, be conducive to controling effectively to the quality of this medicine, contribute to the safety and stability improving this drug use.
embodiment 1there is the preparation of the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect
The bulk drug that the present embodiment has the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect consists of:
Root of Dahurain angelica 65g, rhizoma atractylodis macrocephalae 130g, ginger bark of official magnolia 130g;
Its preparation method comprises the following steps:
Get the root of Dahurain angelica of selected weight, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia, with the general assembly (TW) of the potpourri of the root of Dahurain angelica, rhizoma atractylodis macrocephalae and the ginger bark of official magnolia for benchmark, add 70% ethanol of 5 weight times amount, soak at least 24h, forced circulation 3.5h, filter, it is 1.05 that filtrate is concentrated into 80 DEG C of relative densities, obtains the middle product of described pharmaceutical preparation.
embodiment 2
The present embodiment has the detection method of the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect, and this detection method comprises the following assay step to bighead atractylodes rhizome general flavone:
(1) preparation of need testing solution: the middle product getting pharmaceutical preparation to be measured, accurately weighed, porphyrize, get 0.5 weight portion, accurately weighed, in 250 parts by volume conical flasks, precision adds 80% ethanol 50 parts by volume, weighed weight, and 85 DEG C add hot reflux 30min, let cool, supply the weight of less loss with 80% ethanol, shake up, filter, get subsequent filtrate, as need testing solution;
(2) preparation of standard solution: precision takes 0.020 weight portion rutin standard items, dissolves with 30% ethanol, and is settled to 50 parts by volume, as standard solution;
(3) measure: accurate absorption need testing solution and standard solution 1.0mL respectively, first adds 30% ethanol 10mL, then add 0.7mL5%NaNO
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, add 5mL4%NaOH after placing 6min, shake up, with 30% ethanol constant volume, after placing 10min, measure absorbance in wavelength 510nm place.
embodiment 3
The present embodiment has the detection method of the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect, and this detection method comprises the following assay step to bighead atractylodes rhizome general flavone:
(1) preparation of need testing solution: the middle product getting pharmaceutical preparation to be measured, accurately weighed, porphyrize, get 0.4g, accurately weighed, in 250mL conical flask, precision adds 90% ethanol 40mL, weighed weight, and 85 DEG C add hot reflux 35min, let cool, supply the weight of less loss with 90% ethanol, shake up, filter, get subsequent filtrate, as need testing solution;
(2) preparation of standard solution: precision takes 0.025g rutin standard items, dissolves with 25% ethanol, and is settled to 50mL, as standard solution;
(3) measure: accurate absorption need testing solution and standard solution 1.0mL respectively, first adds 25% ethanol 10mL, then add 0.7mL5%NaNO
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, add 5mL4%NaOH after placing 6min, shake up, with 25% ethanol constant volume, after placing 10min, measure absorbance in wavelength 510nm place.
embodiment 4
The present embodiment has the detection method of the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect, and this detection method comprises the following assay step to bighead atractylodes rhizome general flavone:
(1) preparation of need testing solution: the middle product getting pharmaceutical preparation to be measured, accurately weighed, porphyrize, get 0.6g, accurately weighed, in 250mL conical flask, precision adds 60% ethanol 60mL, weighed weight, and 85 DEG C add hot reflux 25min, let cool, supply the weight of less loss with 60% ethanol, shake up, filter, get subsequent filtrate, as need testing solution;
(2) preparation of standard solution: precision takes 0.015g rutin standard items, dissolves with 35% ethanol, and is settled to 50mL, as standard solution;
(3) measure: accurate absorption need testing solution and standard solution 1.0mL respectively, first adds 35% ethanol 10mL, then add 0.7mL5%NaNO
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, add 5mL4%NaOH after placing 6min, shake up, with 35% ethanol constant volume, after placing 10min, measure absorbance in wavelength 510nm place.
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.
Claims (7)
1. there is a detection method for the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect, it is characterized in that,
The bulk drug of the middle product of described pharmaceutical preparation consists of: the root of Dahurain angelica, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia;
This detection method comprises the following assay step to bighead atractylodes rhizome general flavone:
(1) preparation of need testing solution: the middle product getting pharmaceutical preparation to be measured, accurately weighed, porphyrize, get 0.4-0.6 weight portion, accurately weighed, in 250 parts by volume conical flasks, precision adds 60%-90% ethanol 40-60 parts by volume, weighed weight, and 85 DEG C add hot reflux 25-35min, let cool, supply the weight of less loss with 60%-90% ethanol, shake up, filter, get subsequent filtrate, as need testing solution;
(2) preparation of standard solution: precision takes 0.015-0.025 weight portion rutin standard items, dissolves with 25%-35% ethanol, and is settled to 50 parts by volume, as standard solution;
(3) measure: accurate absorption need testing solution and standard solution 1.0mL respectively, first adds 25%-35% ethanol 10mL, then add 0.7mL5%NaNO
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, add 5mL4%NaOH after placing 6min, shake up, with 25%-35% ethanol constant volume, after placing 10min, measure absorbance in wavelength 510nm place;
The pass of described weight portion and parts by volume is g/mL.
2. the detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect according to claim 1, is characterized in that,
This detection method comprises the following assay step to bighead atractylodes rhizome general flavone:
(1) preparation of need testing solution: the middle product getting pharmaceutical preparation to be measured, accurately weighed, porphyrize, get 0.5 weight portion, accurately weighed, in 250 parts by volume conical flasks, precision adds 80% ethanol 50 parts by volume, weighed weight, and 85 DEG C add hot reflux 30min, let cool, supply the weight of less loss with 80% ethanol, shake up, filter, get subsequent filtrate, as need testing solution;
(2) preparation of standard solution: precision takes 0.020 weight portion rutin standard items, dissolves with 30% ethanol, and is settled to 50 parts by volume, as standard solution;
(3) measure: accurate absorption need testing solution and standard solution 1.0mL respectively, first adds 30% ethanol 10mL, then add 0.7mL5%NaNO
2, shake up, after placing 6min, add 0.7mL10%Al (NO
3)
3, add 5mL4%NaOH after placing 6min, shake up, with 30% ethanol constant volume, after placing 10min, measure absorbance in wavelength 510nm place.
3. the detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect according to claim 1 and 2, is characterized in that, the bulk drug of the middle product of described pharmaceutical preparation consists of:
Root of Dahurain angelica 50-80 weight portion, rhizoma atractylodis macrocephalae 115-145 weight portion, ginger bark of official magnolia 115-145 weight portion.
4. the detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect according to claim 3, is characterized in that, the bulk drug of the middle product of described pharmaceutical preparation consists of:
The root of Dahurain angelica 65 weight portion, rhizoma atractylodis macrocephalae 130 weight portion, the ginger bark of official magnolia 130 weight portion.
5. having according to any one of claim 1-4 is induced sweat the detection method of middle product of pharmaceutical preparation of dampness dissipating, QI regulating and middle effect, it is characterized in that,
Described pharmaceutical preparation is tablet, capsule, pill, granule, honey refining pill, sustained release preparation, quick releasing formulation, controlled release preparation, oral liquid or ejection preparation.
6. having according to any one of claim 1-5 is induced sweat the detection method of middle product of pharmaceutical preparation of dampness dissipating, QI regulating and middle effect, and it is characterized in that, the middle product of described pharmaceutical preparation are prepared by following methods:
Get the root of Dahurain angelica of selected weight portion, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia, with the general assembly (TW) of the potpourri of the root of Dahurain angelica, rhizoma atractylodis macrocephalae and the ginger bark of official magnolia for benchmark, add the 60%-80% ethanol of 3-7 weight times amount, soak at least 24h, forced circulation 2-5h, filter, it is 1.00-1.10 that filtrate is concentrated into 80 DEG C of relative densities, obtains the middle product of described pharmaceutical preparation.
7. the detection method with the middle product of the pharmaceutical preparation of induce sweat dampness dissipating, QI regulating and middle effect according to claim 6, is characterized in that, the middle product of described pharmaceutical preparation are prepared by following methods:
Get the root of Dahurain angelica of selected weight portion, rhizoma atractylodis macrocephalae, the ginger bark of official magnolia, with the general assembly (TW) of the potpourri of the root of Dahurain angelica, rhizoma atractylodis macrocephalae and the ginger bark of official magnolia for benchmark, add 70% ethanol of 5 weight times amount, soak at least 24h, forced circulation 3.5h, filter, it is 1.05 that filtrate is concentrated into 80 DEG C of relative densities, obtains the middle product of described pharmaceutical preparation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510764205.1A CN105300907A (en) | 2015-11-11 | 2015-11-11 | Method for detecting intermediate products for pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510764205.1A CN105300907A (en) | 2015-11-11 | 2015-11-11 | Method for detecting intermediate products for pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN105300907A true CN105300907A (en) | 2016-02-03 |
Family
ID=55198419
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510764205.1A Pending CN105300907A (en) | 2015-11-11 | 2015-11-11 | Method for detecting intermediate products for pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105300907A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634530A (en) * | 2004-11-04 | 2005-07-06 | 贵阳云岩西创药物科技开发有限公司 | Modified Huoxiang Zhengqi drop pill and its preparation method |
| CN103417942A (en) * | 2013-08-13 | 2013-12-04 | 漳州片仔癀药业股份有限公司 | Preparation method of Huoxiang Zhengqi capsules |
| CN104606611A (en) * | 2014-12-29 | 2015-05-13 | 王琪 | Traditional Chinese medicine mixture for treating summer heat and damp disease |
-
2015
- 2015-11-11 CN CN201510764205.1A patent/CN105300907A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1634530A (en) * | 2004-11-04 | 2005-07-06 | 贵阳云岩西创药物科技开发有限公司 | Modified Huoxiang Zhengqi drop pill and its preparation method |
| CN103417942A (en) * | 2013-08-13 | 2013-12-04 | 漳州片仔癀药业股份有限公司 | Preparation method of Huoxiang Zhengqi capsules |
| CN104606611A (en) * | 2014-12-29 | 2015-05-13 | 王琪 | Traditional Chinese medicine mixture for treating summer heat and damp disease |
Non-Patent Citations (3)
| Title |
|---|
| 杨小红等: "白术总黄酮鉴别及含量测定", 《湖南师范大学学报（医学版）》 * |
| 林晓等: "白术总黄酮提取及其抗氧化活性的研究", 《白术总黄酮提取及其抗氧化活性的研究》 * |
| 黄海英: "白术活性成分的提取、纯化及功能性研究", 《中国优秀博硕士学位论文全文数据库（硕士） 医药卫生科技辑》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Liu et al. | Optimization of the extraction of total flavonoids from Scutellaria baicalensis Georgi using the response surface methodology | |
| CN101851261B (en) | Polygonum perfoliatum medicinal material, method for preparing reference substance of active constituents in preparation thereof as well as content determination method | |
| CN101703611B (en) | Quality detection method of Chinese angelica oral liquid for benefiting blood | |
| CN101149361A (en) | Gastrodia elata medicinal materials discrimination method | |
| CN103760254A (en) | Method for determining fingerprint spectrum of traditional Chinese medicine for treating coronary heart disease | |
| CN102048941B (en) | Quality control method of children-welfare tablets serving as Chinese medicinal preparation | |
| CN107677745A (en) | The quality determining method of Desmodium styracifolium extractive of general flavone | |
| CN105806978A (en) | Method for measuring phenolic compounds in immature bitter oranges or fructus aurantii through SPE-HPLC | |
| CN102335402A (en) | Detection method of Chinese preparation mixture for invigorating the spleen and replenishing qi | |
| CN103487538A (en) | Determination method for contents of a plurality of effective components in Huoxiang Zhengqi Liquid | |
| CN100358539C (en) | Quality control method for ginkgo-dipyridamine injection | |
| CN102520103A (en) | Contrast Chinese patent medicine extract of pills of six ingredients with rehmannia, and preparation method and application thereof | |
| CN104407092A (en) | Quality detection method of traditional Chinese medicinal composition with efficacy of appetizing and invigorating spleen | |
| CN103822888B (en) | Catch up with the quality determining method of yellow grass | |
| CN104330482A (en) | Method utilizing HPLC to simultaneously measure 17 characteristic components in tea | |
| CN102608249B (en) | Detection method of Tenghuang Jiangu pill | |
| CN105300907A (en) | Method for detecting intermediate products for pharmaceutical preparation having effects of relieving superficies, dissipating dampness, regulating qi and harmonizing the center | |
| CN101703583B (en) | Quality detection method of Xinning capsules | |
| CN102809618A (en) | Time-of-flight-mass spectrometry (TOF-MS) fingerprint spectrum determination method for Relinqing granules and Polygonum capitatum | |
| CN103604898B (en) | The benefit heart relaxes the fingerprint atlas detection method of preparation | |
| CN103076403B (en) | Inspection method for capsule for treating lower urinary tract infection | |
| CN103969356B (en) | A kind of discrimination method of the finger printing of red rooted salvia | |
| CN105092724B (en) | The construction method and its HPLC finger-prints of Chinese pothos herb HPLC finger-prints | |
| CN103083458A (en) | Warm light drink compound formula granule, as well as preparation method as well as detection method thereof | |
| CN104034839A (en) | Quality detection method of hepatitis B treatment capsule |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination |