CN104931445A - Content detecting method for traditional Chinese medicine composition for ischemia and lochia after delivery - Google Patents
Content detecting method for traditional Chinese medicine composition for ischemia and lochia after delivery Download PDFInfo
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Abstract
The invention aims to disclose a content measuring method for a traditional Chinese medicine composition for ischemia and lochia after delivery. The content measuring method is characterized by comprising the following steps: taking and precisely weighing 0.4g of a ferrous sulfate reference substance, adding a sulfuric acid solution to dissolve the ferrous sulfate reference substance to obtain a mixture I, and precisely measuring and taking 2ml of the mixture I to obtain a reference substance solution; precisely measuring and taking the reference substance solution, respectively adding the reference substance solution into 25ml measuring flasks, adding water until the solution is 10 ml, adding 1ml of a 1% hydroxylamine hydrochloride solution and 1ml of 0.2% 2,2-dipyridyl to uniformly mix to obtain a mixture II, and drawing standard curves; precisely measuring and taking the mixture II, dropwise adding 0.5-5% sodium hydroxide solution into the mixture II until the pH of the mixture II is 3.0-5.5, adding 1ml of the 1% hydroxylamine hydrochloride solution and 1ml of a 0.2% 2,2-dipyridyl alcohol solution into the mixture II to obtain a mixture III, measuring absorbancy of the mixture III, and reading the weight of ferrous sulfate in test sample solutions from the standard curves. The technical problem to be solved by the invention is to improve the defects of an original content measuring method, and improve the accuracy and the controllability of the product quality.
Description
One, technical field: the present invention relates to a kind of detection method of content, particularly relate to
a kind of for postpartum ischemic, lochia the detection method of content of Chinese medicine composition.
Two, background technology:
The a variety of causes iron deficiency that hypoferric anemia refers to causes RBC acceptor garland rate to reduce the anaemia caused, refer to that the demand and supply of body to iron is unbalance, to the greatest extent, then Erythrocyte Iron lacks thus the anaemia caused, and hypoferric anemia is modal anaemia to cause storage iron loss in body.This disease is common type in anaemia, is prevalent in all over the world.Adding up according to the World Health Organization (WHO): about there is 3,000,000,000 people anaemia in various degree in the whole world, causing that the number of various diseases and death is up to ten million because suffering from anaemia every year.The population probability of middle national trouble anaemia is higher than west
country, in the crowd suffering from anaemia, women is apparently higher than the male sex, and old man and children are higher than the young and the middle aged.
More owing to relatively losing blood in stages of labor, postpartum more easily causes puerpera's anaemia.Anaemia not only affects puerpera's physical recovery speed, and provides newborn nutrition and affect, and therefore early prevention and treatment has vital role to prevention postpartum anemia.Postpartum anemia common symptoms drops to master with malaise, poor appetite, resistibility, and severe complication can occur, and clinical slight postpartum anemia (90g/L) is generally corrected can improve by diet.But moderate postpartum anemia (60-90g/L) is treated except dietary adjustments external demand adds medicine.Common oral benefit iron medicine has certain gastrointestinal side effect, as being forced to drug withdrawal when the patient such as Nausea and vomiting, anorexia must not tolerate more.Cause puerpera's physiology, psychological torment and misery especially.
Iron supplementary on market is based on Western medicine, and it just carries out merely supplementing of iron, and its toxic and side effect usually makes patient puzzled simultaneously; Some Chinese medicine iron supplementary are usually because be health products not curative effects and allow patient be at a loss accurately.The problem that ubiquity iron absorptivity of enriching blood is low, takes effect too slow; Some product is with simple chemical iron for principal ingredient, and dosage is difficult to grasp, and excessive irony is deposited in brain tissue, bone, impairs one's health; Many product meeting stimulating gastrointestinals of enriching blood, have mended blood and have hindered stomach; Mouthfeel is bad, iron taste weight, and people are reluctant to eat.That treats anaemia is strengthening the spleen and replenishing qi at all, recovers the transportation capabilities of taste, promotes absorbing of iron.Tangible blood, is born in invisible gas.Blood nourishing oral liquid is exactly blood yiqi, strengthening the spleen and stomach, with the source of abundant anger; Be equipped with date to enrich blood, then Yin grows while yang is generating, the symptom of anaemia is improved rapidly.Sea-buckthorn has obviously anti-oxidant and reduction hyperlipidemia.For the treatment of anaemia, adopt ferrotherapy both at home and abroad at present more.But take the spinoff that chalybeate brings, as anorexia, Nausea and vomiting, diarrhoea etc., not easily by patient is accepted long-term, high-dose.
The formulation ingredients of Chinese medicine is many, and pre-treatment difficulty is larger, and interference is many.Detection method is advanced, eliminates interference, precision and favorable reproducibility, comprehensively can carry out quality control to this medicine, ensures stability, the homogeneity of product quality.About the composition of iron content, in the content assaying method of prior art, the content going out active principle of mensuration is on the low side, inaccurate, is difficult to the quality that science controls product accurately.
Three, summary of the invention:
The object of the invention is to provide
a kind of for postpartum ischemic, lochia the detection method of content of Chinese medicine composition
The present invention seeks to be achieved through the following technical solutions:
The content assaying method of medicine Chinese medicinal composition preparation of the present invention comprises:
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 5 ~ 15ml, puts in 100ml measuring bottle, and instillation 0.5% ~ 5% sodium hydroxide solution is 3.0 ~ 5.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product;
The content assaying method of medicine Chinese medicinal composition preparation of the present invention preferably includes:
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% ~ 2% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instilling 1% sodium hydroxide solution to PH is 3.5 ~ 4.5, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, must not be less than 45mg containing melanterite.
Indication of the present invention for postpartum ischemic, the bulk drug of Chinese medicine composition of lochia and proportioning be: (by weight)
Melanterite 2 ~ 8 weight portion, sea-buckthorn 180 ~ 220 weight portion, hawthorn 80 ~ 120 weight portion, date 80 ~ 120 weight portion.
The bulk drug composition optimum ratio of drug combination preparation of the present invention is (by weight):
Melanterite 5.3 weight portion, sea-buckthorn 200 weight portion, hawthorn 100 weight portion, date 100 weight portion.
Above four traditional Chinese medicine conventionally can make clinical acceptable formulation, as tablet, granule, capsule, oral liquid, dripping pill, controlled release preparation, injection.
The preparation method of this drug combination preparation can be:
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.2 ~ 0.8g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
The preparation method of this drug combination preparation is preferably:
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second time 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.56g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
The preparation method of this drug combination preparation can also be:
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second time 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing; get Sodium Benzoate 2g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml; stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Technical matters to be solved by this invention is the defect improving original content assaying method, the accuracy of improving the quality of products and controllability.The Chinese medicine composition that the present invention studies is made up of melanterite, sea-buckthorn, hawthorn, date, melanterite is as the monarch drug in a prescription of we, its principal ingredient iron is also the effective constituent of this product, in order to control the quality of drug combination preparation of the present invention, ensure its curative effect, the content assaying method that the present invention adopts carries out the assay of iron, and the content method of its iron is rationally more scientific, and data are more accurate.By content assaying method of the present invention, improve the accuracy of product specification product, cut the waste, reduce costs, be conducive to the quality control of suitability for industrialized production.
Experimental example and embodiment are used for further illustrating but are not limited to the present invention below
Experimental example 1: the contrast experiment of detection method of content and content method of the present invention in prior art: getting is that the sample of embodiment 1,2,3,4 carries out assay respectively.
Content assaying method one: the content assaying method conventionally carries out assay:
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, is diluted with water to scale, shake up, obtain reference substance solution (in every 1ml the ferrous 80ug of sulfur acid); Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry (Chinese Pharmacopoeia version in 2010 annex V A), absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, adds water to scale, shake up, precision measures 10ml, puts in 50ml measuring bottle, adds water to scale, shake up, precision measures 5ml, puts in 25ml measuring bottle, adds water to 10ml, then adds 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to quarter, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
Content assaying method two: carry out assay according to content assaying method of the present invention:
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
Result is as follows:
According to result, the measurement result that the sample iron content carried out with method two measures ratio method one is higher, and statistics uses t inspection, and compare with method one, method two has difference, P < 0.05.
(3) brief summary: use the assay that carries out of the present invention to be specification product, but the defect of content assaying method due to prior art, cause specification product and detect
mistake, cause the waste of product and the raising of cost, also cannot the quality of control product of science.
Embodiment 1:
Melanterite 5.3g, sea-buckthorn 200g, hawthorn 100g, date 100g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second time 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing; get Sodium Benzoate 2g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml; stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 49.23mg containing melanterite.
Embodiment 2:
Melanterite 5.3g, sea-buckthorn 200g, hawthorn 100g, date 100g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.56g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 48.56mg containing melanterite.
Embodiment 3:
Melanterite 5.3g, sea-buckthorn 200g, hawthorn 100g, date 100g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.3g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 49.15mg containing melanterite.
Embodiment 4
Melanterite 5.3g, sea-buckthorn 200g, hawthorn 100g, date 100g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.6g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 47.38mg containing melanterite.
Embodiment 5:
Melanterite 4g, sea-buckthorn 180g, hawthorn 90g, date 120g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second time 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing; get Sodium Benzoate 2g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml; stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 44.67mg containing melanterite.
Embodiment 6:
Melanterite 4g, sea-buckthorn 180g, hawthorn 90g, date 120g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.56g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 44.78mg containing melanterite.
Embodiment 7:
Melanterite 4g, sea-buckthorn 180g, hawthorn 90g, date 120g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.3g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 44.46mg containing melanterite.
Embodiment 8
Melanterite 6g, sea-buckthorn 210g, hawthorn 110g, date 100g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.6g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 45.06mg containing melanterite.
Embodiment 9:
Melanterite 6g, sea-buckthorn 210g, hawthorn 110g, date 100g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.3g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 51.23mg containing melanterite.
Embodiment 10
Melanterite 4g, sea-buckthorn 180g, hawthorn 90g, date 120g
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.6g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
Get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, add sulfuric acid solution (1 → 20) 1ml and water 80ml and make it dissolve, add water to scale, shake up, precision measures 2ml, puts in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
The every 10ml of this product in ferrous sulphate, is 50.89mg containing melanterite.
Claims (7)
1.
a kind of for postpartum ischemic, lochia the detection method of content of Chinese medicine compositionto it is characterized in that in the method containing, for example lower content assaying method: get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, adding sulfuric acid solution (1 → 20) 1ml and water 80ml makes it dissolve, add water to scale, shake up, precision measures 2ml, put in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 5 ~ 15ml, puts in 100ml measuring bottle, and instillation 0.5% ~ 5% sodium hydroxide solution is 3.0 ~ 5.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product;
In the method indication for postpartum ischemic, the bulk drug of Chinese medicine composition of lochia and proportioning be: melanterite 2 ~ 8 weight portion, sea-buckthorn 180 ~ 220 weight portion, hawthorn 80 ~ 120 weight portion, date 80 ~ 120 weight portion.
2. as claimed in claim 1
a kind of for postpartum ischemic, lochia the detection method of content of Chinese medicine compositionto it is characterized in that in the method containing, for example lower content assaying method: get ferrous sulphate reference substance 0.4g, accurately weighed, put in 100ml measuring bottle, adding sulfuric acid solution (1 → 20) 1ml and water 80ml makes it dissolve, add water to scale, shake up, precision measures 2ml, put in 100ml measuring bottle, be diluted with water to scale, shake up, obtain reference substance solution; Precision measures reference substance solution 1.0ml, 2.0ml, 4.0ml, 6.0ml, 8.0ml, puts respectively in 25ml measuring bottle, adds water to 10ml, add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine 1ml again, mixing, add water to scale, shake up, with corresponding solution for blank, according to UV-VIS spectrophotometry, absorbance is measured at 522nm wavelength place, take absorbance as ordinate, concentration is horizontal ordinate, drawing standard curve; Precision measures this product 10ml, puts in 100ml measuring bottle, and instillation 1% ~ 2% sodium hydroxide solution is 3.5 ~ 4.5 to PH, add water to scale, shake up, precision measures 5ml, put in 25ml measuring bottle, add water to 10ml, then add 1% hydroxylamine hydrochloride solution 1ml and 0.2%2,2-dipyridine ethanolic solution 1ml, mixing, adds water to scale, shake up, with corresponding solution for blank, measure absorbance, read the weight of ferrous sulphate in need testing solution from typical curve, calculate, to obtain final product.
3. the detection method of content of the Chinese medicine composition as described in as arbitrary in claim 1-2, it is characterized in that the bulk drug of the Chinese medicinal composition preparation of indication in the method consists of: melanterite 5.3 weight portion, sea-buckthorn 200 weight portion, hawthorn 100 weight portion, date 100 weight portion.
4. the detection method of content of the Chinese medicine composition as described in as arbitrary in claim 1-2, it is characterized in that in the method, the Chinese medicinal composition preparation of indication is made by the following method: get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, 10 times amount that add water for the first time decoct 1.5 hours, second is that 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, let cool, add ethanol and make alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.2 ~ 0.8g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
5. the detection method of content of the Chinese medicine composition as described in as arbitrary in claim 4, is characterized in that in the method, the Chinese medicinal composition preparation of indication is made by the following method:
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second time 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing, get NaOH 0.56g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml, stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
6. the detection method of content of the Chinese medicine composition as described in as arbitrary in claim 1-2, is characterized in that in the method, the Chinese medicinal composition preparation of indication is made by the following method:
Get sea-buckthorn, hawthorn, date three taste medicine boiling 2 times, first time 10 times amount that add water decoct 1.5 hours, second time 8 times amount that add water decoct 1 hour, collecting decoction, filter, filtrate is concentrated into every 1ml containing 1g crude drug, lets cool, adding ethanol makes alcohol content be 70%, stir, hold over night, leaching supernatant, filtrate recycling ethanol is to without alcohol taste, for subsequent use; Melanterite adds the sulfuric acid solution 50ml of 0.1%, stirs and makes it dissolve, and filter, filtrate adds vitamin C 5g, is stirred to dissolve, solution for standby; Get sucrose 200g, add suitable quantity of water, make simple syrup, filter, add above-mentioned two kinds of liquids, mixing; get Sodium Benzoate 2g, add in above-mentioned admixing medical solutions, stir evenly, regulate pH value to 2.5-4.0 with citric acid, be added to 1000ml; stir evenly, leave standstill, filter, filling, sterilizing, to obtain final product.
7. the detection method of content of the arbitrary described Chinese medicine composition of claim 1-2, is characterized in that: the every 10ml of this product in ferrous sulphate, must not be less than 45mg containing melanterite.
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| CN101077372A (en) * | 2007-03-07 | 2007-11-28 | 郑光明 | Chinese medicinal materials composition for preventing and treating iron-deficiency anemia and method of making the same |
| CN102309572A (en) * | 2010-07-02 | 2012-01-11 | 程雪翔 | Blood nourishing oral liquid and preparation method thereof |
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| CN101077372A (en) * | 2007-03-07 | 2007-11-28 | 郑光明 | Chinese medicinal materials composition for preventing and treating iron-deficiency anemia and method of making the same |
| CN102309572A (en) * | 2010-07-02 | 2012-01-11 | 程雪翔 | Blood nourishing oral liquid and preparation method thereof |
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| 国家食品药品监督管理局: "《国家药品标准 新药转正标准 第84册》", 31 December 2011 * |
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