CN1994426A - Preparation method and quality control method of 'Sheng Mai' soft capsule - Google Patents
Preparation method and quality control method of 'Sheng Mai' soft capsule Download PDFInfo
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Abstract
The invention relates to soft capsules for restoring pulse beat and the process for preparing the capsules, wherein the raw materials include red ginseng 250g, lilyturf root 500g, and schisandra fruit 250g. The invention also provides a method of thin layer discrimination for red ginseng and lilyturf root, as well as the method for measuring content of schizandrol A for controlling the inner quality of the preparation.
Description
Technical field
The present invention relates to the preparation method and the method for quality control thereof of 'Sheng Mai ' soft capsule.
Background technology
SHENGMAI YIN is the famous ancient prescription of traditional Chinese medical science supplementing QI and nourishing YIN, is made up of Radix Ginseng Rubra, Radix Ophiopogonis, Fructus Schisandrae Chinensis three herbal medicines.The function Yiqi and vein recovery, YIN nourishing and the production of body fluid promoting is used for QIYINLIANGXU, shortness of breath and palpitation, faint pulse spontaneous perspiration." SHENGMAI YIN " recorded in one one of Pharmacopoeia of the People's Republic of China version in 2005, and pharmacopeia over the years is all recorded, and is oral liquid.Modern clinical many application we treatment pulmonary heart diseases, cardiovascular disease etc. belong to deficiency of both vital energy and Yin person, have illness such as the chronic tracheitis of above-mentioned symptom, neurosis, functional low grade fever.
Theory of Chinese medical science thinks, we control card and are heresy damp and hot, summer-heat, consumption impairment of QI the moon, or the chronic cough deficiency of the lung, impairment of both QI and YIN and causing.Because of summer-heat being a kind of YANG pathogen, heat is steamed hyperhidrosis, and the easiest consumption impairment of QI Tianjin causes impairment of both QI and YIN, thus hyperhidrosis, Mental fatigue, body is tired, breathes hard dry pharynx, deficient pulse.Impairing the lung of a specified duration during cough, deficiency of both vital energy and Yin person, also visible above-mentioned sign.Control the method for should supplementing QI and nourishing YIN promoting the production of body fluid.The sweet temperature of Radix Ginseng Rubra in the side, supplementing QI for promoting the production of body fluid be with tonifying the lung, and the prosperous then four dirty gas of lung qi are all prosperous, are monarch drug.Radix Ophiopogonis is sweet cold, replenishing YIN and removing heat, and the lung moistening and production of body fluid promoting is ministerial drug.Radix Ginseng Rubra, Radix Ophiopogonis are share, and then the merit of supplementing QI and nourishing YIN benefit is clear.The trimethyl gallic acid temperature, the hidroschesis of astringing the lung, promoting the production of body fluid to quench thirst is adjuvant drug.Three medicines share.One mends one clear one holds back, and plays supplementing QI and nourishing YIN altogether, promoting the production of body fluid to quench thirst, the effect of astringing YIN to stop sweating.The multiple Tianjin of gas is given birth to, and perspiration stopped the moon is deposited, and arteries and veins is brought about the desired sensation and filled, but then demutation is allly demonstrate,proved to such an extent that remove.
Radix Ginseng Rubra treatment weak body and prostration in the side, faint pulse being about to disappear, extreme cold of the limbs, the anxious critical patient of sweating YANG-depletion has tangible strongly invigorating primordial QI, admittedly take off the effect of multiple arteries and veins.Modern pharmacological research shows: Radix Ginseng Rubra can be strengthened corticocerebral process of excitation, accelerate the conduction of neural impulse, shorten the incubation period of neural reflex, strengthen trained reflex, improve analysis ability, also can strengthen process of inhibition simultaneously, improve lability of nervous process, can improve sleep and emotion to the people, heavy dose also calmness can occur.Radix Ginseng Rubra has the effect of " adaptogen " sample, and the energy enhancing body is to the defence capability (influence to neural 2 hypophysis, 2 interrenal systems is relevant) of various destructive stimuluses.The ginsenoside has obvious anti-stress effect, can significantly suppress the important variation in stress of organs such as mice adrenal gland, thymus, thyroid.Radix Ginseng Rubra does not have gonadotropic Effect, but can secrete promoting sexual gland hormone by excited hypophysis, can promote man, women's gland function, and the energy blood sugar lowering have synergism with islets of langerhans, and the metabolism of energy cholesterol regulating suppresses the generation of hypercholesterolemia.Radix Ginseng Rubra energy hemopoietic organ makes hemopoietic function vigorous.Enhancing human body immunity power promotes immunoglobulin to generate, and prevents and treats the leukopenia that multiple reason causes, lymphocyte is increased, and makes lymphoblastic transformation, strengthens the reticuloendothelial system function.
Be the tuber on its plant fibrous root Radix Ophiopogonis in the side.Its cold nature, sweet in the mouth, little hardship are returned lung, the heart, stomach warp, belong to nourishing YIN class Chinese medicine, and adjustable lung yin nourishing, reinforcing stomach reg fluid, relieving restlessness clears away heart-fire.Contain multiple steroid saponin Radix Ophiopogonis.
Fructus Schisandrae Chinensis is the mature fruit of its plant in the side.Its sour in the mouth, sweet, warm in nature.GUIXIN, lung, kidney channel.This product acid can convergence, Gan Wen and moisten last can QI invigorating astringing the lung, following energy tonifying kidney and nourishing yin, supplementing QI for promoting the production of body fluid, the arresting sweating of bringing down a fever.The modern study Fructus Schisandrae Chinensis can strengthen central nervous system's excitement and process of inhibition, promote the mutual balance of two kinds of nervous process, can improve people's intellectual activity, regulate the cardiovascular system blood circulation, undesired blood pressure there is regulating action, rather remarkable to the circulatory failure person blood pressure effect that raises.Breathing is had excitation, and gastric secretion is regulated in cough-relieving, promotes bile secretion, regulates carbohydrate metabolism, reduces paddy 2 pyruvic transaminases, and hepatocyte is had protective effect.
The traditional Chinese medical science with Radix Ginseng Rubra, Radix Ophiopogonis, the compatible composition compound recipe of Fructus Schisandrae Chinensis, is brought into play the Chinese medicine stage construction in the clinical treatment medication in sum, and many target spots are at the intravital therapeutical effect of people.Three medicines share, and one mends, and one is clear, and one receives, and becomes supplementing QI and nourishing YIN altogether, promoting the production of body fluid to quench thirst, the merit of strengthening superficial resistance to stop perspiration.Simultaneously modern pharmacological research shows: SHENGMAI YIN has protective effect, SHENGMAI YIN to cardiac muscle and can obviously improve the T cell subsets and have immunoregulation effect, SHENGMAI YIN and have removing effect, the SHENGMAI YIN of hydroxy radical had growth promoter and learning and memory facilitation.
We are extensive in modern clinical practice, determined curative effect is mainly used in clinically: heart failure, dilated cardiomyopathy heart failure, old cerebral infarction, hypovolemic shock, silent ischemia, premature beat, in, severe neonatal scleredema, intractable ventricular premature contraction etc.
In a word, studies have shown that our determined curative effect through clinical practice for many years and modern pharmacology, safe in utilization.Be listed in subject in second batch of national nonprescription drugs medicine Chinese patent medicine, be widely used for treating myocardial infarction, angina pectoris, shock, hypotension, arrhythmia, pulmonary heart disease etc.Relevant documents and materials often have report, and constantly explore we's clinical application range, many new clinical application methods of deriving.
'Sheng Mai ' soft capsule develops according to " SHENGMAI YIN ", and has kept former side's effect.Medicine is wrapped in the capsule be isolated from the outside by making soft capsule, has reduced the influence of moisture, air, light, thereby improved stability; And soft capsule does not add excipient, minimizing drug administration amount; The influence that is not stressed disperses fast, good absorbing in gastrointestinal, rapid than pill, disintegration of tablet, the bioavailability height; The soft capsule exquisite appearance, cover bad smell, swallow easily, easily accepted by the patient.Clinical needs have been satisfied better.4/time of the each doses of 'Sheng Mai ' soft capsule after the change dosage form, 2 times/day, every intragranular is tolerant to be 0.6g.
Goal of the invention and summary of the invention
" 2005 editions one " SHENGMAI YIN " of recording of Chinese pharmacopoeia is an oral liquid, and the present invention is made into soft capsule by research.And formulated its method of quality control.
One, preparation of soft capsule
Through technology research, the preparation method of SHENGMAI YIN is:
Pharmacodynamic raw materials is formed: Radix Ginseng Rubra 250g, Radix Ophiopogonis 500g, Fructus Schisandrae Chinensis 250g.
Adjuvant is by vegetable oil: Cera Flava: the vegetable oil mixed-matrix that Arlacel-80 is formed in 18: 1: 1 ratios is an amount of, preferred 360g.
Preparation method: Radix Ginseng Rubra, Radix Ophiopogonis, Fructus Schisandrae Chinensis, be ground into coarse powder, use the 60%-70% ethanol percolation, the collection liquid of filtering reclaim ethanol to there not being the alcohol flavor, and concentrating under reduced pressure becomes clear paste, with the clear paste drying under reduced pressure, dried cream powder is broken into fine powder, crosses 100 mesh sieves, get dry powder, dry powder is added in the vegetable oil mixed-matrix, stir, grind more than three times with colloid mill, suppress in soft gelatin capsule, promptly.
The preferred for preparation method is: Radix Ginseng Rubra, Radix Ophiopogonis, Fructus Schisandrae Chinensis, be ground into coarse powder, make solvent with 65% ethanol, flood and carry out percolation after 24 hours, percolation speed is 2ml/min, the collection about 10L of liquid that filters reclaim ethanol to there not being the alcohol flavor, and concentrating under reduced pressure is that relative density is the clear paste of 1.35～1.40 (60 ℃), with clear paste in 50～60 ℃ of drying under reduced pressure, dried cream powder is broken into fine powder, crosses 100 mesh sieves, gets dry powder, dry powder is added in the vegetable oil mixed-matrix (vegetable oil: Cera Flava: Arlacel-80 is 18: 1: 1), stir, more than three times, suppress in soft gelatin capsule with the colloid mill mill.Conventional typing, dry, wash ball, make 1000, bottling promptly.
The research of preparation method technology condition
The investigation of 1.65% alcohol dipping time
According to production technology, utilized 65% alcohol dipping respectively 12,24,36 hours, handle and obtain clear paste, calculate the content of paste-forming rate and schisandrin respectively.The results are shown in Table 1.
The investigation of 65% alcohol dipping time of table 1
| Batch | Dip time (h) | Blank panel heavy (g) | Gross weight (g) | Clear paste heavy (g) | Paste-forming rate (%) | Schisandrin content (mg/g) |
| 1 2 3 | 12 24 36 | 93.2447 95.3560 90.2787 | 96.6589 99.0127 93.9361 | 3.4142 3.6567 3.6574 | 8.49 9.089 9.09 | 0.0361 0.0389 0.0387 |
The result shows: dip time is too short can not effectively to extract effective ingredient, and overlong time then extracts non-main action component easily.Therefore select 24 hours as best dip time.
2. the screening of percolation speed
The experiment of three batches of same amounts is carried out simultaneously.According to production technology, during percolation speed be respectively 1,2,3ml/min, collect the liquid of filtering, handle assay method with 1.Experimental result sees Table 2.
The screening of table 2 percolation speed
| Batch | Percolation speed (ml/min) | Blank panel heavy (g) | Gross weight (g) | Clear paste heavy (g) | Paste-forming rate (%) | Schisandrin content (mg/g) |
| 1 2 3 | 1 2 3 | 92.6473 91.5520 94.3215 | 96.8510 95.3517 97.9180 | 4.2037 3.7997 3.5965 | 10.51 9.50 8.99 | 0.038 0.039 0.039 |
The result shows: percolation speed is slow, the paste-forming rate height, but schisandrin content is on the low side.Percolation speed is fast, then can not fully extract, and when percolation speed is 2ml/min, can enhance productivity, and can fully extract again, therefore selects 2ml/min as percolation speed.
3. the selection of the liquid collected volume of filtering
The experiment of three batches of same amounts is carried out simultaneously.According to production technology, percolation speed 2ml/min collects long-pending 5,10,15 times (V/W) that are respectively material quantity of the liquid of filtering, and next step processing assay method is with 1.Experimental result sees Table 3.
The filter selection of liquid collected volume of table 3
| Batch | The liquid collected volume of filtering (ml) | Blank panel heavy (g) | Gross weight (g) | Clear paste heavy (g) | Paste-forming rate (%) | Schisandrin content (mg/g) |
| 1 2 3 | 5 10 15 | 91.2587 91.3940 90.5879 | 94.0796 95.2103 94.4915 | 2.82 3.82 3.90 | 7.05 9.55 9.76 | 0.041 0.040 0.039 |
The result shows: the big paste-forming rate height of the liquid collected volume of filtering, but schisandrin content is on the low side.Selecting collected volume is 10 times of volumes of feeding quantity, can guarantee paste-forming rate, can guarantee schisandrin content again.
4. preparations shaping technical study
4.1 prescription design
Prescription: give birth to arteries and veins xeraphium 40%
Adjuvant: vegetable oil 54%
Cera Flava 3%
Arlacel-80 3%
4.2 auxilliary amount consumption is selected
According to the galenic pharmacy requirement, the soft capsule multiselect disperse medium of vegetable oil as suspension, selecting suitable wetting agent and suspending agent to make content keep stablizing for a long time is the key of soft capsule preparation.Be down that supplementary product consumption is selected situation:
1. the Cera Flava usage ratio is determined
With 50ml tool plug test tube, in medicated powder, add vegetable oil, Cera Flava in following ratio, placed 6 hours, viewing test result is as follows:
Vegetable oil Cera Flava result (suspending situation)
90% 2% better
5% is good
7% is bad
Can determine that by The above results the Cera Flava consumption is 5%.
2. the Arlacel-80 usage ratio is determined
With 50ml tool plug test tube, in medicated powder, add vegetable oil, Arlacel-80 in following ratio, placed 6 hours, viewing test result is as follows:
Vegetable oil Arlacel-80 result (hydrotropy situation)
90% 2% better
5% is good
7% is good
By the result as can be known the Arlacel-80 consumption be 7% and 5% o'clock result of the test unanimity, we select the Arlacel-80 consumption is 5%, so promptly can play Action of Surfactant, its content proportion of Arlacel-80 is few.
Can determine that by above-mentioned result of the test the optimal proportion of vegetable oil, Cera Flava, Arlacel-80 is 18: 1: 1
3. medicated powder and substrate ratio are determined: select different proportion substrate for use, the medicated powder situation that sees drying and disintegrate situation
Table 4 supplementary product consumption selection result
| Numbering | Medicated powder: vegetable oil mixed-matrix | Dry medicated powder situation | The disintegrate situation |
| 1 | 1∶2 | Good fluidity | Up to specification |
| 2 | 1∶1.5 | Good fluidity | Up to specification |
| 3 | 1∶1 | Bad | Up to specification |
Medicated powder and substrate ratio are that 1: 1.5 situation is best as can be known by table 4 result.
5. rate of transform test
The main effective ingredient schisandrin content of the used Fructus Schisandrae Chinensis of test agent is 0.409% in three batches, schisandrin content is respectively 0.57mg/ grain, 0.56mg/ grain, 0.57mg/ grain in the preparation, and the rate of transform of schisandrin is respectively 57.0%, 56.0%, 57.0%.
6. day is obeyed Rapid Dose Calculation
According to former dosage form day clothes dosage, changing the capsule taking dose into is each 4,2 times on the one, and every 0.6 gram.Every to contain the decoction pieces dose identical with former dosage form.
7. pilot scale research
| Technical parameter | Lot number 050501 | Lot number 050502 | Lot number 050503 |
| About material inventory (KG) | 10 | 10 | 10 |
| Dry powder heavy (kg) | 2.40 | 2.39 | 2.42 |
| Adjuvant amount (KG) | 3.6 | 3.6 | 3.6 |
| Capsule grain (individual) | 9700 | 9800 | 9800 |
| Packing Unit | 97 | 98 | 98 |
| Schisandrin content (mg/ grain) | 0.57 | 0.56 | 0.57 |
Two, the formulation of 'Sheng Mai ' soft capsule method of quality control
This product content 4g is got in [discriminating] (1), adds methanol 20ml, supersound process 20 minutes, filter, the filtrate evaporate to dryness adds water 20ml and makes dissolving, with ether extraction 3 times, each 20ml discards ether liquid, aqueous solution adds water saturated n-butanol extraction 2 times, and each 20ml merges n-butyl alcohol liquid, add ammonia solution washing 2 times, each 20ml discards ammoniacal liquor, the saturated water washing of reuse n-butyl alcohol 2 times, each 20ml discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue add water 5ml makes dissolving, by HPD100 macroporous resin (internal diameter 1cm, high 8cm), earlier use the 50ml water elution, discard water liquid, continue with 50ml 20% ethanol elution, discard pure liquid, reuse 50ml 70% ethanol elution is collected eluent, evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the ginsenoside Rg
1, Rb
1Add methanol and make the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw test sample 6 μ l, each 2 μ l of reference substance solution, point (into strips) is on same silica gel g thin-layer plate (Merck precoated plate) respectively, (15: 40: 22: 10) lower floor's solution of placing below 10 ℃ was developing solvent, and presaturation launched 9cm after 15 minutes with chloroform-ethyl acetate-methanol-water, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing in 105 ℃.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(2) get this product content 2g, add water 20ml, supersound process 20 minutes, centrifugal (2000 rev/mins), inclining supernatant, uses ether extraction 3 times, each 20ml discards ether solution, and water layer low temperature is flung to ether, add hydrochloric acid 2ml, reflux 1 hour is put cold, add diethyl ether and extract 2 times, each 20ml merges ether solution, low temperature evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution.Other gets control medicinal material powder Radix Ophiopogonis (80 order) 2g, adds 65% ethanol 20ml, and reflux 1 hour is put coldly, centrifugal, and inclining supernatant, steams to there not being the alcohol flavor, adds water 20ml and makes dissolving, adds hydrochloric acid 2ml, shines medical material chloroformic solution 2ml in pairs with legal system.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw test sample, each 2 μ l of reference substance medical material solution, put respectively on same silica gel g thin-layer plate, with petroleum ether (60～90 ℃)-ethyl acetate-formic acid (7: 3: 0.2) is developing solvent, and presaturation launched 9cm after 15 minutes, take out, dry, the spray with 5% phosphomolybdic acid ethanol solution, be heated to speckle by Huang become slightly black-and-blue till.In the test sample chromatograph, with the corresponding position of reference substance medical material chromatograph on, show the speckle of same color.
[assay] measured according to high performance liquid chromatography (appendix VID of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (62: 38) is a mobile phase; The detection wavelength is 254nm.Number of theoretical plate calculates by the schisandrin peak should be not less than 2000.
The preparation precision of reference substance solution takes by weighing schisandrin reference substance 2mg, puts in the 25ml measuring bottle, uses dissolve with methanol, and is diluted to scale, shake up, precision is measured above-mentioned solution 5ml, puts in the 10ml measuring bottle, add methanol and be diluted to scale, shake up, promptly get (every 1ml contains schisandrin 40 μ g).
10 of soft capsules are got in the preparation of need testing solution, extrude content, stir evenly, precision takes by weighing 0.25g, adds methanol 20ml, claims to decide weight, supersound process 20 minutes is put coldly, weighs, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, and evaporate to dryness, residue add water 20ml makes dissolving, with ether extraction 4 times, each 20ml merges ether solution, and decompression (60 ℃) is recycled to dried, residue adds methanol makes dissolving, be transferred in the 10ml measuring bottle, and be diluted to scale, shake up, filter with microporous filter membrane (0.5 μ m), promptly.
Accurate respectively reference substance solution and each the 20 μ l of need testing solution of drawing of assay method inject chromatograph of liquid, measure, promptly.
Every of this product contains Fructus Schisandrae Chinensis with schisandrin (C
24H
32O
7) meter, must not be less than 0.6mg.
Claims (4)
1. the preparation method of 'Sheng Mai ' soft capsule is characterized in that may further comprise the steps:
The ratio of 500g, Fructus Schisandrae Chinensis 250g is got raw material in Radix Ginseng Rubra 250g, Radix Ophiopogonis, is ground into coarse powder, uses the 60%-70% ethanol percolation, the collection liquid of filtering reclaim ethanol to there not being the alcohol flavor, and concentrating under reduced pressure becomes clear paste, with the clear paste drying under reduced pressure, dried cream powder is broken into fine powder, crosses 100 mesh sieves, get dry powder, dry powder is added by vegetable oil: Cera Flava: in the vegetable oil mixed-matrix that Arlacel-80 is formed by 18: 1: 1 ratios, stir, grind more than three times with colloid mill, suppress in soft gelatin capsule, promptly.
2. preparation method according to claim 1, it is characterized in that Radix Ginseng Rubra, Radix Ophiopogonis, Fructus Schisandrae Chinensis powder are broken into coarse powder, make solvent with 65% ethanol, flood and carry out percolation after 24 hours, percolation speed is 2ml/min, collects the about 10L of liquid that filters, and reclaims ethanol to there not being the alcohol flavor, and concentrating under reduced pressure is that 60 ℃ of heat survey relative densities are 1.35～1.40 clear paste, in 50～60 ℃ of drying under reduced pressure, dried cream powder is broken into fine powder with clear paste, crosses 100 mesh sieves, get dry powder, dry powder is added in the vegetable oil mixed-matrix, stir, grind more than three times with colloid mill, suppress in soft gelatin capsule, promptly.
3. identify the method for certain constituents in the compositions that contains Radix Ginseng Rubra, Radix Ophiopogonis, Fructus Schisandrae Chinensis, comprise following at least one:
(1) gets this product content 4g, add methanol 20ml, supersound process 20 minutes, filter, the filtrate evaporate to dryness adds water 20ml and makes dissolving, with ether extraction 3 times, each 20ml discards ether liquid, aqueous solution adds water saturated n-butanol extraction 2 times, and each 20ml merges n-butyl alcohol liquid, add ammonia solution washing 2 times, each 20ml discards ammoniacal liquor, the saturated water washing of reuse n-butyl alcohol 2 times, each 20ml discards water liquid, n-butyl alcohol liquid evaporate to dryness, residue adds water 5ml makes dissolving, by the HPD100 macroporous resin, uses earlier the 50ml water elution, discard water liquid, continue and use the 50ml20% ethanol elution, discard pure liquid, reuse 50ml70% ethanol elution, collect eluent, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution; Other gets the ginsenoside Rg
1, Rb
1Add methanol and make the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin layer chromatography, draw each 2 μ l of test sample 6 μ l reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-ethyl acetate-methanol-water by 15: 40: 22: the mixed liquor that 10 volume ratios are formed is developing solvent placing lower floor's solution that layering forms below 10 ℃, and presaturation launched 9cm after 15 minutes, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing in 105 ℃; Relatively in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, whether show the speckle of same color;
(2) get this product content 2g, add water 20ml, supersound process 20 minutes, centrifugal, inclining supernatant, uses ether extraction 3 times, each 20ml discards ether solution, and water layer low temperature is flung to ether, add hydrochloric acid 2ml, reflux 1 hour is put cold, add diethyl ether and extract 2 times, each 20ml merges ether solution, low temperature evaporate to dryness, residue add chloroform 2ml makes dissolving, as need testing solution; Other gets control medicinal material powder 2g Radix Ophiopogonis, adds 65% ethanol 20ml, and reflux 1 hour is put coldly, centrifugal, and inclining supernatant, steams to there not being the alcohol flavor, adds water 20ml and makes dissolving, adds hydrochloric acid 2ml, shines medical material chloroformic solution 2ml in pairs with legal system; Test according to thin layer chromatography, draw test sample, each 2 μ l of reference substance medical material solution, put respectively on same silica gel g thin-layer plate, be that the mixed liquor that petroleum ether-ethyl acetate-formic acid of 60～90 ℃ is formed by 7: 3: 0.2 volume ratios is developing solvent with boiling point, presaturation launched 9cm after 15 minutes, take out, dry, the spray with 5% phosphomolybdic acid ethanol solution, be heated to speckle by Huang become slightly black-and-blue till; Relatively in the test sample chromatograph, with the corresponding position of reference substance medical material chromatograph on whether show the speckle of same color.
4. measure the method for schisandrin content in the compositions that contains Radix Ginseng Rubra, Radix Ophiopogonis, Fructus Schisandrae Chinensis, it is characterized in that adopting high performance liquid chromatography, assay method is:
With octadecylsilane chemically bonded silica is filler; Methanol-water is a mobile phase by the mixed liquor of 62: 38 volume ratio compositions; The detection wavelength is 254nm, and number of theoretical plate calculates by the schisandrin peak should be not less than 2000;
Methanol solution with the schisandrin reference substance is a reference substance solution, and every 1ml contains schisandrin 40 μ g;
The preparation of need testing solution: get 10 of soft capsules, extrude content, stir evenly, precision takes by weighing 0.25g, adds methanol 20ml, claims to decide weight, supersound process 20 minutes is put coldly, weighs, supply the weight that subtracts mistake with methanol, shake up, filter, precision is measured subsequent filtrate 10ml, and evaporate to dryness, residue add water 20ml makes dissolving, with ether extraction 4 times, each 20ml merges ether solution, and reclaim under reduced pressure is to doing, residue adds methanol makes dissolving, be transferred in the 10ml measuring bottle, and be diluted to scale, shake up, filter with 0.5 μ m microporous filter membrane, promptly;
Algoscopy: accurate respectively reference substance solution and each 20 μ l of need testing solution of drawing, inject chromatograph of liquid, measure, promptly.
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| CN101745009B (en) * | 2008-12-05 | 2013-01-02 | 天津天士力之骄药业有限公司 | Method for extracting ginseng, dwarf lilyturf tuber and schisandra chinensis and preparation thereof |
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| CN101745009B (en) * | 2008-12-05 | 2013-01-02 | 天津天士力之骄药业有限公司 | Method for extracting ginseng, dwarf lilyturf tuber and schisandra chinensis and preparation thereof |
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Assignee: Beijing Handian Pharmaceutical Co., Ltd. Assignor: Handian Chinese-Western Medicine Research and Development Center, Beijing Contract record no.: 2010990000895 Denomination of invention: Preparation method, and identification and assaying method of 'Sheng Mai' soft capsule Granted publication date: 20100623 License type: Exclusive License Open date: 20070711 Record date: 20101110 |