CN1857381A - Quality control method for flatstem milkvetch seed preparation - Google Patents
Quality control method for flatstem milkvetch seed preparation Download PDFInfo
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Abstract
The present invention relates to quality control method for flatstem milkvetch seed preparation. The method includes thin-layer chromatography for identification and spectrophotograhy for content measurement. The method has high precision, high sensitivity and high stability to ensure the quality safety, homogeneity, stability, effectiveness and controllability.
Description
Technical field:
The present invention relates to a kind of method of quality control of Chinese medicine preparation, particularly the method for quality control of flatstem milkvetch seed preparation.
Background technology:
Flatstem milkvetch seed preparation is to be extracted by the Chinese medicine Semen Astragali Complanati to be processed into, and the dosage form of having gone on the market has granule.
The Semen Astragali Complanati granule records in the 12 the 71st page in the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation.Its function cures mainly and is invigorating the liver and kidney, controlling nocturnal emission with astringent drugs, and reducing urination makes eye bright.Be used for lumbago due to renal deficiency, seminal emission premature ejaculation, nebulousurine leukorrhagia, dribbling urination, dizzy blurred vision.
Semen Astragali Complanati mainly contains aminoacid, polypeptide, protein, phenols, tannin, sterol and triterpenes components, and alkaloid, flavones ingredient with obvious physiologically active.
Semen Astragali Complanati has following health-care effect:
1, benefit essence, controlling nocturnal emission with astringent drugs, arresting seminal emission
The successive dynasties book on Chinese herbal medicine has been recorded and narrated these effects of Semen Astragali Complanati more, " all families of solar corona book on Chinese herbal medicine " controls " letting out essence, hematuria ", " book on Chinese herbal medicine covers bamboo fish trap " ended man's incontinence of urine and let out essence, Compendium of Material Medica is controlled lumbago, is let out essence, " Bencao Congxin " cloud: " benefit is smart ", essentials of Matea Medica cloud: " benefit is smart ", " Leng Lu Yi Hua (Deserted House Medical Talks) " cloud: the compatibility Stamen Nelumbinis, medicines such as Air Bladder pseudosciaenae seu Acipenser glue are controlled the spermatorrhea of suffering from a deficiency of the kidney." herbal classic is met former " cloud: this product " for letting out smart asthenia key medicine, can controlling nocturnal emission with astringent drugs ", " Gu Shi cures mirror " cloud: this product " reinforcing YIN-essence controlling nocturnal emission with astringent drugs, the special the kidney invigorating of merit." the smart and random sun of Semen Astragali Complanati benefit, YANG invigorating and not random body.
2, the application on water channel
How to treat bed-wetting clinically with this product." all families of solar corona book on Chinese herbal medicine " cloud " it is dirty cold to treat water, and urine is many, only loses drop ...." " book on Chinese herbal medicine converges and says " cloud: " double only urine is lost drop, " ... " must join book on Chinese herbal medicine " cloud: " letting out of the water that reinforces the kidney warmed up the essence of lacking sun ..." " can medicine doctor mirror " this product " only losing drop, hematuria, urine reducing, " " it is former that book on Chinese herbal medicine is asked " speech " frequent micturition, incontinence of urine ... " successive dynasties book on Chinese herbal medicine speech Semen Astragali Complanati the kidney invigorating and solid urine, be credible and consolidate what treat incontinence of urine.
3, make eye bright
Supplement to Thousand Golden Prescriptions cloud: " make eye bright and make light of one's life by commiting suicide." " book on Chinese herbal medicine covers bamboo fish trap " cloud: " making light of one's life by commiting suicide, it is long-living to make eye bright ", " book on Chinese herbal medicine converges and says " said: " can nourishing the liver to improve visual acuity." " " book on Chinese herbal medicine is taken advantage of refined partly brave " and " herbal secret record " and " herbal readability " " state-promulgated pharmacopoeia " or the like all illustrate energy ' making eye bright '.The Dali, Shaanxi is among the people also to be said, and " Semen Astragali Complanati brews up and can make eye bright.”
4, the kidney invigorating
Herbal for Relief of Famines cloud: be " kidney-reinforcing drug " that the Compendium of Material Medica cloud: " the kidney invigorating is used more." " book on Chinese herbal medicine secret green " say: " invigorating the liver and kidney "." herbal readability " " kidney-reinforcing drug is used it more." also have essentials of Matea Medica " herbal classic is met former " " Bencao Congxin " " book on Chinese herbal medicine is high former " etc. all to use it with kidney-reinforcing drug.The function kidney-supplementing liver-boosting of this and Semen Astragali Complanati is inseparable in a word.
5, control dizziness
Carry according to the Pharmacopoeia of the People's Republic of China, " this product is used for ... dizzy blurred vision ... " Semen Astragali Complanati is applicable to the blurred vision due to the deficiency of the liver and kindey, and just senile disease such as drop is caused dizzy for treatment lumbago due to renal deficiency blurred vision, and special ground is also arranged, the Semen Astragali Complanati curative effect is wider, is medicine likely.
The pharmacological toxicology of Semen Astragali Complanati is as follows:
1, toxicity
The phase toxicity test, the hemogram of each dosage group rat, liver function, kidney merit laboratory values and matched group compare as a result, all in normal range; The heart, liver, spleen, lung, kidney are not seen obvious pathological change.
2, to hemorheological influence
Irritate stomach and give experimental hyperlipidemia rat 30g/kg the semen astragali complanati general flavone of crude drug, the hemorheology blood index of the rat of medication group as a result, whole blood contrast viscosity and whole blood reduction degree significantly descend, packed cell volume raises, erythrocyte sedimentation rate slows down, erythrocyte electrophoretic time is accelerated, with the moulding matched group than p＜0.01.It is relevant with erythrocytic surface charge and deformability to infer that semen astragali complanati general flavone changes hemorheology index.
3, to the influence of blood pressure and cerebral blood flow
Vein gives anesthetized dog Semen Astragali Complanati water decoction-alcohol sedimentation agent 0.125, and 0.250g/kg, blood pressure promptly begin to descend, and gives low dose of 3～5min.Blood pressure and cardiac muscular tension index significantly descend (P＜0.05, P＜0.01), decreased heart rate, and cerebral blood flow significantly increases (P＜0.05) during 1min, and blood pressure drops continues 30min.Vein gives anesthetized rat Semen Astragali Complanati 0.1, and 0.2g/kg, blood pressure and cardiac muscular tension index significantly descend (P＜0.01), and the blood pressure drops persistent period then is respectively 20min and 30min.
4, analgesic, analgesia, calm, cold-resistant, antifatigue effect
Find that by hot plate method, writhing method test the Semen Astragali Complanati water decoction can prolong the mice pain response latency significantly, the 10g/kg Semen Astragali Complanati reduces the mouse writhing reaction times that causes because of chemical stimulation significantly.Analgesic experimental observation does not have obvious influence to Semen Astragali Complanati to the body temperature of normal mouse, and the 20g/kg Semen Astragali Complanati can reduce the body temperature of heating mice; In addition, Semen Astragali Complanati can significantly reduce the body temperature of fever in rabbit.Calm test shows: 40g/kg Semen Astragali Complanati and thiopentone have obvious synergism, but the 20g/kg Semen Astragali Complanati can significantly improve the spontaneous activity in mice ability.To put into ice chest (10 ℃) after the mice administration, observe 24h, Semen Astragali Complanati 10g/kg can obviously improve the tolerance to cold (P＜0.01) of mice as a result.Irritate stomach and give mice Semen Astragali Complanati water decoction continuous 12d, in 28 ℃ of water-baths, make swimming test, 10g/kg as a result, but the equal significant prolongation mice swimming time (P＜0.05, P＜0.01) of 20g/kg Semen Astragali Complanati.The 10g/kg Semen Astragali Complanati can obviously increase the mice body weight in addition.
5, antiinflammatory action
Filling stomaches such as Zhou Peifang give rat with Semen Astragali Complanati 100% water decoction-alcohol sedimentation agent 20,30g/kg, can significantly suppress the generation (P＜0.05, P＜0.01) of formaldehyde swollen joint.
6, anticancer growth
In vitro tests has inhibitory action to tumor cell.Semen Astragali Complanati contains more bioflavonoids and has anticancer and antimutagenic effect, can suppress the formation of tumor.
7, effect for reducing fat
For hyperlipidemia rats due to the feed material, the semen astragali complanati general flavone that is equivalent to crude drug 30g/kg dosage has significant effect for reducing blood fat, can make higher cholesterol, triglyceride and low-density lipoprotein cholesterol significantly reduce (P＜0.01), and can make HDL-C meter height (P＜0.05).
8, anticoagulant effect
Find that with the Born optical densitometric method semen astragali complanati general flavone when final concentration 1.25,2.5 and the 5mg/mL, all can suppress the platelet aggregation (P＜0.01, P＜0.05) that ADP and collagen cause significantly.
9, hepatoprotective effect
The flavonoid position of Semen Astragali Complanati decoct and extraction, water soluble part, total amino acids position are to normal mouse and carbon tetrachloride (CCl
4) the hepatic injury rat irritates stomach respectively, the decoct energy of 5g/kg significantly reduces liver glycogen (P＜0.01), triglyceride (P＜0.01) regulating liver-QI total protein (P＜0.01), also can make CCl
4Sterin content significantly descend (P＜0.05) in hepatic injury rat SGPT and the liver.
10, to Immune Effects
Semen Astragali Complanati decoct 5g/kg or 10g/kg gavage, can significantly improve the vigor of mouse boosting cell or serum lysozyme, obviously promote normal and phytohaemagglutinin (PHA) to stimulate mouse spleen down, but do not influence the picked-up of thymus, do not increase spleen weight 3H-TdR to the mixing of 3H-TdR.
11, anti-aging effects
136 of secondary Kunming female mices fall in Xiao Aizhen etc., and body weight 18～22g is divided into Semen Astragali Complanati group, compound recipe Semen Astragali Complanati group, normal saline matched group, aging model group by random table.Semen Astragali Complanati group, compound recipe Semen Astragali Complanati group are irritated stomach with Semen Astragali Complanati, compound recipe Semen Astragali Complanati water decoction 015ml respectively, and (the sub-water decoction in garden contains crude drug amount 200mg/ml; The compound recipe Semen Astragali Complanati is extracted by water cooking liquids such as Semen Astragali Complanati, Formica fusca, Radix Rhodiolae, Radix Schisandrae Bicoloris, Fructus Lycii, Radix Ophiopogonis, Rhizoma Chuanxiongs to be formed, and contains crude drug amount 400mg/ml), every day 1 time; Normal saline matched group and aging model group are irritated stomach with the normal saline of equivalent.Medication 28d surveys whole blood malonaldehyde, superoxide dismutase, glutathione peroxidase content, interleukin 1,6,8 levels and mice body weight change.Result: Yuan Zineng obviously reduces malonaldehyde MDA and improves superoxide dismutase SOD, glutathione peroxidase (GSH-Px) activity, compare with the aging model group, difference has significance meaning (P＜0.05) medication group and aging model group relatively, interleukin 1 and 8 levels raise, and have statistical significance (P＜0.05); Interleukin-6 has trend of rising, but no difference of science of statistics; Each mice body weight does not have significant difference.
Existing flatstem milkvetch seed preparation exists method of quality control to fall behind the uppity shortcoming of product quality.Its composition is not differentiated in the existing method of quality control, or its composition is carried out the content of assay.So existing method of quality control can not effectively be controlled the quality of flatstem milkvetch seed preparation, thereby will influence the production of product and ensure the quality of products.
For effectively controlling product quality, we have set up the new method of quality control of flatstem milkvetch seed preparation, and this method adopts thin layer chromatography to differentiate, adopt spectrophotography to carry out assay.This method of quality control precision, sensitivity, stability are all good, guarantee " safety, the homogeneous, stable, effective, controlled " of product quality.
Summary of the invention:
The object of the invention is to provide the method for quality control of flatstem milkvetch seed preparation.
The flatstem milkvetch seed preparation prescription consists of:
Semen Astragali Complanati (salt is processed) 500g
Semen Astragali Complanati oral liquid method for making is as follows: get Semen Astragali Complanati (salt is processed) 500 grams, add water and extract secondary, 1.5 hours first time, 1 hour for the second time in 80 ℃.Merge extractive liquid, filters, and filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (80～85 ℃ of heat are surveyed), add ethanol and make and contain alcohol amount and reach 60%, stir evenly, left standstill 12 hours, filter, filtrate recycling ethanol adds correctives, antiseptic is an amount of, adding water makes and makes 1000ml, mixing, embedding, sterilization, promptly.
The present invention be directed to the Semen Astragali Complanati oral liquid formulations and propose method of quality control, but also be not limited to the Semen Astragali Complanati oral liquid formulations, also can comprise other oral formulations of Semen Astragali Complanati such as tablet, capsule, syrup, granule.
Its prescription of other dosage forms of the Semen Astragali Complanati that the present invention includes is identical with the Semen Astragali Complanati oral liquid formulations, and composition is by weight as proportioning, can increase or reduce according to corresponding proportion when producing, and be no more than 100% at most, as Semen Astragali Complanati (salt is processed) 250-1000g.
Large-scale production can be unit with the kilogram, or is unit with the ton.More than composition can be made into 1000 doses of pharmaceutical preparatioies, described 1000 doses of fingers, and the final drug preparation of making, as make 1000 of capsule preparations, and 1000 in tablet, granule 1000g, liquid preparation 1000ml etc.,
The preparation method of other dosage forms of Semen Astragali Complanati of the present invention can adopt following method:
By the raw material of Chinese medicine of above-mentioned prescription is processed through extraction or other modes, making pharmaceutically active substance, subsequently, is raw material with this material, add the medicine acceptable carrier when needing, make capsule, tablet, syrup, granule according to the routine techniques of galenic pharmacy.Described active substance can obtain by the method that is selected from following mode, as: by pulverize, squeeze, calcine, grind, sieve, percolation, extraction, water are carried, alcohol extraction, ester are carried, methods such as ketone is carried, chromatography obtain, these active substances can be the materials of extractum form, can be that dry extract also can be a fluid extract, can also be the high-purity extract, make different concentration according to the different needs decision of preparation.
Other dosage forms of Semen Astragali Complanati of the present invention, when making preparation, can add the medicine acceptable carrier as required, these carriers can be any carriers that is fit to make preparation of the present invention, as: benzoic acid or potassium salt, mannitol, sorbitol, sorbic acid or potassium salt, xylitol, maltose, glucose, fructose, dextran, glycine, starch, sucrose, lactose, mannitol, Nepal's methyl ester, Nepal's ethyl ester, Nepal's propyl ester, Nepal's butyl ester, sodium pyrosulfite, sodium sulfite, sodium thiosulfate, cysteine hydrochloride, TGA, methionine, vitamin A, vitamin C, vitamin E, vitamin D, azone, the EDTA disodium, EDTA calcium sodium, the alkali-metal carbonate of monovalence, acetate, phosphate or its aqueous solution, hydrochloric acid, acetic acid, sulphuric acid, phosphoric acid, aminoacid, sodium chloride, potassium chloride, sodium lactate, silicon derivative, cellulose and derivant thereof, alginate, gelatin, polyvinylpyrrolidone, glycerol, propylene glycol, ethanol, soil temperature 60-80, Arlacel-80, Cera Flava, lanoline, liquid paraffin, hexadecanol, gallate ester, agar, triethanolamine, basic amino acid, carbamide, allantoin, surfactant, Polyethylene Glycol, cyclodextrin, beta-schardinger dextrin-, phospholipid material etc.
Flatstem milkvetch seed preparation of the present invention, particularly oral liquid formulations, it is as follows that its function cures mainly usage and dosage:
[function with cure mainly] temperature compensation Liver and kidney, controlling nocturnal emission with astringent drugs, reducing urination makes eye bright.Be used for lumbago due to renal deficiency, seminal emission premature ejaculation, nebulousurine leukorrhagia, dribbling urination, dizzy blurred vision.
[usage and consumption] is oral, one time 1 bottle, 2 times on the one.
[specification] every bottled 10 milliliters
[storage] is airtight.
[effect duration] 2 years
The present invention is to provide the method for quality control at above flatstem milkvetch seed preparation, particularly oral liquid formulations, be the quality of control flatstem milkvetch seed preparation.At its characteristics and prescription of the present invention, we provide following method of quality control:
Method of quality control of the present invention may further comprise the steps:
The observation of character, the discriminating of content, the inspection of content is carried out assay to the composition that contains, and therefore, the main step of method of quality control of the present invention is:
The observation of character, step is:
[character] this product is that pale brown color is to brown liquid; It is sweet to distinguish the flavor of, little hardship.
The discriminating of content, step is:
This product 0.5ml is got in [discriminating] (1), adds water 2ml, adds 4～5 of hydrochloric acid, and a small amount of magnesium powder, and it is hot slightly to put water-bath, promptly shows red.
(2) preparation of need testing solution: get this product, as need testing solution.Other gets Semen Astragali Complanati control medicinal material 1.0g, puts in the apparatus,Soxhlet's, adds an amount of reflux 4h of petroleum ether, and medicinal residues volatilize solvent, adds 80% ethanol 20ml, and reflux 1.5h is put coldly, filters, and filtrate is medical material solution in contrast.Test according to thin layer chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, with methanol-water (4: 1) is developing solvent, launches, and takes out, dry, spray is with 1% aluminum chloride alcoholic solution, and the heating colour developing is put under the ultra-violet lamp (365nm) and inspected.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The inspection of content, step is:
[inspection] pH value should be 4.5～6.5 (an appendix VII of Chinese Pharmacopoeia version in 2005 G).
Other should meet every regulation relevant under the mixture item (an appendix I of Chinese Pharmacopoeia version in 2005 J).The composition that contains is carried out assay, and step is:
The preparation precision of [assay] reference substance solution takes by weighing the control substance of Rutin 25.0mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 50ml measuring bottle, and it is an amount of to add methanol, and slight fever makes dissolving, and the back that cools is diluted to scale with methanol, shakes up, promptly.
The preparation precision of standard curve is measured reference substance solution 0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0ml, puts respectively in the 50ml measuring bottle, adds 10%AlCl
3Solution 1ml adds water to scale, shakes up, placed 15 minutes, and be blank with corresponding solution.According to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2005 B), measure trap at 415nm wavelength place, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
The algoscopy precision is measured this product 1ml, puts in the 100ml measuring bottle, and the method under the preparation of sighting target directrix curve is from " adding 10%AlCl
3Solution 1ml " rise, measure trap in accordance with the law, read the weight of rutin the need testing solution from standard curve, calculate, promptly.
This product contains total flavones with rutin (C for every bottle
27H
30O
16) meter, must not be less than 4.8mg.
In order effectively to control the quality of the medical material that feeds intake, the present invention also comprises the method for inspection of Semen Astragali Complanati (salt is processed) medical material, and step is as follows:
The preparation precision of [assay] reference substance solution takes by weighing the control substance of Rutin 25.0mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 50ml volumetric flask, and it is an amount of to add methanol, and slight fever makes dissolving, and the back that cools is diluted to scale with methanol, shakes up, promptly.
The preparation precision of standard curve is measured reference substance solution 0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0ml, puts respectively in the 50ml measuring bottle, adds 10%AlCl
3Solution 1ml adds water to scale, shakes up, placed 15 minutes, and be blank with corresponding solution.According to spectrophotography (appendix V B), measure trap at 415nm wavelength place, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
Algoscopy takes by weighing the about 2.0g of Semen Astragali Complanati (salt is processed) powder (crossing 20 mesh sieves), and accurate the title decides, and puts in the apparatus,Soxhlet's, add an amount of reflux 4h of petroleum ether, medicinal residues volatilize solvent, accurately add 80% ethanol 60ml, weigh,, take out and put cold weighing in 85 ℃ of reflux 1.5h of water-bath, replenish 80% ethanol to former weight, mixing is placed, the accurate supernatant 1ml that draws, put in the 25ml measuring bottle, the method under the preparation of sighting target directrix curve is from " adding 10%AlCl
3Solution 1ml " rise, measure trap in accordance with the law, read the weight of rutin the need testing solution from standard curve, calculate, promptly.
This product contains total flavones by rutin (C
27H
30O
16) must not count and be less than 0.4%.
Instrument and reagent
Ultraviolet-uisible spectrophotometer: Perkin Elmer instruments Lambda 25UV/VISspectrometer
Sample: 10 10 batches of Semen Astragali Complanatis in the place of production (salt is processed) medical material
Reference substance: rutin: available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, assay usefulness, lot number: the making of 0080-9705 rutin standard curve
The preparation of standard solution: get 120 ℃ of drying under reduced pressure to the about 25.0mg of the control substance of Rutin of constant weight, the accurate title, decide.Put in the 50ml measuring bottle, it is an amount of to add methanol, and slight fever makes dissolving, and the back that cools is diluted to scale with methanol, shakes up, and precision is measured 0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0ml, puts respectively in the 50ml measuring bottle, adds 10%AlCl
3Solution 1ml adds water to scale, shakes up, placed 15 minutes, and be blank with corresponding solution.According to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2005 B), measure trap at 415nm wavelength place, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
Measurement result is as follows:
Table 1 reference substance concentration and trap
| Concentration (μ g/ml) | 0.000 | 5.072 | 10.144 | 15.216 | 20.288 | 25.360 | 30.432 |
| Trap (A) | 0.0000 | 0.1721 | 0.3404 | 0.5035 | 0.6590 | 0.8175 | 0.9626 |
Regression equation: Y=0.0317X+0.0117
Correlation coefficient: r=0.9996
The result shows that rutin is good in 0.000 μ g/ml-30.432 μ g/ml concentration range internal linear relation.
Algoscopy takes by weighing the about 2.0g of Semen Astragali Complanati (salt is processed) powder (crossing 20 mesh sieves), and accurate the title decides, and puts in the apparatus,Soxhlet's, add an amount of reflux 4h of petroleum ether, medicinal residues volatilize solvent, accurately add 80% ethanol 50ml, weigh,, take out and put cold weighing in 85 ℃ of reflux 1.5h of water-bath, replenish 80% ethanol to former weight, mixing is placed, the accurate supernatant 1ml that draws, put in the 25ml measuring bottle, the method under the preparation of sighting target directrix curve is from " adding 10%AlCl
3Solution 1ml " rise, measure trap in accordance with the law, read the weight of rutin the need testing solution from standard curve, calculate.
The assay of 10 batches of Semen Astragali Complanatis (salt is processed) sample
Measure general flavone content in 10 batch samples as stated above, the result is as shown in the table.
Total flavones measurement result in table 10 batches of Semen Astragali Complanatis of 15-2 (salt is processed) medical material
| The place of production | General flavone content % | Average % | |
| Qinghai, Zhejiang, Henan, Shaanxi | 0.920 0.600 0.549 0.671 | 0.933 0.611 0.523 0.654 | 0.926 0.605 0.536 0.663 |
| Anhui, Hunan, Xinjiang, Yunnan, Inner Mongol, Shanxi | 0.433 0.742 0.435 1.105 1.446 0.390 | 0.452 0.762 0.426 1.121 1.432 0.375 | 0.443 0.752 0.431 1.113 1.439 0.382 |
The average content of 10 batches of medical material total flavones is 0.729%, according to above result, considers place of production difference, simultaneously in order to control the quality of Semen Astragali Complanati (salt is processed) medical material, decides to contain total flavones with rutin (C in Semen Astragali Complanati (salt is processed) medical material
27H
30O
16) meter, must not be less than 0.4%.
Semen Astragali Complanati oral liquid of the present invention is the particulate agent product that changes of Semen Astragali Complanati, therefore production technology is improved, the extraction process of Semen Astragali Complanati oral liquid is continued to use the particulate extraction process of Semen Astragali Complanati, selected optimum extraction condition is: add 10 times of water gagings for the first time and decocted 1.5 hours, add 8 times of water gagings for the second time and decocted 1 hour.
Simultaneously, pharmaceutical formulation is screened, antiseptic kind, consumption and correctives consumption are investigated, finally be defined as adding 0.3% potassium sorbate and 0.05% acesulfame potassium.
On test chamber lab scale basis, carried out many batches according to this technology in the production of test agent, the general flavone content data show this process stabilizing in yield rate and the finished product, and are feasible.
Method of quality control is improved on the basis of continuing to use and improves:
1, differentiates with reference to the 12 particulate quality standard of Semen Astragali Complanati of the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation and relevant list of references, Semen Astragali Complanati (salt is processed) in the prescription has been carried out Study on Identification.The outcome quality standard body has been continued to use the physicochemical identification in the Semen Astragali Complanati granule, and the Semen Astragali Complanati discrimination method is improved, and the thin layer that has increased Semen Astragali Complanati is differentiated.
2, assay Semen Astragali Complanati (salt is processed) medical material and Semen Astragali Complanati granule proper mass standard do not have the assay item.This research is used colorimetry with reference to relevant document, is reference substance with the rutin, by methodological study, has set up in the Semen Astragali Complanati oral liquid content of total flavone assay method and has determined content limit.Simultaneously, tentatively determined content of total flavone limit in Semen Astragali Complanati (salt is processed) medical material.
By measuring content of total flavone in the 10 batches of Semen Astragali Complanatis in the different places of production (salt is processed) medical material, tentatively determine to contain total flavones with rutin (C in the Semen Astragali Complanati (salt is processed)
27H
30O
16) meter, must not be less than 0.4%.
Simultaneously, be defined as every bottle and contain total flavones with rutin (C according to the measurement result of test agent in ten batches
27H
30O
16) meter, must not be less than 4.8mg.
Preparation of the present invention is accelerated tests 6 months and 12 months (experimentation is also underway) of room temperature investigation under the condition of temperature (40 ℃ ± 2 ℃), relative humidity 75%, and every index does not have obvious variation, steady quality.
More than this product described in the method for quality control of the present invention, be meant Semen Astragali Complanati oral liquid according to prepared of the present invention, when other dosage forms are measured, refer to corresponding other dosage forms.
The invention has the advantages that: method of quality control of the present invention has guaranteed that the quality inspection standard of preparation of the present invention can be than the qualitative character of effectively controlling preparation comprehensively, have accuracy and advance, can be used as the effective technology means of the stability of quality control and investigation technology.Be of great importance to improving the quality of products.
The specific embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
The quality control of embodiment 1 Semen Astragali Complanati oral liquid
[character] this product is that pale brown color is to brown liquid; It is sweet to distinguish the flavor of, little hardship.
The discriminating of content, step is:
This product 0.5ml is got in [discriminating] (1), adds water 2ml, adds 4～5 of hydrochloric acid, and a small amount of magnesium powder, and it is hot slightly to put water-bath, promptly shows red.
(2) preparation of need testing solution: get this product, as need testing solution.Other gets Semen Astragali Complanati control medicinal material 1.0g, puts in the apparatus,Soxhlet's, adds an amount of reflux 4h of petroleum ether, and medicinal residues volatilize solvent, adds 80% ethanol 20ml, and reflux 1.5h is put coldly, filters, and filtrate is medical material solution in contrast.Test according to thin layer chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, with methanol-water (4: 1) is developing solvent, launches, and takes out, dry, spray is with 1% aluminum chloride alcoholic solution, and the heating colour developing is put under the ultra-violet lamp (365nm) and inspected.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color.
The inspection of content, step is:
[inspection] pH value should be 4.5～6.5 (an appendix VII of Chinese Pharmacopoeia version in 2005 G).
Other should meet every regulation relevant under the mixture item (an appendix I of Chinese Pharmacopoeia version in 2005 J).The composition that contains is carried out assay, and step is:
The preparation precision of [assay] reference substance solution takes by weighing the control substance of Rutin 25.0mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 50ml measuring bottle, and it is an amount of to add methanol, and slight fever makes dissolving, and the back that cools is diluted to scale with methanol, shakes up, promptly.
The preparation precision of standard curve is measured reference substance solution 0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0ml, puts respectively in the 50ml measuring bottle, adds 10%AlCl
3Solution 1ml adds water to scale, shakes up, placed 15 minutes, and be blank with corresponding solution.According to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2005 B), measure trap at 415nm wavelength place, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve.
The algoscopy precision is measured this product 1ml, puts in the 100ml measuring bottle, and the method under the preparation of sighting target directrix curve is from " adding 10%AlCl
3Solution 1ml " rise, measure trap in accordance with the law, read the weight of rutin the need testing solution from standard curve, calculate, promptly.
This product contains total flavones with rutin (C for every bottle
27H
30O
16) meter, must not be less than 4.8mg.
Embodiment 2
The Semen Astragali Complanati oral liquid
Semen Astragali Complanati oral liquid method for making is as follows: get Semen Astragali Complanati (salt is processed) 500 grams, add water and extract secondary, 1.5 hours first time, 1 hour for the second time in 80 ℃.Merge extractive liquid, filters, and filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (80～85 ℃ of heat are surveyed), add ethanol and make and contain alcohol amount and reach 60%, stir evenly, left standstill 12 hours, filter, filtrate recycling ethanol adds 0.3% potassium sorbate and 0.05% acesulfame potassium, adds water and makes and make 1000ml, mixing, embedding, sterilization, promptly.
Embodiment 3
The Semen Astragali Complanati oral liquid
Semen Astragali Complanati oral liquid method for making is as follows: get Semen Astragali Complanati (salt is processed) 250 grams, add water and extract secondary, 1.5 hours first time, 1 hour for the second time in 80 ℃.Merge extractive liquid, filters, and filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (80～85 ℃ of heat are surveyed), add ethanol and make and contain alcohol amount and reach 60%, stir evenly, left standstill 12 hours, filter, filtrate recycling ethanol adds 0.3% potassium sorbate and 0.05% acesulfame potassium, adds water and makes and make 1000ml, mixing, embedding, sterilization, promptly.
Embodiment 4
The Semen Astragali Complanati oral liquid
Semen Astragali Complanati oral liquid method for making is as follows: get Semen Astragali Complanati (salt is processed) 1000 grams, add water and extract secondary, 1.5 hours first time, 1 hour for the second time in 80 ℃.Merge extractive liquid, filters, and filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (80～85 ℃ of heat are surveyed), add ethanol and make and contain alcohol amount and reach 60%, stir evenly, left standstill 12 hours, filter, filtrate recycling ethanol adds 0.3% potassium sorbate and 0.05% acesulfame potassium, adds water and makes and make 1000ml, mixing, embedding, sterilization, promptly.
Claims (10)
1, a kind of method of quality control of flatstem milkvetch seed preparation is characterized in that, comprises the observation of character, the discriminating of content, and the step of assay is carried out in the inspection of content to the composition that contains.
2, the method for claim 1 is characterized in that, described flatstem milkvetch seed preparation is an oral formulations.
3, the method for claim 2 is characterized in that, described oral formulations is oral liquid, granule, tablet or capsule.
4, the method for claim 2 is characterized in that, described oral formulations is an oral liquid.
5, the method for claim 4 is characterized in that, described method step is as follows:
The observation of character, step is:
[character] this product is that pale brown color is to brown liquid; It is sweet to distinguish the flavor of, little hardship;
The discriminating of content, step is:
This product 0.5ml is got in [discriminating] (1), adds water 2ml, adds 4～5 of hydrochloric acid, and a small amount of magnesium powder, and it is hot slightly to put water-bath, promptly shows red;
(2) preparation of need testing solution: get this product, as need testing solution; Other gets Semen Astragali Complanati control medicinal material 1.0g, puts in the apparatus,Soxhlet's, adds an amount of reflux 4h of petroleum ether, and medicinal residues volatilize solvent, adds 80% ethanol 20ml, and reflux 1.5h is put coldly, filters, and filtrate is medical material solution in contrast; Test according to thin layer chromatography (2005 editions one appendix VI B of Chinese Pharmacopoeia), draw each 2 μ l of above-mentioned two kinds of solution, put respectively on same polyamide film, with methanol-water (4: 1) is developing solvent, launches, and takes out, dry, spray is with 1% aluminum chloride alcoholic solution, and the heating colour developing is put under the ultra-violet lamp (365nm) and inspected; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the fluorescence speckle of same color;
The inspection of content, step is:
[inspection] pH value should be 4.5～6.5 (an appendix VII of Chinese Pharmacopoeia version in 2005 G);
Other should meet every regulation relevant under the mixture item (an appendix I of Chinese Pharmacopoeia version in 2005 J); The composition that contains is carried out assay, and step is:
The preparation precision of [assay] reference substance solution takes by weighing the control substance of Rutin 25.0mg of 120 ℃ of drying under reduced pressure to constant weight, puts in the 50ml measuring bottle, and it is an amount of to add methanol, and slight fever makes dissolving, and the back that cools is diluted to scale with methanol, shakes up, promptly;
The preparation precision of standard curve is measured reference substance solution 0ml, 0.5ml, 1.0ml, 1.5ml, 2.0ml, 2.5ml, 3.0ml, puts respectively in the 50ml measuring bottle, adds 10%AlCl
3Solution 1ml adds water to scale, shakes up, placed 15 minutes, and be blank with corresponding solution; According to spectrophotography (an appendix V of Chinese Pharmacopoeia version in 2005 B), measure trap at 415nm wavelength place, be that vertical coordinate, concentration are abscissa with the trap, the drawing standard curve;
The algoscopy precision is measured this product 1ml, puts in the 100ml measuring bottle, and the method under the preparation of sighting target directrix curve is from " adding 10%AlCl
3Solution 1ml " rise, measure trap in accordance with the law, read the weight of rutin the need testing solution from standard curve, calculate, promptly;
This product contains total flavones in rutin (C27H30O16) for every bottle, must not be less than 4.8mg.
According to the method for claim 1, it is characterized in that 6, described flatstem milkvetch seed preparation is to be made by the raw material of Chinese medicine of following weight: Semen Astragali Complanati (salt is processed) 250-1000g.
According to the method for claim 1, it is characterized in that 7, described flatstem milkvetch seed preparation is to be made by the raw material of Chinese medicine of following weight: Semen Astragali Complanati (salt is processed) 500g.
8, according to the method for claim 1, it is characterized in that, wherein said flatstem milkvetch seed preparation is by Semen Astragali Complanati (salt is processed) raw material of Chinese medicine is processed through extraction or other modes, make pharmaceutically active substance, subsequently, with this material is raw material, add the medicine acceptable carrier when needing, make according to the routine techniques of galenic pharmacy, described active substance obtains by the method that is selected from following mode: pulverize, squeeze, calcine, grind, sieve, percolation, extraction, water are carried, alcohol extraction, ester are carried, ketone is carried or chromatography.
9, method according to Claim 8 is characterized in that, wherein said flatstem milkvetch seed preparation is an oral liquid.
According to the method for claim 9, it is characterized in that 10, wherein said oral liquid is by preparing through following method: get Semen Astragali Complanati (salt is processed) 500 grams, add water and extract secondaries, 1.5 hours first time, 1 hour for the second time in 80 ℃; Merge extractive liquid, filters, and filtrate is concentrated into the clear paste that relative density is 1.20～1.25 (80～85 ℃ of heat are surveyed), add ethanol and make and contain alcohol amount and reach 60%, stir evenly, left standstill 12 hours, filter, filtrate recycling ethanol adds correctives, antiseptic is an amount of, adding water makes and makes 1000ml, mixing, embedding, sterilization, promptly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610065644 CN1857381A (en) | 2006-03-23 | 2006-03-23 | Quality control method for flatstem milkvetch seed preparation |
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|---|---|---|---|
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203474A (en) * | 2015-09-01 | 2015-12-30 | 贵州师范大学 | Detection method of traditional Chinese medicine health care preparation for protecting chemical liver injuries |
| CN110018269A (en) * | 2019-04-29 | 2019-07-16 | 四川新绿色药业科技发展有限公司 | A kind of thin-layer identification method of salt semen astragali complanati granule |
-
2006
- 2006-03-23 CN CN 200610065644 patent/CN1857381A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105203474A (en) * | 2015-09-01 | 2015-12-30 | 贵州师范大学 | Detection method of traditional Chinese medicine health care preparation for protecting chemical liver injuries |
| CN105203474B (en) * | 2015-09-01 | 2018-06-15 | 贵州师范大学 | A kind of detection method of the traditional Chinese medicine health care product preparation of protection chemical damage |
| CN110018269A (en) * | 2019-04-29 | 2019-07-16 | 四川新绿色药业科技发展有限公司 | A kind of thin-layer identification method of salt semen astragali complanati granule |
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Open date: 20061108 |