CN1857591A - Quality control method for diabetes treating Tangniaole bolus - Google Patents
Quality control method for diabetes treating Tangniaole bolus Download PDFInfo
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Abstract
The present invention relates to quality control method for diabetes treating Tangniaole bolus. The quality control method includes thin layer chromatography process for material identification and spectrophotometric method for content measurement. The quality control method is precise, sensitive and stable, and can ensure the high and stable product quality.
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 TANGNIAOLE ball (concentrated pill) preparation.
Background technology:
TANGNIAOLE derives from the 13rd of ministry standard, and the 225th page, standard is numbered WS3-B-2644-97, is capsule.Prescription consists of: Radix Trichosanthis, Rhizoma Dioscoreae, the Radix Astragali, Radix Ginseng Rubra, Radix Rehmanniae, Fructus Lycii, the Rhizoma Anemarrhenae, Radix Asparagi, Poria, Fructus Corni, Fructus Schisandrae Chinensis, Radix Puerariae, Endothelium Corneum Gigeriae Galli (stir-fry) are formed.Have enriching yin and nourishing kidney, the QI invigorating lung moistening, stomach function regulating promotes the production of body fluid, regulates metabolism.Be used for polyphagia, polydipsia, polyuria that diabetes causes, diseases such as myasthenia of limbs, blood sugar lowering, glucose in urine.
It is relevant that the morbidity of type 2 diabetes mellitus and insulin resistant and B cell secretory function go down, and is the coefficient result of multiple h and E factor (obesity, high caloric diet, physical exertion minimizing etc.).Its pathological change can cause that general metabolism is disorderly and large, medium and small, microangiopathies and neuropathy, so its complication is more.Common complication has hypertension, coronary heart disease, ischemic cerebrovascular, diabetic nephropathy, diabetic renal papillary necrosis, diabetic foot, diabetic peripheral neuropathy etc.
Type 2 diabetes mellitus has formed the diagnosis and treatment pattern that the doctor trained in Western medicine differential diagnosis of diseases combines with Chinese medical discrimination clinically.The diagnostic criteria of doctor trained in Western medicine, the traditional Chinese medical science are also generally accepted.After the diagnosis of the at first clear and definite doctor trained in Western medicine disease of the traditional Chinese medical science, capable again determination of treatment based on pathogenesis obtained through differentiation of symptoms and signs.Though more than the kind, can be merged, be reduced 4 kinds of the most basic pattern of syndrome, i.e. intense heat due to deficiency of YIN card, syndrome of yin deficiency of liver and kidney, syndrome of deficiency of both qi and yin, deficiency syndrome of both YIN and YANG surplus type 2 diabetes mellitus Chinese medical discrimination typing can have seven or eight kinds even ten.Wherein see at most with syndrome of deficiency of both qi and yin again, can account for 50% of whole pattern of syndrome.
TANGNIAOLE
[1]In the prescription there be drugs for nourishing yin: Radix Rehmanniae, Fructus Corni, Fructus Lycii, Radix Asparagi, the Rhizoma Anemarrhenae, Radix Trichosanthis, Qi-tonifying drug are as the Radix Astragali, Radix Ginseng Rubra, Rhizoma dioscoreae, Fructus Schisandrae Chinensis.Other adds Poria, Endothelium Corneum Gigeriae Galli (stir-fry) stimulating appetite; Radix Puerariae is to bring down a fever.
Wang Yufen
[2]Deng employing intact animal and diabetes model animal the blood sugar reducing function of TANGNIAOLE is observed.The result shows: TANGNIAOLE can reduce normal mouse and rat blood serum insulin level and hepatic glycogen content and raise; Epinephrine induced hyperglycemia rat blood sugar is obviously reduced, and hepatic glycogen obviously increases; Mice and rat blood sugar due to the alloxan all there is the obvious suppression effect; Can also improve the rat carbohydrate tolerance.
In sum, TANGNIAOLE has the effect of enriching yin boost qi stomach function regulating.Be used for the type 2 diabetes mellitus syndrome of deficiency of both qi and yin.
Existing TANGNIAOLE 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 TANGNIAOLE 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 TANGNIAOLE 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 TANGNIAOLE preparation.
The TANGNIAOLE preparation prescription consists of:
One, prescription
Radix Trichosanthis 104.3g Rhizoma Dioscoreae 104.3g Radix Astragali 26g
Radix Ginseng Rubra 15.65g Radix Rehmanniae 26g Fructus Lycii 15.65g
Rhizoma Anemarrhenae 15.65g Radix Asparagi 7.8g Poria 10.5g
Fructus Corni 10.5g Fructus Schisandrae Chinensis 7.8g Radix Puerariae 10.5g
Endothelium Corneum Gigeriae Galli (stir-fry) 10.5g
TANGNIAOLE ball (concentrated pill) method for making:
More than 13 the flavor, get Rhizoma Dioscoreae 52.15g, Radix Trichosanthis 52.15g, Endothelium Corneum Gigeriae Galli, Radix Ginseng Rubra, be ground into fine powder; All the other Rhizoma Dioscoreae 52.15g, Radix Trichosanthis 52.15g, the Radix Astragali, the Radix Rehmanniae, Fructus Corni, Fructus Lycii, Fructus Schisandrae Chinensis, the Rhizoma Anemarrhenae, Radix Puerariae, Radix Asparagi, Poria decoct with water and add 10 times of water gagings decoctions 2 hours for the first time, adding for the second time 8 times of water gagings decocted 2 hours, collecting decoction, filter, filtrate is concentrated into relative density and is about 1.30 (50 ℃) thick paste; With Rhizoma Dioscoreae, Radix Trichosanthis, Endothelium Corneum Gigeriae Galli, Radix Ginseng Rubra fine powder, mixing is made 1000 balls, drying, and polishing, promptly.
The present invention be directed to TANGNIAOLE ball (concentrated pill) preparation and propose method of quality control, but also be not limited to TANGNIAOLE ball (concentrated pill) preparation, also can comprise other oral formulations of TANGNIAOLE ball such as tablet, capsule, syrup, granule.
Its prescription of other dosage forms of the TANGNIAOLE that the present invention includes is identical with TANGNIAOLE ball (concentrated pill) preparation, 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.
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 TANGNIAOLE 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 TANGNIAOLE 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.
TANGNIAOLE preparation of the present invention, particularly concentrated pill preparation, it is as follows that its function cures mainly usage and dosage:
[function with cure mainly] enriching yin and nourishing kidney, the QI invigorating lung moistening, stomach function regulating promotes the production of body fluid, regulates metabolism.Be used for polyphagia, polydipsia, polyuria that diabetes causes, diseases such as myasthenia of limbs, blood sugar lowering, glucose in urine.
[usage and consumption] is oral, one time 6～8 ball, 3 times on the one.
[specification] per 8 balls are equivalent to crude drug 3 grams.
[storage] sealing.
[effect duration] tentative 2 years
The present invention is to provide the method for quality control at above TANGNIAOLE preparation, particularly oral liquid formulations, be the quality of control TANGNIAOLE 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 the concentrated pill of yellowish-brown; Feeble QI perfume (or spice), acrid in the mouth, little hardship.
The discriminating of content, step is:
This product is got in [discriminating] (1), and put microscopically and observe, starch grain simple grain similar round, flat avette, the square circle, diameter 6～35 μ m, omphalion point-like, herringbone shape, crosswise or short seam shape, laminated striation mays be seen indistinctly.Irregular agglomerate or irregular lamellar, faint yellow or closely colourless, be cullet quarrel sample, corner angle are clearly demarcated, the visible wire texture that has.
(2) get this product, porphyrize takes by weighing about 8g, add chloroform 50ml, refluxed 1 hour, filter, discard filtrate, filtering residue volatilizes chloroform, adds methanol 50ml reflux, extract, 1 hour, filter, filtrate evaporate to dryness, residue add an amount of dissolve with methanol, be added on the neutral alumina post (100-120 order, 5g, internal diameter 10-15mm), with 40% methanol 100ml methanol-eluted fractions, collect eluent, evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, ammonia solution washing with 3 times discards ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the Ginsenoside Rb
1, panaxoside Rg
1Reference substance adds methanol respectively and makes 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 need testing solution 5 μ l reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get this product, porphyrize takes by weighing about 8g, adds methanol 30ml merceration 1 hour, filters, and filtrate evaporate to dryness, residue add methanol 1ml dissolving, and as need testing solution, other gets the puerarin reference substance, adds methanol and makes 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 need testing solution 5 μ l and reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(4) get this product, porphyrize takes by weighing about 8g, add chloroform 50ml, refluxed 1 hour, filter, residue volatilizes chloroform, adds methanol 50ml reflux, extract, 1 hour, filters, evaporate to dryness, residue is dissolved in water, and extracts 2 times with water saturated n-butyl alcohol liquid, each 20ml discards water liquid, the ammonia solution washing that n-butyl alcohol liquid reuse is 3 times, with n-butyl alcohol liquid evaporate to dryness, residue adds the 1ml dissolve with methanol as need testing solution.Other gets the astragaloside reference substance, adds methanol and makes 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 each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ are heated to clear spot.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Place again under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(5) get this product, porphyrize takes by weighing about 40g, adds chloroform 80ml reflux, extract, 1 hour, filter, filtrate is washed with 1% sodium hydroxide solution 50ml, discards sodium hydroxide solution, with chloroform liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Fructus Schisandrae Chinensis control medicinal material 1g, water decocts twice, merge water liquid, extract with the jolting of 20ml chloroform, discard water liquid, chloroform extraction liquid washs with 1% sodium hydroxide solution 20ml, discard sodium hydroxide solution, with chloroform extraction liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 15 μ l and control medicinal material solution 5 μ l, putting respectively on same silica GF254 lamellae, is developing solvent with toluene-ethyl acetate (6: 4), launches, take out, dry, put under the ultra-violet lamp (254nm) and inspect, 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] should meet every regulation relevant under the pill item (appendix IA of Chinese Pharmacopoeia version in 2005).
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (Chinese Pharmacopoeia appendix VI D in 2005).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (20: 80)
Be mobile phase; The detection wavelength is 250nm; Column temperature is 30 ℃.Number of theoretical plate calculates by puerarin peak should be not less than 4000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the puerarin reference substance, adds 30% ethanol and make the solution that contains puerarin 50 μ g among every 1ml, shakes up, promptly.
This product under the weight differential item is got in the preparation of need testing solution, is ground into fine powder, gets about 4.0g, the accurate title, decide, and puts in the conical flask, the accurate 30% ethanol 50ml that adds, claim to decide weight, supersound extraction 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 30% ethanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every gram of this product contains Radix Puerariae with puerarin (C
21H
20O
9) meter, must not be less than 0.46mg.
The present invention changes agent on former dosage form basis, simultaneously production technology is reformed, the extraction process amount of water is studied and the cream powder ratio of the soft material of pill molding carried out research is final determines technology of the present invention: can influence molding the ratio of powder in the soft material is bigger than normal, cause the ball bar more coarse, easily broken; The ratio soft material that can make again less than normal is soft excessively, also is unfavorable for molding.Test is found, therefore the large percentage of the powder of this product is that index is tested and seen the following form with the relative density of clear paste,
| The relative density of extractum (g/ml) | |
| 1.35(50℃) 1.30(50℃) | The soft material of making can cause the ball shaping rate on the low side because of moisture is too low, the ball bar is more coarse, the easily broken soft material of making is more suitable, pill is smooth, the ball bar is continuous not coarse yet, ball shape rounding, the surface is flawless |
So determine that the extractum relative density is controlled near 1.30 (50 ℃).The soft material of so making is moderate, and pill is smooth, and the ball bar is continuous not coarse yet, ball shape rounding, and the surface is flawless.The Pulvis Talci of reuse 5%, 0.0375% river wax powder glazing, the finished product ball outward appearance rounding light of making, free from flaw, and dissolve scattered time limit also meets the requirements.
With YUJ-16A type high speed pellet processing machine, 6.5mm mould, the control ball focuses on 0.17g, pill, heat-wind circulate drying baking oven inner drying, 50 ~ 55 ℃ of design temperatures dry by the fire to water content below 7%, take out, the sieve ball, polishing, the finished product ball.
This product is made up of 13 flavor medical materials such as variola, Rhizoma Dioscoreae, the Radix Astragali, Radix Ginseng Rubra, Radix Rehmanniae, is by TANGNIAOLE JIAONANG (national drug standards WS
3-B-2644-97) dosage changing form research forms.One microscopical identification is only arranged in the primary standard, is better control product quality, and we increase the thin layer discriminating to Radix Ginseng Rubra, Radix Puerariae, the Radix Astragali, Fructus Schisandrae Chinensis, and feminine gender is not disturbed.Set up the assay method of puerarin content in the finished product simultaneously.
14.2.1 differentiate
14.2.1.1 the microscopical identification of Radix Trichosanthis and Endothelium Corneum Gigeriae Galli in discriminating (1) side of being
Get this product, put microscopically and observe, starch grain simple grain similar round, flat avette, the square circle, diameter 6～35 μ m, omphalion point-like, herringbone shape, crosswise or short seam shape, laminated striation mays be seen indistinctly.Irregular agglomerate or irregular lamellar, faint yellow or closely colourless, be cullet quarrel sample, corner angle are clearly demarcated, the visible wire texture that has.Consistent with former TANGNIAOLE JIAONANG microscopic features.
14.2.1.2 differentiating the thin layer of Radix Ginseng Rubra in (2) side of being differentiates
We are with the Ginsenoside Rb
1, panaxoside Rg
1, ginsenoside Re's reference substance for the contrast carry out Study on Identification, make negative control simultaneously, put respectively and inspect under daylight and the ultra-violet lamp (365nm), the result shows, the Ginsenoside Rb
1, panaxoside Rg
1Negative control is not seen interference, some interference of ginsenoside Re's negative control.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.So this discriminating is with the Ginsenoside Rb
1, panaxoside Rg
1For contrast is listed in this product quality standard.
14.2.1.3 differentiating the thin layer of Radix Puerariae in (3) side of being differentiates
We serve as that Study on Identification is carried out in contrast with the puerarin reference substance, make negative control simultaneously, and the result shows: negative control is not seen interference, in the test sample chromatograph with contrast chromatograph corresponding position on, show the speckle of same color.So this discriminating is listed in this product quality standard.
14.2.1.4 differentiating the thin layer of the Radix Astragali in (4) side of being differentiates
We serve as that Study on Identification is carried out in contrast with the astragaloside reference substance, make negative control simultaneously, and the result shows: negative control is not seen interference, in the test sample chromatograph with contrast chromatograph corresponding position on, show the speckle of same color.So this discriminating is listed in this product quality standard.
14.2.1.5 differentiating the Pu layer of Fructus Schisandrae Chinensis in (5) side of being differentiates
We serve as that Study on Identification is carried out in contrast with the Fructus Schisandrae Chinensis control medicinal material, make negative control simultaneously, and the result shows: negative control is not seen interference, in the test sample chromatograph with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.So this discriminating is listed in this product quality standard.
14.2.1.6 other
14.2.1.6.1 the Study on Identification of the Rhizoma Anemarrhenae
List of references is taken methanol supersound process 30min, filters, and evaporate to dryness, residue add methanol 1ml makes dissolving, Rhizoma Anemarrhenae control medicinal material water decocted 1 hour, used dissolve with methanol behind the evaporate to dryness, filtered, residue adds methanol 1ml makes dissolving, and test sample gained speckle is not obvious as a result, so be not listed as standard body.
14.2.1.6.2 the Study on Identification of Radix Rehmanniae
List of references is got this product powder 10g, adds methanol 20ml, and reflux 1 hour is put coldly, filters, and filtrate is reclaimed methanol to 5ml, as need testing solution.Other gets the catalpol reference substance and adds methanol and make the solution that every 1ml contains 0.5mg, product solution in contrast, draw each 5 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel g thin-layer plate, is developing solvent with chloroform-methanol-water (14: 6: 1), launches, take out, dry, spray is with the anisaldehyde test solution, and 105 ℃ to be heated to speckle colour developing clear.The result shows that feminine gender has interference, so do not list standard body in.
14.2.2 check
14.2.2.1 dissolve scattered time limit
Check that according to dissolve scattered time limit inspection technique under the pill item [2000 editions appendix IA of Chinese Pharmacopoeia] result is all up to specification.
14.2.2.2 weight differential
Check that according to weight differential inspection technique under the pill item [2000 editions appendix IA of Chinese Pharmacopoeia] result is all up to specification.
14.2.2.3 moisture content
Measure according to first method in the aquametry [an appendix IX of Chinese Pharmacopoeia version in 2000 H], the result is up to specification.
14.2.2.4 heavy metal
Checked 3 batch samples by heavy metal inspection technique [2000 editions one appendix IX E of Chinese Pharmacopoeia, second method], the result all surpasses 10/1000000ths, so quality standard is not included in an inspection temporarily in.
14.2.2.5 arsenic salt
Having checked 3 batch samples according to arsenic salt inspection technique [2000 editions one appendix IX F of Chinese Pharmacopoeia, first method], the result all surpasses 1,000,000/, so check and not include quality standard temporarily in.
14.2.2.6 limit test of microbe
Press 2000 editions one appendix XIII C of Chinese Pharmacopoeia " microbial limit standard " regulation, the pill bacterial population that contains medical material must not be crossed 30000/g, and mycete, yeast count must not be crossed 100/g, and the demodicid mite that lives must not detect, and colibacillus must not detect.Several batches of testing results of this preparation are all up to specification.
14.2.3 assay
Content of puerarin is measured
(1) instrument and reagent
Instrument: Agilent1100 type high performance liquid chromatograph, G1315A VWD;
Hypersil Yi Lite analytical column (4.6 * 250mm, 5 μ m);
AB204-S type electronic balance (prunus mume (sieb.) sieb.et zucc. Teller-holder benefit company);
AG-135 type electronic balance (prunus mume (sieb.) sieb.et zucc. Teller-holder benefit company).
Reagent: methanol is chromatographically pure, and water is redistilled water, and other reagent is analytical pure.
Reference substance: the puerarin reference substance (is identified lot number: 110752-200209) available from Chinese pharmaceutical biological product
(2) method and result
1, chromatographiccondition
Immobile phase: octadecylsilane chemically bonded silica
Mobile phase: methanol: water (20: 80)
Detect wavelength 250nm, 30 ℃ of column temperatures, flow velocity 1.0ml/min,
2, system suitability test: in the above conditions, the adjacent component with other of puerarin all can reach baseline separation well, and number of theoretical plate calculates by puerarin peak and is not less than 4000.And the negative control of scarce Radix Puerariae does not have absworption peak under identical retention time, illustrates with this condition feasible.
3, result of the test
The result of methodological study shows that puerarin concentration becomes the good linear relation in 4.034～80.68 μ g/ml, the repeatability test of the stability of reference substance solution and need testing solution, precision and sample, RSD% all＜3.0%, average recovery is 100.5%.By its quality standard check, the result is all up to specification to three batches of pilot products.
4, content limit is determined
According to 10 batch samples, in conjunction with the rate of transform of preparation technology's puerarin, determine that finally the content limit of this product is: the every gram of this product contains Radix Puerariae with puerarin (C
21H
20O
9) meter, must not be less than 0.46mg.
More than this product described in the method for quality control of the present invention, be meant TANGNIAOLE ball (concentrated pill) 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 TANGNIAOLE ball (concentrated pill)
The observation of character, step is:
[character] this product is the concentrated pill of yellowish-brown; Feeble QI perfume (or spice), acrid in the mouth, little hardship.
The discriminating of content, step is:
This product is got in [discriminating] (1), and put microscopically and observe, starch grain simple grain similar round, flat avette, the square circle, diameter 6～35 μ m, omphalion point-like, herringbone shape, crosswise or short seam shape, laminated striation mays be seen indistinctly.Irregular agglomerate or irregular lamellar, faint yellow or closely colourless, be cullet quarrel sample, corner angle are clearly demarcated, the visible wire texture that has.
(2) get this product, porphyrize takes by weighing about 8g, add chloroform 50ml, refluxed 1 hour, filter, discard filtrate, filtering residue volatilizes chloroform, adds methanol 50ml reflux, extract, 1 hour, filter, filtrate evaporate to dryness, residue add an amount of dissolve with methanol, be added on the neutral alumina post (100-120 order, 5g, internal diameter 10-15mm), with 40% methanol 100ml methanol-eluted fractions, collect eluent, evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, ammonia solution washing with 3 times discards ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the Ginsenoside Rb
1, panaxoside Rg
1Reference substance adds methanol respectively and makes 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 need testing solution 5 μ l reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color.
(3) get this product, porphyrize takes by weighing about 8g, adds methanol 30ml merceration 1 hour, filters, and filtrate evaporate to dryness, residue add methanol 1ml dissolving, and as need testing solution, other gets the puerarin reference substance, adds methanol and makes 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 need testing solution 5 μ l and reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(4) get this product, porphyrize takes by weighing about 8g, add chloroform 50ml, refluxed 1 hour, filter, residue volatilizes chloroform, adds methanol 50ml reflux, extract, 1 hour, filters, evaporate to dryness, residue is dissolved in water, and extracts 2 times with water saturated n-butyl alcohol liquid, each 20ml discards water liquid, the ammonia solution washing that n-butyl alcohol liquid reuse is 3 times, with n-butyl alcohol liquid evaporate to dryness, residue adds the 1ml dissolve with methanol as need testing solution.Other gets the astragaloside reference substance, adds methanol and makes 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 each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ are heated to clear spot.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Place again under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(5) get this product, porphyrize takes by weighing about 40g, adds chloroform 80ml reflux, extract, 1 hour, filter, filtrate is washed with 1% sodium hydroxide solution 50ml, discards sodium hydroxide solution, with chloroform liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets Fructus Schisandrae Chinensis control medicinal material 1g, water decocts twice, merge water liquid, extract with the jolting of 20ml chloroform, discard water liquid, chloroform extraction liquid washs with 1% sodium hydroxide solution 20ml, discard sodium hydroxide solution, with chloroform extraction liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, in contrast medical material solution.Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 15 μ l and control medicinal material solution 5 μ l, putting respectively on same silica gel 6F254 lamellae, is developing solvent with toluene-ethyl acetate (6: 4), launches, take out, dry, put under the ultra-violet lamp (254nm) and inspect, 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] should meet every regulation relevant under the pill item (appendix IA of Chinese Pharmacopoeia version in 2005).
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (Chinese Pharmacopoeia appendix VI D in 2005).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (20: 80)
Be mobile phase; The detection wavelength is 250nm; Column temperature is 30 ℃.Number of theoretical plate calculates by puerarin peak should be not less than 4000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the puerarin reference substance, adds 30% ethanol and make the solution that contains puerarin 50 μ g among every 1ml, shakes up, promptly.
This product under the weight differential item is got in the preparation of need testing solution, is ground into fine powder, gets about 4.0g, the accurate title, decide, and puts in the conical flask, the accurate 30% ethanol 50ml that adds, claim to decide weight, supersound extraction 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 30% ethanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The every gram of this product contains Radix Puerariae with puerarin (C
21H
20O
9) meter, must not be less than 0.46mg.
Embodiment 2 TANGNIAOLE balls (concentrated pill)
One, prescription
Radix Trichosanthis 104.3g Rhizoma Dioscoreae 104.3g Radix Astragali 26g
Radix Ginseng Rubra 15.65g Radix Rehmanniae 26g Fructus Lycii 15.65g
Rhizoma Anemarrhenae 15.65g Radix Asparagi 7.8g Poria 10.5g
Fructus Corni 10.5g Fructus Schisandrae Chinensis 7.8g Radix Puerariae 10.5g
Endothelium Corneum Gigeriae Galli (stir-fry) 10.5g
TANGNIAOLE ball (concentrated pill) method for making:
More than 13 the flavor, get Rhizoma Dioscoreae 52.15g, Radix Trichosanthis 52.15g, Endothelium Corneum Gigeriae Galli, Radix Ginseng Rubra, be ground into fine powder; All the other Rhizoma Dioscoreae 52.15g, Radix Trichosanthis 52.15g, the Radix Astragali, the Radix Rehmanniae, Fructus Corni, Fructus Lycii, Fructus Schisandrae Chinensis, the Rhizoma Anemarrhenae, Radix Puerariae, Radix Asparagi, Poria decoct with water and add 10 times of water gagings decoctions 2 hours for the first time, adding for the second time 8 times of water gagings decocted 2 hours, collecting decoction, filter, filtrate is concentrated into relative density and is about 1.30 (50 ℃) thick paste; With Rhizoma Dioscoreae, Radix Trichosanthis, Endothelium Corneum Gigeriae Galli, Radix Ginseng Rubra fine powder, mixing is made 1000 balls, drying, and polishing, promptly.
Claims (8)
1, a kind of method of quality control of TANGNIAOLE 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 TANGNIAOLE preparation is an oral solid formulation.
3, the method for claim 2 is characterized in that, described oral solid formulation is the TANGNIAOLE ball.
4, the method for claim 3 is characterized in that, described method step is as follows:
The observation of character, step is:
[character] this product is the concentrated pill of yellowish-brown; Feeble QI perfume (or spice), acrid in the mouth, little hardship;
The discriminating of content, step is:
This product is got in [discriminating] (1), and put microscopically and observe, starch grain simple grain similar round, flat avette, the square circle, diameter 6～35 μ m, omphalion point-like, herringbone shape, crosswise or short seam shape, laminated striation mays be seen indistinctly; Irregular agglomerate or irregular lamellar, faint yellow or closely colourless, be cullet quarrel sample, corner angle are clearly demarcated, the visible wire stricture of vagina reason that has;
(2) get this product, porphyrize takes by weighing about 8g, add chloroform 50ml, refluxed 1 hour, filter, discard filtrate, filtering residue volatilizes chloroform, adds methanol 50ml reflux, extract, 1 hour, filter, filtrate evaporate to dryness, residue add an amount of dissolve with methanol, be added on the neutral alumina post (100-120 order, 5g, internal diameter 10-15mm), with 40% methanol 100ml methanol-eluted fractions, collect eluent, evaporate to dryness, residue adds water 20ml makes dissolving, extracts 2 times with water saturated n-butyl alcohol jolting, each 20ml, merge n-butyl alcohol liquid, ammonia solution washing with 3 times discards ammonia solution, n-butyl alcohol liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets the Ginsenoside Rb
1, panaxoside Rg
1Reference substance adds methanol respectively and makes 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 need testing solution 5 μ l reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launches, and takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ to be heated to the speckle colour developing clear, puts respectively under daylight and the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color;
(3) get this product, porphyrize takes by weighing about 8g, adds methanol 30ml merceration 1 hour, filters, and filtrate evaporate to dryness, residue add methanol 1ml dissolving, and as need testing solution, other gets the puerarin reference substance, adds methanol and makes 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 need testing solution 5 μ l and reference substance solution 2 μ l, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launch, take out, dry, under ultra-violet lamp (365nm), inspect; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(4) get this product, porphyrize takes by weighing about 8g, add chloroform 50ml, refluxed 1 hour, filter, residue volatilizes chloroform, adds methanol 50ml reflux, extract, 1 hour, filters, evaporate to dryness, residue is dissolved in water, and extracts 2 times with water saturated n-butyl alcohol liquid, each 20ml discards water liquid, the ammonia solution washing that n-butyl alcohol liquid reuse is 3 times, with n-butyl alcohol liquid evaporate to dryness, residue adds the 1ml dissolve with methanol as need testing solution; Other gets the astragaloside reference substance, adds methanol and makes 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 each 5 μ l of need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate, with chloroform-methanol-water (65: 35: 10) subnatant is developing solvent, launch, take out, dry, spray is with 10% ethanol solution of sulfuric acid, and 105 ℃ are heated to clear spot; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the speckle of same color; Place again under the ultra-violet lamp (365nm) and inspect, in the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color;
(5) get this product, porphyrize takes by weighing about 40g, adds chloroform 80ml reflux, extract, 1 hour, filter, filtrate is washed with 1% sodium hydroxide solution 50ml, discards sodium hydroxide solution, with chloroform liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, as need testing solution; Other gets Fructus Schisandrae Chinensis control medicinal material 1g, water decocts twice, merge water liquid, extract with the jolting of 20ml chloroform, discard water liquid, chloroform extraction liquid washs with 1% sodium hydroxide solution 20ml, discard sodium hydroxide solution, with chloroform extraction liquid evaporate to dryness, residue adds methanol 1ml makes dissolving, in contrast medical material solution; Test according to thin layer chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005), draw need testing solution 15 μ l and control medicinal material solution 5 μ l, putting respectively on same silica gel 6F254 lamellae, is developing solvent with toluene-ethyl acetate (6: 4), launches, take out, dry, put under the ultra-violet lamp (254nm) and inspect, 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] should meet every regulation relevant under the pill item (appendix IA of Chinese Pharmacopoeia version in 2005);
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (Chinese Pharmacopoeia appendix VI D in 2005);
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica; Methanol-water (20: 80)
Be mobile phase; The detection wavelength is 250nm; Column temperature is 30 ℃; Number of theoretical plate calculates by puerarin peak should be not less than 4000;
It is an amount of that the preparation precision of reference substance solution takes by weighing the puerarin reference substance, adds 30% ethanol and make the solution that contains puerarin 50 μ g among every 1ml, shakes up, promptly;
This product under the weight differential item is got in the preparation of need testing solution, is ground into fine powder, gets about 4.0g, the accurate title, decide, and puts in the conical flask, the accurate 30% ethanol 50ml that adds, claim to decide weight, supersound extraction 30 minutes is put cold, claim to decide weight again, supply the weight that subtracts mistake with 30% ethanol, shake up, filter, get subsequent filtrate, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly;
The every gram of this product contains Radix Puerariae with puerarin (C
21H
20O
9) meter, must not be less than 0.46mg.
According to the method for claim 1, it is characterized in that 5, described TANGNIAOLE preparation is to be made by the raw material of Chinese medicine of following weight:
Radix Trichosanthis 104.3g Rhizoma Dioscoreae 104.3g Radix Astragali 26g
Radix Ginseng Rubra 15.65g Radix Rehmanniae 26g Fructus Lycii 15.65g
Rhizoma Anemarrhenae 15.65g Radix Asparagi 7.8g Poria 10.5g
Fructus Corni 10.5g Fructus Schisandrae Chinensis 7.8g Radix Puerariae 10.5g
Endothelium Corneum Gigeriae Galli (stir-fry) 10.5g.
6, according to the method for claim 1, it is characterized in that, wherein said TANGNIAOLE preparation is by raw material of Chinese medicine is processed through extraction or other modes, make pharmaceutically active substance, subsequently, be raw material with this 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.
According to the method for claim 6, it is characterized in that 7, wherein said TANGNIAOLE preparation is a concentrated pill.
According to the method for claim 7, it is characterized in that 8, wherein said concentrated pill is by preparing through following method: get Rhizoma Dioscoreae 52.15g, Radix Trichosanthis 52.15g, Endothelium Corneum Gigeriae Galli, Radix Ginseng Rubra, be ground into fine powder; All the other Rhizoma Dioscoreae 52.15g, Radix Trichosanthis 52.15g, the Radix Astragali, the Radix Rehmanniae, Fructus Corni, Fructus Lycii, Fructus Schisandrae Chinensis, the Rhizoma Anemarrhenae, Radix Puerariae, Radix Asparagi, Poria decoct with water and add 10 times of water gagings decoctions 2 hours for the first time, adding for the second time 8 times of water gagings decocted 2 hours, collecting decoction, filter, filtrate is concentrated into relative density and is about 1.30 (50 ℃) thick paste; With Rhizoma Dioscoreae, Radix Trichosanthis, Endothelium Corneum Gigeriae Galli, Radix Ginseng Rubra fine powder, mixing is made 1000 balls, drying, and polishing, promptly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610065643XA CN100478683C (en) | 2006-03-23 | 2006-03-23 | Quality control method for diabetes treating Tangniaole bolus |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB200610065643XA CN100478683C (en) | 2006-03-23 | 2006-03-23 | Quality control method for diabetes treating Tangniaole bolus |
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|---|---|
| CN1857591A true CN1857591A (en) | 2006-11-08 |
| CN100478683C CN100478683C (en) | 2009-04-15 |
Family
ID=37296579
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB200610065643XA Expired - Fee Related CN100478683C (en) | 2006-03-23 | 2006-03-23 | Quality control method for diabetes treating Tangniaole bolus |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008153502A1 (en) * | 2007-06-08 | 2008-12-18 | Eu Yan Sang International Ltd | Compositions for prevention and/or treatment of diabetes |
| CN102614378A (en) * | 2012-04-26 | 2012-08-01 | 陕西方舟制药有限公司 | Yin nourishing and blood sugar lowering Chinese medicinal composition and preparation method as well as detection method thereof |
| CN106770882A (en) * | 2016-12-14 | 2017-05-31 | 四川新绿色药业科技发展有限公司 | A kind of detection method of the Chinese medicine preparation containing ginseng or pseudo-ginseng |
-
2006
- 2006-03-23 CN CNB200610065643XA patent/CN100478683C/en not_active Expired - Fee Related
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008153502A1 (en) * | 2007-06-08 | 2008-12-18 | Eu Yan Sang International Ltd | Compositions for prevention and/or treatment of diabetes |
| CN102614378A (en) * | 2012-04-26 | 2012-08-01 | 陕西方舟制药有限公司 | Yin nourishing and blood sugar lowering Chinese medicinal composition and preparation method as well as detection method thereof |
| CN106770882A (en) * | 2016-12-14 | 2017-05-31 | 四川新绿色药业科技发展有限公司 | A kind of detection method of the Chinese medicine preparation containing ginseng or pseudo-ginseng |
| CN106770882B (en) * | 2016-12-14 | 2018-02-13 | 四川新绿色药业科技发展有限公司 | A kind of detection method of the Chinese medicine preparation containing ginseng or pseudo-ginseng |
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| Publication number | Publication date |
|---|---|
| CN100478683C (en) | 2009-04-15 |
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Address after: 1266 No. 330052 Nanchang Huiren Jiangxi economic and Technological Development Zone Avenue. Patentee after: JIANGXI HUIREN PHARMACEUTICAL CO.,LTD. Address before: 330043 1189 Yingbin Avenue, Nanchang, Jiangxi Patentee before: Jiangxi Huiren Pharmaceutical Co.,Ltd. |
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