CN1857588A - Quality control method for Xianlinggubao preparation - Google Patents
Quality control method for Xianlinggubao preparation Download PDFInfo
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- CN1857588A CN1857588A CN 200610065646 CN200610065646A CN1857588A CN 1857588 A CN1857588 A CN 1857588A CN 200610065646 CN200610065646 CN 200610065646 CN 200610065646 A CN200610065646 A CN 200610065646A CN 1857588 A CN1857588 A CN 1857588A
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Abstract
The present invention relates to quality control method for Xianlinggubao preparation. 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 XIANLING GUBAO pill.
Background technology:
XIANLING GUBAO JIAONANG is the medicine of existing treatment osteoporosis, osteoporosis is that the osseous tissue total amount is the absolute minimizing of bone amount in the unit volume, and the structural change of bone and function are changed, thus skeleton pain around occurring, symptoms such as figure's distortion, and the pathological changes of easily generation fracture.Osteoporosis is a kind of very serious, and may fatal diseases, and suffer from this sick number and reaches several hundred millionly approximately in the world at present, and this disease reaches an advanced stage; It is fragile unusually that osseous tissue can become, and turns over body or in bed and all might fracture even cough.Estimate that according to the U.S.'s osteoporosis foundation female patient finally reaches 20% because of the wide articular fracture of bone is lethal, its medical expense also is quite high, and only in the U.S., the medical fee of being spent in a year just reaches 70 ~ 10,000,000,000,000 dollars.Along with the arrival of aging society, the sickness rate of primary osteoporosis obviously rises, and osteoporotic fracture becomes clinical common injury disease, very easily causes bone delay in healing and disunion and disables.Its pathogenic factor it is generally acknowledged and calcium or malnutrition that factors such as endocrine dysfunction and hypomotility are relevant.Though Chinese scholars proposes many therapeutic schemes, do not obtain highly effective treatment measure up to now yet.
Chinese medicine is thought " the kidney being the origin of congenital constitution ", " main bone give birth to marrow ", and deficiency of kidney-QI then muscles and bones is abundant, and the kidney qi bone that declines then is withered and marrow subtracts.Male eight woman seven of " element asks ancient times exceedingly high opinion " more direct description are for the radix age increases progressively the positive relation of the sx of suffering from a deficiency of the kidney, propose " woman seventy-seven, exhaustion of kidney-essence with promoting reproductive function and senile appearance, the man seven or eight, exhaustion of kidney-essence with promoting reproductive function ... kidney declines and physique and configuration of the body being very feeble and atrophied ".Illustrate bone growth, growth, powerfully weakly direct substantial connection is arranged with the kidney essense prosperity and decline, then bone marrow biochemistry is passive for deficiency of kidney-essence, bone loses to moisten and supports and flaccidity is weak unable.
Modern medicine study confirms, the patient's that suffers from a deficiency of the kidney hypothalamic pituitary gonadal axis hypofunction.Cause osteogenesis function and descend, the unit volume osseous tissue reduces and causes osteoporosis.With trace element change in hormonal system dysfunction, immunologic hypofunction and the body in the body direct relation is arranged, primary osteoporosis comprises postmenopausal osteoporosis and senile osteoporosis, the former is mainly due to estrogen deficiency, the bone resorption hyperfunctioning of osteoclast, belong to hypermetabolism conversion type osteoporosis, the latter is aging mainly due to osteoblast, due to the functional defect, belongs to low metabolism conversion type osteoporosis.The phenomenon of suffering from a deficiency of the kidney is in various degree all arranged clinically, and its bone density is all obviously low, so the just saying of " the nephrasthenia syndrome bone density is lowly " is arranged.
In recent years studies confirm that; kidney-nourishing tcm drug passability hormone-like effect; be enhanced to the balance that osteocyte is active and regulate body bone environment and trace element; promote mineral in bone deposition and bring into play osteoporosis; promote the growth of spur effect; so clinically multiselect with the product of going into kidney channel for first choice of taking orally; the XIANLING GUBAO FENSANPIAN main component is by Herba Epimedii; Radix Dipsaci; medicines such as Fructus Psoraleae are formed; the kidney-nourishing tcm drug Herba Epimedii of going into the warp of Liver and kidney with Xin Ganwen in the side is a principal agent; can directly increase the osteoblast activity; promote osteoblast regeneration; can pass through the protectiveness glandular tissue and the maintenance hormonal readiness again; also can accelerate the metabolic activity of callus tissue; the mineralising of callus is shifted to an earlier date; mould quickening again; the Radix Dipsaci that cooperates liver and kidney tonifying again; reunion of bone; promoting blood circulation and pain relieving; the weakness of the waist and knees of the tonification insufficiency of kidney-YANG of Fructus Psoraleae; three medicines share; healing time is shortened; pharmacological evaluation confirms, takes this medicine and can make whole bone amount; bone mineral content increases, and makes the constituent ratio of bone calcium and organic matrix approaching to normal level; thereby regulate the metabolism disorder of body better; reverse the high turnover state, reach the treatment of fractures purpose that osteoporosis is caused.
XIANLING GUBAO ball (concentrated pill) is the kind that develops through reform on the basis of original capsule type, and existing XIANLING GUBAO ZHIJI 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 XIANLING GUBAO ZHIJI, 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 XIANLING GUBAO ZHIJI, 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 XIANLING GUBAO ZHIJI.
The XIANLING GUBAO ZHIJI prescription consists of:
[prescription] Herba Epimedii 350.1g Radix Dipsaci 50.1g Radix Salviae Miltiorrhizae 24.9g
Rhizoma Anemarrhenae 24.9g Fructus Psoraleae 24.9g Radix Rehmanniae 24.9g
XIANLING GUBAO ball (concentrated pill) method for making is as follows: above Six-element, Radix Dipsaci, Radix Salviae Miltiorrhizae, Fructus Psoraleae are ground into fine powder, and three flavors such as all the other Herba Epimedii decoct with water each one hour three times, collecting decoction, being concentrated into relative density is that 1.35～1.38 (30 ℃) get thick paste, adds above-mentioned fine powder, mixing, make 1000 balls, drying, polishing, promptly.
The present invention be directed to XIANLING GUBAO ball (concentrated pill) preparation and propose method of quality control, but also be not limited to XIANLING GUBAO ball (concentrated pill) preparation, also can comprise other oral formulations of XIANLING GUBAO such as tablet, capsule, syrup, granule.
Its prescription of other dosage forms of the XIANLING GUBAO that the present invention includes is identical with XIANLING GUBAO 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 XIANLING GUBAO 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 XIANLING GUBAO 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.
XIANLING GUBAO ZHIJI of the present invention, particularly concentrated pill preparation, it is as follows that its function cures mainly usage and dosage:
[function with cure mainly] nourishing the liver and kidney, promoting blood circulation to remove obstruction in the collateral, bone and muscle strengthening.Be used for deficiency of the liver and kindey, osteoporosis due to the obstruction of collaterals by blood stasis.
[usage and consumption] is oral, one time 10 ball, and 2 times on the one, 4～6 weeks were a course of treatment, or followed the doctor's advice.
Should not take during [attention] severe cold.
[specification] per 10 balls are equivalent to crude drug 5 grams.
[storage] sealing.
[effect duration] 2 years.
The present invention is to provide the method for quality control at above XIANLING GUBAO ZHIJI, particularly the concentrated pill preparation is the quality of control XIANLING GUBAO ZHIJI.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 tan concentrated pill, mildly bitter flavor.
The discriminating of content, step is:
This product is got in [discriminating] (1), and put microscopically and observe: calcium oxalate cluster crystal is present in the parenchyma cell of light brown yellow shrinkage, and constant is individual to be arranged in rows.Stone cell is near colourless or faint yellow, similar round, class triangle, rectangle like or irregular shape, diameter 20～65 μ m, edge out-of-flatness.Plant skin palisade cells light brown or rufous, the class polygon is seen on the surface, and wall is thick slightly, and cell contains the rufous thing.
(2) get this product 2g, porphyrize adds dehydrated alcohol 30ml, and supersound process 60 minutes filters, and filtrate is concentrated into 1ml, and as need testing solution, other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel G plate, is developing solvent with toluene-ethyl acetate (19: 1), launches, take out, dry, inspect under the daylight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) get this product 1.5g, porphyrize adds ethyl acetate 20ml, supersound process 5 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution, other gets psoralen, the isopsoralen reference substance adds ethyl acetate and makes the solution that every 1ml contains 0.4mg, in contrast product solution, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 10 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 10% potassium hydroxide methanol solution.In the test sample chromatograph, with the corresponding position of reference substance 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 (an appendix I of Chinese Pharmacopoeia version in 2005 A)
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (appendix VII of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and acetonitrile-water acid (25: 75) is mobile phase, and the detection wavelength is 270nm.Column temperature: 30 ℃.Number of theoretical plate calculates by the icariin peak should be not less than 2500.
It is an amount of that the preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and make the solution that every 1ml contains 0.10mg, promptly.
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got about 0.20g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 10ml that adds, claim to decide weight, supersound process (power 250W, frequency 25KHZ) 1 hour, put coldly, claim again to decide weight, supply with methanol and subtract weight loss, 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 Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 2.4mg.
The present invention changes agent on former dosage form basis, simultaneously production technology reformed,
Mainly reform around extracting solvent load and concentrated pill molding technological condition.
(1), medical material is identified and pre-treatment
Prescription with crude drug source and appraisal basis referring to No. 8 data.
(2), Study on extraction
This product kind changes the domestic pharmaceutical formulation of list marketing kind, and technology does not have the change of matter, we at former extraction process by water only clear and definite isoparametric situation of extraction time, extraction time, investigated of the influence of solvent different amounts to result of the test.
1, extracts
By former prescription, get Herba Epimedii, the Rhizoma Anemarrhenae, Radix Rehmanniae, decoct with water three times, each 1 hour, collecting decoction filtered, and enters separation, enrichment process.
Each time amount of water is investigated in test, is evaluation index with each time test dry extract amount (leaching amount), extracting solution with the icariin rate of transform.
Experimental technique:
(1) sample preparation: take by weighing totally three parts of Herba Epimedii 350.1g, Rhizoma Anemarrhenae 24.9g, Radix Rehmanniae 24.9g, add 8 times, 10 times, 12 times decoctings respectively and boil three times, each 1 hour, collecting decoction filtered, and filtrate concentrates, and the drying under reduced pressure powder that gets dry extract is weighed, and is standby.
(2) investigate index: principal agent in the Herba Epimedii side of being, its main constituent are compositions such as icariin.In order to investigate and estimate the extraction process quality, we select to measure, and icariin content is index in the dried cream, determines the extraction process by water condition according to dried cream yield simultaneously.
(3) assay method
Chromatographic condition is a filler with octadecyl silicon bonded silica gel, and acetonitrile-water (25: 75) is a mobile phase, and the detection wavelength is 270nm, flow velocity: 1ml/min, column temperature: 30 ℃.
The preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and makes the solution that every 1ml contains 0.1mg, promptly.
It is an amount of that dried cream powder is got in the preparation of need testing solution, porphyrize, and precision claims to conclude a contract or treaty puts 0.1g in the tool plug conical flask, accurate methanol 10ml, the close plug of adding, claim decide weight, supersound process 1 hour is taken out, and puts coldly, and weight decided in title again, supply the weight that subtracts mistake with methanol, shake up, filter, get subsequent filtrate, promptly.
Accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, and, see Table 1 that is.
Table 1 solvent different amounts is investigated result of the test
| Solvent load (doubly) | Inventory (g) | Dried cream (g) | Dried cream yield (%) | Icariin content (mg/g) in the extractum | The icariin rate of transform (%) |
| 8 10 | 399.9 399.9 | 66.0 74.0 | 16.50 18.50 | 26.24 25.56 | 51.69 56.45 |
| 12 | 399.9 | 79.8 | 19.95 | 24.05 | 57.28 |
By above result as seen, solvent load extracts and extracts with 12 times of water gagings icariin rate of transform influence little (only differing 0.8%) with 10 times of water gagings, promptly use the water extracting component of 10 times of amounts more complete, according to energy-conservation principle and the practical situation that reduces production costs, we determine that solvent load uses 10 times of amounts for the first time, with 10 times of amounts, use 8 times of amounts for the third time for the second time.
2, separate
XIANLING GUBAO ball (concentrated pill) is a pill, and characteristics are oral administration.By the trial test result, the dosage that calculates expection according to solid yield conforms to substantially, for keeping effective ingredient as much as possible, saves cost, so do not consider to make with extra care.For improving the filtration effect of extracting solution, reduce loss, according to existing equipment, after extracting, select medicinal residues the slagging-off of filtration method for use.Be merge extractive liquid,, filter, change enrichment process over to 200 order filter clothes.
3, concentrate
According to former preparation process, filtrate decompression is condensed into the thick paste that relative density is 1.30～1.38 (30 ℃), enters the concentrated pill molding procedure.
(3), disintegrating process research
The research dosage form is a concentrated pill, and Radix Dipsaci, Radix Salviae Miltiorrhizae, Fructus Psoraleae etc. are pulverized according to former prescription and former dosage form technology and are fine powder in the prescription, with the mixed system of extracting solution thick paste soft material, enter the concentrated pill molding procedure then.
Test shows that Radix Dipsaci, Radix Salviae Miltiorrhizae, Fructus Psoraleae are pulverized to such an extent that the powder rate is satisfied, see Table 3.
Table 3 pulverizing medicinal materials gets the powder rate and investigates (%)
| Medical material | Weight (g) before pulverizing | Pulverize back weight (g) | Get powder rate (%) | Average yield (%) |
| Radix Dipsaci | 100 100 100 | 97.05 97.23 96.14 | 97.05 97.23 96.14 | 96.81 |
| Radix Salviae Miltiorrhizae | 100 100 100 | 96.22 97.02 96.69 | 96.22 97.02 96.69 | 96.44 |
| Fructus Psoraleae | 100 100 100 | 95.54 96.65 95.73 | 95.54 96.65 95.73 | 95.97 |
(4), moulding process
Get the extracting solution thick paste, (ratio of extractum and medicated powder was near 1: 1 in this prescription and the method for making for fine powder, the preparation concentrated pill is comparatively desirable, hardly with adding binding agent or diluent, therefore according to concentrated pill routine operation pill), make soft material with trough type mixing machine, with the pellet processing machine pill, ball cutter and the diameter that goes out the ball plate are 6.5mm, 60 ℃ of dryings 4 hours, upper strata diameter 6.6mm, lower floor be with the vibration ball of 6.4mm sieve sieve ball, adds an amount of 75% ethanol glazing, 60 ℃ of dryings 24 hours, control ball moisture is less than 7%.Upper strata diameter 6.6mm, the selected qualified concentrated pill that gets sieves with the vibration ball of 6.4mm in lower floor, packing, promptly.
Conclusion:
Above Six-element, Radix Dipsaci, Radix Salviae Miltiorrhizae, Fructus Psoraleae are ground into fine powder, and three flavors such as all the other Herba Epimedii decoct with water each one hour three times, collecting decoction, being concentrated into relative density is that 1.35～1.38 (30 ℃) get thick paste, adds above-mentioned fine powder, mixing, make 1000 balls, drying, polishing, promptly.
14.2 the testing data of quality research work
14.2.1 differentiate
14.2.1.1 differentiate the microscopical identification of Radix Dipsaci, Radix Salviae Miltiorrhizae, Fructus Psoraleae in (1) side of being
Get this product, put microscopically and observe: calcium oxalate cluster crystal is present in the parenchyma cell of light brown yellow shrinkage, and constant is individual to be arranged in rows.Stone cell is near colourless or faint yellow, similar round, class triangle, rectangle like or irregular shape, diameter 20～65 μ m, edge out-of-flatness.Plant skin palisade cells light brown or rufous, the class polygon is seen on the surface, and wall is thick slightly, and cell contains the rufous thing.Consistent with former XIANLING GUBAO JIAONANG microscopic features.
14.2.1.2 differentiating the thin layer of Radix Salviae Miltiorrhizae in (2) side of being differentiates
We serve as that Study on Identification is carried out in contrast with the Radix Salviae Miltiorrhizae control medicinal material, make negative control simultaneously, and the result shows that 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.
14.2.13 differentiating the thin layer of Fructus Psoraleae medical material in (3) side of being differentiates
We serve as that Study on Identification is carried out in contrast with psoralen, isopsoralen 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 other
14.2.1.4.1 the Study on Identification of Radix Dipsaci
Once the method on the reference literature in the experiment, adopted multiple extraction solvents such as chloroform to handle sample with different sample treatments, screened different developing solvents, but all do not occur and the corresponding speckle of control medicinal material in the gained test sample chromatograph, and disturb very big, so we do not include its discriminating in this product quality standard in temporarily.
14.2.1.3.2 the Study on Identification of Radix Rehmanniae
We serve as that the thin layer Study on Identification has been carried out in contrast with reference to diplomatic method with the Radix Rehmanniae control medicinal material in the experiment, all do not occur and the corresponding speckle of control medicinal material in the gained test sample chromatograph as a result, so this discriminating is not included in this product quality standard.
14.2.1.4.3 the Study on Identification of the Rhizoma Anemarrhenae
We are with reference to diplomatic method in the experiment, with Rhizoma Anemarrhenae control medicinal material serves as that the thin layer Study on Identification has been carried out in contrast, the speckle separation is bad in the gained test sample chromatograph as a result, and in the chromatograph of negative sample interference is arranged, so we do not include its discriminating in this product quality standard in temporarily.
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 one appendix I A 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 one appendix I A 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
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 2/1000000ths, so quality standard is not included in an inspection 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
XIANLING GUBAO ball (concentrated pill) is made by medical materials such as Herba Epimedii, and Herba Epimedii is monarch drug and consumption maximum in the side, and tool kidney-replenishing, bone and muscle strengthening, wind-damp dispelling are used for diseases such as impotence and seminal emission, muscles and bones flaccidity be soft.The master contains icariin in the epimedium herb, and the assay item is testing index with the icariin in the original capsule standard, and mobile phase is methanol: 1.5% glacial acetic acid (60: 40).Through experiment, we find that the content assaying method in the original capsule standard is not suitable for this kind, and experimentize by the method for an epimedium herb of Chinese Pharmacopoeia version in 2000 again, and just the proportioning of mobile phase need be done an adjustment, investigate through methodology, this method is accurately feasible.
14.2.7.1 instrument and reagent
Instrument: waters2695 type high performance liquid chromatograph, waters2487 UV-detector;
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: acetonitrile is a chromatographically pure, and methanol is analytical pure.
Reference substance: the icariin reference substance (is identified lot number: 110737-200312) XIANLING GUBAO ball (concentrated pill): Jiangxi Huiren Pharmaceutical Co., Ltd's self-control available from Chinese pharmaceutical biological product
Research lot number: 20040901,20040902,20040903
14.2.7.2 detection wavelength determination
The detection wavelength of icariin is 270nm in the primary standard, still to select to detect wavelength be 270nm.
14.2.7.3 chromatographic condition
Mobile phase: acetonitrile-water (25: 75), flow velocity: 1ml/min detects wavelength: 270nm, column temperature: 30 ℃.Other composition is noiseless to icariin under this condition, can reach effective separation, and theoretical cam curve is calculated as 6104 by the icariin peak
14.2.7.4 negative sample test
Prepare the sample that does not contain Herba Epimedii by prescription and production technology, press the test of text content assaying method, the result does not see interference at place, icariin peak.
14.2.7.5 the investigation of linear relationship
Precision takes by weighing icariin reference substance 11.28mg and puts in the 100ml measuring bottle, add dissolve with methanol and be diluted to scale, shake up, therefrom accurate respectively again absorption 2 μ l, 5 μ l, 10 μ l, 20 μ l, 50 μ l inject chromatograph of liquid, the record chromatogram, with the peak area is vertical coordinate, sample size is an abscissa, the drawing standard curve, get regression equation: y=2E+06x, R=0.9999 (n=5), result show that icariin peak area integrated value and sample size in the sample size scope of 0.2256～5.64 μ g are good linear relationship, and determination data sees Table 14-5.
Table 14-5 icariin standard curve
| Sequence number | 1 | 2 | 3 | 4 | 5 |
| Sample size (μ g) peak area average peak area | 0.2256 504093 514088 505090.5 | 0.564 1314512 1395993 1355253 | 1.128 2689679 2626059 2657869 | 2.256 5241880 5270229 5256055 | 5.64 12959490 12992170 12975830 |
Figure 14-5 icariin standard curve
14.2.7.6 precision test
The same reference substance solution 10 μ l of accurate respectively absorption, continuous sample introduction 6 times is measured, and the record peak area the results are shown in Table 14-6, and RSD is 0.4%.
The test of table 14-6 precision
| The sample introduction number of times | The reference substance solution peak area value | RSD(％) |
| 1 2 3 4 5 6 | 2576571 2593055 2591609 2610779 2599798 2598768 | 0.4 |
14.2.7.7 need testing solution study on the stability
(lot number: 20040901) measured respectively in 0,1,2,4,8,12 hour, RSD is 0.9% as a result, shows that need testing solution is stable in 12 hours, sees Table 14-7 to get need testing solution.
Table 14-7 need testing solution stability test
| Standing time (hour) | Peak area | RSD(％) |
| 0 1 2 4 8 12 | 6733670 6628218 6718004 6941766 7046156 6893940 | 2.12 |
14.2.7.8 reference substance solution study on the stability
Get the icariin reference substance and measured respectively in 0,1,2,4,8,12 hour, RSD is 0.9% as a result, shows that sample solution is stable in 12 hours, sees Table 14-8.
Table 14-8 reference substance solution stability test
| Standing time (hour) | Peak area | RSD(％) |
| 0 1 2 4 8 12 | 2607778 2650053 2683451 2663444 2662402 2681053 | 0.95 |
14.2.7.9 replica test
Get same lot number sample (lot number: 20040901) totally 6 parts, measure according to content assaying method in the text, the results are shown in Table 14-9.
Table 14-9 replica test
| Sequence number | Content (mg/g) | Average content (mg/g) | RSD(％) |
| 1 2 3 4 5 6 | 8.61 8.73 8.49 8.46 8.51 8.43 | 8.54 | 1.20 |
14.2.7.10 average recovery test
Get known content this product (lot number: 20040901) an amount of, porphyrize, precision takes by weighing in right amount, totally 6 parts, accurately respectively add a certain amount of icariin reference substance, according to content assaying method mensuration in the text, calculate recovery rate and RSD the results are shown in Table 14-10.
Table 14-10 application of sample recovery test
| Sample weighting amount (mg) | Content in the sample (mg) | Add reference substance amount (mg) | Measured value (mg) | The response rate (%) | Average recovery rate (%) | RSD (％) |
| 106.09 | 0.9018 | 1.061 | 1.956 | 99.65 | 98.51 | 1.19 |
| 107.99 99.94 102.92 112.57 109.65 | 0.9179 0.8495 0.8748 0.9569 0.9320 | 1.061 1.061 1.061 1.061 1.061 | 1.931 1.895 1.868 1.985 1.988 | 97.58 99.19 96.50 98.37 99.75 |
14.2.7.10 sample determination
Measure 10 batch samples respectively by the text content assaying method, the results are shown in Table 14-11.
Table 14-11 sample determination result
| The sample lot number | Icariin content (mg/g) | Average content (mg/g) | |
| 20,040,901 20,040,902 20,040,903 20,041,012 20,041,013 20,041,014 20,041,015 20,051,125 20,051,126 20051127 mean values (mg/g) | 8.3 7.1 7.2 5.9 5.7 6.8 6.3 11.2 11.3 9.5 | 8.7 7.5 7.0 5.3 6.1 6.6 6.7 11.0 11.7 10.1 | 8.5 7.3 7.1 5.6 5.9 6.7 6.5 11.1 11.5 9.8 8.0 |
According to above measurement result, consider the diversity of medical material and the difference of operation, we draft the every gram of this product and contain Herba Epimedii with icariin (C with reference to the standard of former XIANLING GUBAO JIAONANG
33H
40O
15) meter, must not be less than 2.4mg.
More than this product described in the method for quality control of the present invention, be meant XIANLING GUBAO 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 XIANLING GUBAO ball (concentrated pill)
Method of quality control of the present invention may further comprise the steps:
The observation of character, step is:
[character] this product is that pale brown color is to tan concentrated pill, mildly bitter flavor.
The discriminating of content, step is:
This product is got in [discriminating] (1), and put microscopically and observe: calcium oxalate cluster crystal is present in the parenchyma cell of light brown yellow shrinkage, and constant is individual to be arranged in rows.Stone cell is near colourless or faint yellow, similar round, class triangle, rectangle like or irregular shape, diameter 20～65 μ m, edge out-of-flatness.Plant skin palisade cells light brown or rufous, the class polygon is seen on the surface, and wall is thick slightly, and cell contains the rufous thing.
(2) get this product 2g, porphyrize adds dehydrated alcohol 30ml, and supersound process 60 minutes filters, and filtrate is concentrated into 1ml, and as need testing solution, other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, shines medical material solution in pairs with legal system.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel G plate, is developing solvent with toluene-ethyl acetate (19: 1), launches, take out, dry, inspect under the daylight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
(3) get this product 1.5g, porphyrize adds ethyl acetate 20ml, supersound process 5 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution, other gets psoralen, the isopsoralen reference substance adds ethyl acetate and makes the solution that every 1ml contains 0.4mg, in contrast product solution, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 10 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 10% potassium hydroxide methanol solution.In the test sample chromatograph, with the corresponding position of reference substance 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 (an appendix I of Chinese Pharmacopoeia version in 2005 A)
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (appendix VII of Chinese Pharmacopoeia version in 2005).
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and acetonitrile-water acid (25: 75) is mobile phase, and the detection wavelength is 270nm.Column temperature: 30 ℃.Number of theoretical plate calculates by the icariin peak should be not less than 2500.
It is an amount of that the preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and make the solution that every 1ml contains 0.10mg, promptly.
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got about 0.20g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 10ml that adds, claim to decide weight, supersound process (power 250W, frequency 25KHZ) 1 hour, put coldly, claim again to decide weight, supply with methanol and subtract weight loss, 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 Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 2.4mg.
The preparation of embodiment 2 XIANLING GUBAO balls (concentrated pill)
[prescription] Herba Epimedii 350.1g Radix Dipsaci 50.1g Radix Salviae Miltiorrhizae 24.9g
Rhizoma Anemarrhenae 24.9g Fructus Psoraleae 24.9g Radix Rehmanniae 24.9g
XIANLING GUBAO ball (concentrated pill) method for making is as follows: above Six-element, Radix Dipsaci, Radix Salviae Miltiorrhizae, Fructus Psoraleae are ground into fine powder, and three flavors such as all the other Herba Epimedii decoct with water each one hour three times, collecting decoction, being concentrated into relative density is that 1.35～1.38 (30 ℃) get thick paste, adds above-mentioned fine powder, mixing, make 1000 balls, drying, polishing, promptly.
Claims (8)
1, a kind of method of quality control of XIANLING GUBAO ZHIJI 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 XIANLING GUBAO ZHIJI is an oral solid formulation.
3, the method for claim 2 is characterized in that, described oral solid formulation is the XIANLING GUBAO 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 that pale brown color is to tan concentrated pill, mildly bitter flavor;
The discriminating of content, step is:
This product is got in [discriminating] (1), and put microscopically and observe: calcium oxalate cluster crystal is present in the parenchyma cell of light brown yellow shrinkage, and constant is individual to be arranged in rows; Stone cell is near colourless or faint yellow, similar round, class triangle, rectangle like or irregular shape, diameter 20～65 μ m, edge out-of-flatness; Plant skin palisade cells light brown or rufous, the class polygon is seen on the surface, and wall is thick slightly, and cell contains the rufous thing;
(2) get this product 2g, porphyrize adds dehydrated alcohol 30ml, and supersound process 60 minutes filters, and filtrate is concentrated into 1ml, and as need testing solution, other gets Radix Salviae Miltiorrhizae control medicinal material 0.5g, shines medical material solution in pairs with legal system; Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw each 10 μ l of above-mentioned two kinds of solution, putting respectively on same silica gel G plate, is developing solvent with toluene-ethyl acetate (19: 1), launches, take out, dry, inspect under the daylight, in the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color;
(3) get this product 1.5g, porphyrize adds ethyl acetate 20ml, supersound process 5 minutes, filter, filtrate evaporate to dryness, residue add ethyl acetate 1ml makes dissolving, as need testing solution, other gets psoralen, the isopsoralen reference substance adds ethyl acetate and makes the solution that every 1ml contains 0.4mg, in contrast product solution, test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B), draw need testing solution 10 μ l, reference substance solution 5 μ l put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (4: 1) is developing solvent, launch, take out, dry, spray is put under the ultra-violet lamp (365nm) and is inspected with 10% potassium hydroxide methanol solution; In the test sample chromatograph, with the corresponding position of reference substance 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 (an appendix I of Chinese Pharmacopoeia version in 2005 A)
The composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (appendix VII of Chinese Pharmacopoeia version in 2005);
Chromatographic condition and system suitability test are filler with octadecylsilane chemically bonded silica, and acetonitrile-water acid (25: 75) is mobile phase, and the detection wavelength is 270nm; Column temperature: 30 ℃; Number of theoretical plate calculates by the icariin peak should be not less than 2500;
It is an amount of that the preparation precision of reference substance solution takes by weighing the icariin reference substance, adds methanol and make the solution that every 1ml contains 0.10mg, promptly;
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got about 0.20g, the accurate title, decide, and puts in the tool plug conical flask, the accurate methanol 10ml that adds, claim to decide weight, supersound process (power 250W, frequency 25KHZ) 1 hour, put coldly, claim again to decide weight, supply with methanol and subtract weight loss, 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 Herba Epimedii with icariin (C
33H
40O
15) meter, must not be less than 2.4mg.
According to the method for claim 1, it is characterized in that 5, described XIANLING GUBAO ZHIJI is to be made by the raw material of Chinese medicine of following weight:
Herba Epimedii 350.1g Radix Dipsaci 50.1g Radix Salviae Miltiorrhizae 24.9g
Rhizoma Anemarrhenae 24.9g Fructus Psoraleae 24.9g Radix Rehmanniae 24.9g
6, according to the method for claim 1, it is characterized in that, wherein said XIANLING GUBAO ZHIJI 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 XIANLING GUBAO ZHIJI 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: Six-element, Radix Dipsaci, Radix Salviae Miltiorrhizae, Fructus Psoraleae are ground into fine powder, and three flavors such as all the other Herba Epimedii decoct with water each one hour three times, collecting decoction, being concentrated into relative density is that 1.35～1.38 (30 ℃) get thick paste, adds above-mentioned fine powder, mixing, make 1000 balls, drying, polishing, promptly.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102343027A (en) * | 2011-10-18 | 2012-02-08 | 贵州同济堂制药有限公司 | Xianlinggubao extract, preparation containing same and preparation method thereof |
| CN103083521A (en) * | 2013-02-20 | 2013-05-08 | 贵州同济堂制药有限公司 | Extraction method, separated extract and preparation of Xianlinggubao |
| CN109709240A (en) * | 2019-01-29 | 2019-05-03 | 北京中研同仁堂医药研发有限公司 | A kind of detection method of traditional Chinese medicine composition and its application |
| CN110057961A (en) * | 2019-05-21 | 2019-07-26 | 国药集团同济堂（贵州）制药有限公司 | A kind of XIANLING GUBAO JIAONANG product inspection method |
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2006
- 2006-03-23 CN CNB2006100656463A patent/CN100533139C/en not_active Expired - Fee Related
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102343027A (en) * | 2011-10-18 | 2012-02-08 | 贵州同济堂制药有限公司 | Xianlinggubao extract, preparation containing same and preparation method thereof |
| CN103083521A (en) * | 2013-02-20 | 2013-05-08 | 贵州同济堂制药有限公司 | Extraction method, separated extract and preparation of Xianlinggubao |
| CN103083521B (en) * | 2013-02-20 | 2015-04-15 | 贵州同济堂制药有限公司 | Extraction method, separated extract and preparation of Xianlinggubao |
| CN109709240A (en) * | 2019-01-29 | 2019-05-03 | 北京中研同仁堂医药研发有限公司 | A kind of detection method of traditional Chinese medicine composition and its application |
| CN109709240B (en) * | 2019-01-29 | 2022-04-26 | 北京中研同仁堂医药研发有限公司 | Detection method and application of traditional Chinese medicine composition |
| CN110057961A (en) * | 2019-05-21 | 2019-07-26 | 国药集团同济堂（贵州）制药有限公司 | A kind of XIANLING GUBAO JIAONANG product inspection method |
| CN110057961B (en) * | 2019-05-21 | 2020-05-19 | 国药集团同济堂（贵州）制药有限公司 | Detection method of Xianlinggubao capsule finished product |
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| CN100533139C (en) | 2009-08-26 |
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