CN100533141C - Detection method for trauma treating Diedahongyao preparation - Google Patents
Detection method for trauma treating Diedahongyao preparation Download PDFInfo
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- CN100533141C CN100533141C CNB2006100656482A CN200610065648A CN100533141C CN 100533141 C CN100533141 C CN 100533141C CN B2006100656482 A CNB2006100656482 A CN B2006100656482A CN 200610065648 A CN200610065648 A CN 200610065648A CN 100533141 C CN100533141 C CN 100533141C
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Abstract
The present invention relates to quality control method for trauma treating Diedahongyao 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 trauma treating Diedahongyao pill.
Background technology:
" trauma treating Diedahongyao " is that the product in the 20th in the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation has promoting blood circulation and stopping pain, the removing blood stasis for promoting tissue regeneration effect.Be used for traumatic injury, muscles and bones blood stasis and swelling pain, rheumatic numbness.
Monarch drug in a prescription pseudo-ginseng removing blood stasis and hemostasis in the side, the analgesic therapy of invigorating blood circulation, the hemostasis and do not stay the stasis of blood, be the regulating blood condition quality goods." pseudo-ginseng and battalion hemostasis, the capable stasis of blood of promoting blood circulation, row hemostasis and hold back new blood in " beautiful Chinese catalpa medicine is separated ".All ... fall beat, too fat to move, all hemostasis are all broken; Knife wound, arrow are penetrated, and all new blood all end." minister is with ground bettle, it is salty, cold to distinguish the flavor of, and goes into the conscience the spleen channel, dissipating blood stasis with potent drugs, and reunion of fractured tendons and bones, " Bencao Jingshu ": " ground bettle is controlled traumatic injury, and continuous muscles and bones has special effect.Be the meridian of Foot-JUE YIN medicine also.Husband's blood person, also Kidney-Yin in the body irrigated bones of the body collectively, and circumfluence channels and collaterals person is also.Blood is if stagnate, channels and collaterals difference then, and usefulness of negative and positive is well-behaved mutually, and here fever and chills wash life.Salty-coldly can go into the soft heavily fortified point of blood, so main trusted subordinate's blood is long-pending ... blood and and battalion defends unobstructedly, passages through which vital energy circulates is mixed well ... " the hot temperature of safflower, go into the heart, liver blood branch, grasp the hot logical property of temperature of loosing, to invigorate blood circulation and moisturize, pain-relieving powder for treating is swollen, and the various stasis syndromes of dispelling; Radix Angelicae Sinensis Gan Xinwen enriches blood, invigorates blood circulation, pain relieving, and be used for hemostasis and have a pain, traumatic injury, the numbness pain is numb; The hot fragrant row of Ligusticum wallichii looses, and warm promoting blood circulation is the gas medicine in the blood, can promoting blood circulation, again can activating QI to alleviate the depression, and the wind-expelling pain-stopping effect is rather good; It is adjutant altogether that three medicines cooperate, to reach the merit of promoting blood circulation to remove blood stasis; Make with the root of Dahurain angelica, Xin Wen reaches on the fragrance, wind-expelling pain-stopping; Cooperate with Ligusticum wallichii, safflower, Radix Angelicae Sinensis, strengthen the merit of promoting blood circulation to remove blood stasis, promoting qi circulation and relieving pain.All medicine compatibilities are to reach promoting blood circulation and stopping pain, the merit of removing blood stasis for promoting tissue regeneration.Trauma treating Diedahongyao has following pharmacological action:
1. antiinflammatory action: can obviously suppress the increase (P＜0.01) of the mouse skin capillary permeability that histamine phosphate causes; Mouse ear inflammation (P＜0.01) due to the obvious antagonism dimethylbenzene; The rat toes swelling that egg white or noradrenaline are caused has obvious antagonism (P＜0.05).
2. analgesic activity: this product can obviously suppress the mouse writhing reaction (P＜0.01) due to the acetic acid, significantly improves hot plate method mouse pain threshold.
3. improve microcirculation: obviously improve the microcirculation of mouse auricular concha.
4. to the lymphocytic influence of t: the cellular immune function that obviously improves mouse.
Mainly be applicable to fall beat, sprain, push, collision, injured in the sinews or bones, hemostasis swelling, soft tissue injury.Rheumatic numbness, scapulohumeral periarthritis, tenosynovitis, diseases such as the pain that cervical spondylopathy, lumbar vertebra disease, spur cause, numbness.
Existing trauma treating Diedahongyao 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 trauma treating Diedahongyao 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 trauma treating Diedahongyao preparation, and this method adopts thin-layered chromatography to differentiate, adopt spectrophotometric method 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 trauma treating Diedahongyao preparation.
The trauma treating Diedahongyao preparation prescription consists of:
Pseudo-ginseng 50.7g safflower 11.8g Radix Angelicae Sinensis 11.8g
Ligusticum wallichii 11.8g root of Dahurain angelica 11.8g ground bettle 11.8g
Trauma treating Diedahongyao ball (condensed pill) method for making
Above Six-element, pseudo-ginseng, Ligusticum wallichii, the root of Dahurain angelica, Radix Angelicae Sinensis are ground into fine powder respectively, and be standby.Safflower, ground bettle add 3.5 times for the first time with 60% alcohol reflux three times, extract 6 hours, for the second time add 2.5 times, extracted 4 hours, add 2 times for the third time, extracted 2 hours, and merged ethanol extract, filter, filtrate recycling ethanol also is condensed into the clear cream that relative density is 1.05～1.07 (50 ℃), clear cream and above-mentioned fine powder and an amount of maltose mixing are made 1000 balls, drying, polishing, promptly.
The present invention be directed to trauma treating Diedahongyao ball (condensed pill) preparation and propose method of quality control, but also be not limited to trauma treating Diedahongyao ball (condensed pill) preparation, also can comprise other oral formulations of trauma treating Diedahongyao ball such as tablet, capsule, syrup, granule.
Its prescription of other dosage forms of the trauma treating Diedahongyao that the present invention includes is identical with trauma treating Diedahongyao ball (condensed 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 preparations, 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 trauma treating Diedahongyao of the present invention can adopt following method:
By the Chinese medicine material 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, diacolation, extraction, water are carried, alcohol extracting, ester are carried, methods such as ketone is carried, chromatography obtain, these active substances can be the materials of medicinal extract form, can be that dry extract also can be a liquid extract, can also be the high-purity extract, make different concentration according to the different needs decision of preparation.
Other dosage forms of trauma treating Diedahongyao 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 sylvite, sweet mellow wine, sorbierite, sorbic acid or sylvite, xylitol, maltose, glucose, fructose, dextran, glycocoll, starch, sucrose, lactose, mannitol, Nepal's methyl esters, Nepal's ethyl ester, Nepal's propyl ester, Nepal's butyl ester, sodium pyrosulfite, sodium bisulfite, sodium thiosulfate, cysteine hydrochloride, mercaptoacetic acid, 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, sulfuric acid, phosphoric acid, amino acid, sodium chloride, potassium chloride, sodium lactate, silicon derivative, cellulose and derivant thereof, alginates, gelatin, polyvinylpyrrolidone, glycerine, propylene glycol, ethanol, soil temperature 60-80, Arlacel-80, beeswax, sheep oil, whiteruss, hexadecanol, gallate ester, agar, triethanolamine, basic amino acid, urea, allantoin, surfactant, polyglycol, cyclodextrin, β-cyclodextrin, phospholipid material etc.
Trauma treating Diedahongyao preparation of the present invention, particularly condensed pill preparation, it is as follows that its function cures mainly usage and dosage:
[function with cure mainly] promoting blood circulation and stopping pain, eliminate blood stasis and promote tissue regeneration.Be used for traumatic injury, muscles and bones blood stasis and swelling pain, rheumatic numbness.
[usage and consumption] is oral, one time 4 ball, and 2 times on the one, children reduce by half.
[attention] is not taken by pregnant women, and withdraw menstrual period.
[specification] per 4 balls are equivalent to crude drug 0.44g.
Shady and cool dry place is put in [storage] sealing.
[term of validity] 2 years.
The present invention is to provide the method for quality control at above trauma treating Diedahongyao preparation, particularly the condensed pill preparation is the quality of control trauma treating Diedahongyao 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 proterties, 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 proterties, step is:
[proterties] this product is that pale brown look is to tan condensed pill, distinguish the flavor of little suffering, hardship.
The discriminating of content, step is:
This product 5g is got in [discriminating] (1), pulverizes, and adds sherwood oil (60～90 ℃) 20ml, and sonicated 20 minutes filters, and filtrate volatilizes, and residue adds sherwood oil (60～90 ℃) 1ml makes dissolving, as need testing solution.Other gets root of Dahurain angelica control medicinal material 0.1g, adds sherwood oil (60～90 ℃) 10ml, floods 30 minutes, and jolting is constantly left standstill, and supernatant is medicinal material solution in contrast.Get Imperatorin, Isomperatorin reference substance again, add ethyl acetate and make the solution that every 1ml contains 1mg, in contrast product solution.According to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 4 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (17: 3) is developping agent, launches, and takes out, dry, put under the ultraviolet lamp (254nm) and inspect.In the test sample chromatogram, with reference substance chromatogram and the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(2) get this product 5g, pulverize, the 30ml sonicated that adds diethyl ether 30min filters, and filtrate volatilizes ether, adds ethyl acetate 1ml and makes dissolving, as need testing solution.Other gets the Ligusticum wallichii control medicinal material, and each 1g of Radix Angelicae Sinensis control medicinal material makes control medicinal material solution respectively with method.According to thin-layered chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia) test, draw each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (9: 1) is developping agent, launches, and takes out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatogram with control medicinal material chromatogram relevant position on, show the fluorescence spot 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) composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (Chinese Pharmacopoeia version appendix in 2005 VII).
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 4000; Column temperature: 25 ℃.
The preparation precision of reference substance solution takes by weighing the ginsenoside Rg1, the Rb1 reference substance is an amount of, adds methyl alcohol and makes the solution that every 1ml contains 0.8mg, promptly.
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got about 1.50g, and accurate the title decides, the accurate methyl alcohol 20ml that adds, claim decide weight, reflux 2 hours is put coldly, and weight decided in title again, supply with methyl alcohol and to subtract weight loss, shake up, filter with miillpore filter (0.45 μ m), promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
The every gram of this product contains pseudo-ginseng with ginsenoside Rb1 (C
54H
92O
23) and ginsenoside Rg1 (C
42H
72O
14) the total amount meter, must not be less than 9.3mg.
The present invention changes agent on former formulation basis, simultaneously production technology reformed,
Disintegrating process is investigated
Pseudo-ginseng, Radix Angelicae Sinensis, Ligusticum wallichii, the root of Dahurain angelica are used as medicine with fine powder.Plan takes by weighing a certain amount of medicinal material, pulverizes respectively, crosses 100 mesh sieves, investigate powder rate (the results are shown in Table 12-1).
Table 12-1 gets the powder rate and investigates
12.4.3.2 Study on extraction
Clearly stipulated the extraction solvent of medicinal material under the primary standard method for making item, extraction time, extraction time and solvent load, so need not investigate, still adopt the extraction process under the former method for making item, and extract reclaimed ethanol and be condensed into the clear cream that relative density is 1.05～1.07 (50 ℃), it is safflower, ground bettle is with 60% alcohol reflux three times, for the first time add 3.5 times, extracted 6 hours, for the second time add 2.5 times, extracted 4 hours, add 2 times for the third time, extracted 2 hours, merge ethanol extract, filter, reclaim ethanol and be condensed into the clear cream that relative density is 1.05～1.07 (50 ℃).
To receive the cream rate is index, to above extraction process checking three times, the results are shown in Table 12-2
Table 12-2 extraction process demonstration test
By The above results as can be known, receive the cream rate and change not quite, illustrate that former extraction process stablizes feasiblely, have reappearance.
12.4.3.3 Study on Forming
Because the many cream of this product powder are few, cause the ball bar more coarse, easily broken, therefore easy-formation does not need to add an amount of binder to make suitable softwood.Maltose is a binder commonly used in the medicine pill, so this product selects for use maltose as binder.Get respectively three parts of pseudo-ginseng 101.4g, safflower 23.6g, Radix Angelicae Sinensis 23.6g, Ligusticum wallichii 23.6g, root of Dahurain angelica 23.6g, ground bettle 23.6g, extract by the above-mentioned technology of drafting, reclaim ethanol and be condensed into the clear cream of 1.05～1.07 (50 ℃), add fine powders such as pseudo-ginseng, and add the maltose of 100g, 125g, 150g respectively, mixing, system softwood, making situation with softwood is that index is investigated the maltose consumption, the results are shown in Table 12-3.
The investigation of table 12-3 maltose consumption
The softwood that is made when adding 125g as can be known by experimental result is more suitable, therefore determines to add maltose 125g.
With YUJ-16A type high speed pellet processing machine, the control wet-pill making focuses on 0.17g, pill, and 50～55 ℃ of dryings are taken out, the sieve ball, polishing gets the finished product ball.
The technical study brief summary:
According to above technical study, get pseudo-ginseng, Ligusticum wallichii, the root of Dahurain angelica, Radix Angelicae Sinensis and be ground into fine powder respectively, standby; Safflower, ground bettle add 3.5 times for the first time with 60% alcohol reflux three times, extract 6 hours, for the second time add 2.5 times, extracted 4 hours, add 2 times for the third time, extracted 2 hours, merge ethanol extract, filtrate recycling ethanol also is condensed into the clear cream that relative density is 1.05～1.07 (50 ℃), clear cream and above-mentioned fine powder and an amount of maltose mixing, make 1000 balls, drying, polishing, promptly.
12.4.4 the adjustment that prescription is made total amount
The trauma treating Diedahongyao tablet recipe is:
The single dose is 2 and (is equivalent to crude drug 0.4388g, be 0.44g), consider that the single dose with the trauma treating Diedahongyao ball is decided to be 4 balls (being equivalent to crude drug 0.4388g, i.e. 0.44g), the amount that this prescription is made pill is 2000 balls, and is consistent with former tablets amount.Being converted into 1000 balls prescription is:
Do not differentiate and the assay item in the former preparation quality standard, we study its quality standard, the thin layer that has increased Radix Angelicae Sinensis, Ligusticum wallichii, the root of Dahurain angelica is differentiated, has set up the method for pseudo-ginseng assay simultaneously, the quality standard of this product is improved and improves.
14.2.5.1 differentiating the thin layer of the root of Dahurain angelica in (1) side of being differentiates
We serve as that Study on Identification is carried out in contrast with Imperatorin, Isomperatorin reference substance with reference to relevant document, make negative control simultaneously, and the result shows, negative control is not seen interference, in the test sample chromatogram, with contrast chromatogram corresponding position on, show the fluorescence spot of same color.
14.2.5.2 differentiating the thin layer of Radix Angelicae Sinensis, Ligusticum wallichii medicinal material in (2) side of being differentiates
We serve as that Study on Identification is carried out in contrast with Radix Angelicae Sinensis, Ligusticum wallichii control medicinal material, make negative control simultaneously, and the result shows: negative control is not seen interference, in the test sample chromatogram with contrast chromatogram corresponding position on, show same color fluorescence spot.
[14.2.6 inspection]
14.2.6.1 stipulate down, moisture, weight differential, the microbial limit of this product three batch samples are checked the result meets the pharmacopeia regulation according to an appendix pill of Chinese Pharmacopoeia version in 2005 item.
14.2.6.2 heavy metal
Checked 3 batch samples by heavy metal inspection technique [2005 editions one appendix XI E of Chinese Pharmacopoeia, second method], the result all surpasses 10/1000000ths, so quality standard is not included in an inspection temporarily in.
14.2.6.3 arsenic salt
Having checked 3 batch samples according to arsenic salt inspection technique [2005 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.
[14.2.7 assay]
Trauma treating Diedahongyao ball (condensed pill) is made by medicinal materials such as pseudo-ginseng, and pseudo-ginseng is monarch drug in a prescription and consumption maximum in the side.With reference to pseudo-ginseng assay of Chinese Pharmacopoeia version in 2000, determine with the ginsenoside Rg
1, Rb
1Be index determining pseudo-ginseng content.But method is thin layer chromatography scanning in the pharmacopeia, and is more loaded down with trivial details, and we (comprise the selection of 1. measuring wavelength with reference to relevant document by methodology, 2. extract determining of solvent, 3. extraction time is definite, and 4. system suitability test and specificity are investigated, and 5. linear relationship is investigated, 6. stability test, 7. precision test, 8. replica test, 9. recovery test, 10. the mensuration of sample) investigate, set up the high performance liquid chromatography of measuring ginsenoside Rg1, Rb1 in this product.Characteristics such as this method has accurately, favorable reproducibility, specificity are strong, fast and simple can be used for controlling the inherent quality of this product.
14.2.7.1 instrument and reagent
Agilent 1100 high performance liquid chromatographs; Phenomenex Luna chromatographic column (5 μ m, 4.6 * 250mm); AB204-S type electronic balance (plum Teller-holder benefit company); AG-135 type electronic balance (plum Teller-holder benefit company); Electric-heated thermostatic water bath (Qin Tai medical apparatus and instruments factory).Acetonitrile is chromatographically pure (a Merck KGaA company); Water is double distilled water; It is pure that all the other reagent are analysis
The ginsenoside Rg
1Reference substance (available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: 0703-200221),
Ginsenoside Rb
1Reference substance (available from Nat'l Pharmaceutical ﹠ Biological Products Control Institute, lot number: 110704-200217);
Trauma treating Diedahongyao ball (condensed pill): Jiangxi Huiren Pharmaceutical Co., Ltd's self-control
Research lot number: 20040728,20040729,20040730
14.2.7.2 chromatographic condition
Chromatographic column (Phenomenex Luna chromatographic column 250mm * 4.6mm, 5 μ m), moving phase: with the acetonitrile is mobile phase A, is Mobile phase B with water, the regulation in the according to the form below is carried out gradient elution; Flow velocity: 1ml/min detects wavelength: 203nm, column temperature: 25 ℃.Other composition is to the ginsenoside Rg under this condition
1, Rb
1Noiseless, can reach effective separation, theoretical cam curve is calculated as 62261 by the ginsenoside Rg1 peak.
14.2.7.3 negative sample test
Prepare the sample that does not contain pseudo-ginseng by prescription and production technology, press the test of text content assaying method, the result does not see interference at ginsenoside Rg1, place, Rb1 peak.
14.2.7.4 the investigation of linear relationship
Precision takes by weighing the ginsenoside Rg
1, Rb
1Reference substance 8.33mg, 8.02mg put in the 10ml 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, 15 μ l, 20 μ l inject liquid chromatograph, the record chromatogram is an ordinate with the peak area, and concentration is horizontal ordinate, the drawing standard curve the results are shown in Table 4.
Table 4 ginsenoside Rg
1, Rb
1Standard curve determination
The ginsenoside Rg
1Regression equation: Y=3182.2X+109.36, r=0.9997 (n=5), the result shows, the ginsenoside Rg
1In 0.1666～1.666mg/ml concentration range, be good linear relationship.
Ginsenoside Rb
1Regression equation: Y=2552.1X-9.3276, r=0.9998 (n=5), the result shows, ginsenoside Rb
1In 0.1604～1.604mg/ml concentration range, be good linear relationship.
14.2.7.5 precision test
Get same reference substance solution, continuous sample introduction 6 times is measured, and the record peak area the results are shown in Table 5, and RSD is for being respectively 0.85%, 0.70%.
The test of table 5 precision
14.2.7.6 need testing solution study on the stability
(lot number: 20040728) measured respectively in 0,2,4,8,12,24 hour, the RSD value is respectively 1.66%, 1.67% as a result, shows that need testing solution is stable in 24 hours, sees Table 6 to get need testing solution.
Table 6 need testing solution stability
14.2.7.7 replica test
Get same lot number sample (lot number: 20040728) totally 5 parts, measure according to content assaying method in the text, the results are shown in Table 7.
Table 7 replica test
14.2.7.8 recovery test
Get known content this product (lot number: 20040728) an amount of, porphyrize, precision takes by weighing in right amount, totally 6 parts, a certain amount of ginsenoside Rg of accurate respectively adding
1, Rb
1Reference substance is measured according to content assaying method in the text, and calculate recovery rate and RSD the results are shown in Table 8,9.
Table 8 ginsenoside Rg
1The application of sample recovery test
Table 9 ginsenoside Rb
1The application of sample recovery test
14.2.7.9 sample determination
Measure 10 batch samples respectively by the text content assaying method, the results are shown in Table 10.
Table 10 sample determination
The formulation of content limit: according to above measurement result, ginsenoside Rg in the sample
1With ginsenoside Rb
1The average content of total amount is 22.5mg/g.For formulation content limit more effectively and reasonably, will be according to the ginsenoside Rg
1With ginsenoside Rb
1The rate of transform of total amount is calculated, formula: every gram this product contains ginsenoside Rg in amount * pseudo-ginseng crude drug of pseudo-ginseng
1With ginsenoside Rb
1Content limit * the rate of transform of total amount * 80%, wherein every gram contains the pseudo-ginseng amount and is about 0.307g, ginsenoside Rg in the pseudo-ginseng crude drug
1With ginsenoside Rb
1The content limit of total amount is 3.8%, and the rate of transform is about about 94%, and result of calculation is 9.3mg/g, so the tentative every gram of this product contains pseudo-ginseng with ginsenoside Rb
1(C
54H
92O
23) and the ginsenoside Rg
1(C
42H
72O
14) the total amount meter, must not be less than 9.3mg.
More than this product described in the method for quality control of the present invention, be meant trauma treating Diedahongyao ball (condensed pill) according to technology preparation of the present invention, when other formulations are measured, refer to corresponding other formulations.
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.
Figure of description:
Fig. 1 ginsenoside Rg
1Typical curve
y＝3182.2x+109.36
R2＝0.9995
Fig. 2 ginsenoside Rb1 typical curve
y＝2552.1x-9.3276
R2＝0.9996
Embodiment:
Further specify the present invention by the following examples, but not as limitation of the present invention.
The quality control of embodiment 1 trauma treating Diedahongyao ball (condensed pill)
Method of quality control of the present invention may further comprise the steps:
The observation of proterties, 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 proterties, step is:
[proterties] this product is that pale brown look is to tan condensed pill, distinguish the flavor of little suffering, hardship.
The discriminating of content, step is:
This product 5g is got in [discriminating] (1), pulverizes, and adds sherwood oil (60～90 ℃) 20ml, and sonicated 20 minutes filters, and filtrate volatilizes, and residue adds sherwood oil (60～90 ℃) 1ml makes dissolving, as need testing solution.Other gets root of Dahurain angelica control medicinal material 0.1g, adds sherwood oil (60～90 ℃) 10ml, floods 30 minutes, and jolting is constantly left standstill, and supernatant is medicinal material solution in contrast.Get Imperatorin, Isomperatorin reference substance again, add ethyl acetate and make the solution that every 1ml contains 1mg, in contrast product solution.According to thin-layered chromatography (appendix VIB of Chinese Pharmacopoeia version in 2005) test, draw each 4 μ l of above-mentioned solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (17: 3) is developping agent, launches, and takes out, dry, put under the ultraviolet lamp (254nm) and inspect.In the test sample chromatogram, with reference substance chromatogram and the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color.
(2) get this product 5g, pulverize, the 30ml sonicated that adds diethyl ether 30min filters, and filtrate volatilizes ether, adds ethyl acetate 1ml and makes dissolving, as need testing solution.Other gets the Ligusticum wallichii control medicinal material, and each 1g of Radix Angelicae Sinensis control medicinal material makes control medicinal material solution respectively with method.According to thin-layered chromatography (2005 editions appendix VIB of Chinese Pharmacopoeia) test, draw each 5 μ L of above-mentioned three kinds of solution, put respectively on same silica gel g thin-layer plate, with normal hexane-ethyl acetate (9:1) is developping agent, launches, and takes out, dry, put under the uviol lamp (365nm) and inspect.In the test sample chromatogram with control medicinal material chromatogram relevant position on, show the fluorescence spot 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) composition that contains is carried out assay, and step is:
[assay] measured according to high performance liquid chromatography (Chinese Pharmacopoeia version appendix in 2005 VII).
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 203nm.Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 4000; Column temperature: 25 ℃.
The preparation precision of reference substance solution takes by weighing the ginsenoside Rg1, the Rb1 reference substance is an amount of, adds methyl alcohol and makes the solution that every 1ml contains 0.8mg, promptly.
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got about 1.50g, and accurate the title decides, the accurate methyl alcohol 20ml that adds, claim decide weight, reflux 2 hours is put coldly, and weight decided in title again, supply with methyl alcohol and to subtract weight loss, shake up, filter with miillpore filter (0.45 μ m), promptly.
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly.
The every gram of this product contains pseudo-ginseng with ginsenoside Rb1 (C
54H
92O
23) and ginsenoside Rg1 (C
42H
72O
14) the total amount meter, must not be less than 9.3mg.
The preparation of embodiment 2 trauma treating Diedahongyao balls (condensed pill)
Pseudo-ginseng 50.7g safflower 11.8g Radix Angelicae Sinensis 11.8g
Ligusticum wallichii 11.8g root of Dahurain angelica 11.8g ground bettle 11.8g
Trauma treating Diedahongyao ball (condensed pill) method for making
Above Six-element, pseudo-ginseng, Ligusticum wallichii, the root of Dahurain angelica, Radix Angelicae Sinensis are ground into fine powder respectively, and be standby.Safflower, ground bettle add 3.5 times for the first time with 60% alcohol reflux three times, extract 6 hours, for the second time add 2.5 times, extracted 4 hours, add 2 times for the third time, extracted 2 hours, and merged ethanol extract, filter, filtrate recycling ethanol also is condensed into the clear cream that relative density is 1.05～1.07 (50 ℃), clear cream and above-mentioned fine powder and an amount of maltose mixing are made 1000 balls, drying, polishing, promptly.
Claims (1)
1, a kind of detection method of trauma treating Diedahongyao preparation, wherein, above-mentioned trauma treating Diedahongyao preparation is made by following Chinese medicine material:
Pseudo-ginseng 50.7g safflower 11.8g Radix Angelicae Sinensis 11.8g
Ligusticum wallichii 11.8g root of Dahurain angelica 11.8g ground bettle 11.8g
It is characterized in that described method step is as follows:
The observation of proterties, step is: proterties, this product are that pale brown look is to tan condensed pill, distinguish the flavor of little suffering, hardship; The discriminating of content, step is:
Differentiate that (1) gets this product 5g, pulverize that 60～90 ℃ add sherwood oil 20ml, sonicated 20 minutes filters, and filtrate volatilizes, and 60～90 ℃ of residues add sherwood oil 1ml makes dissolving, as need testing solution; Other gets root of Dahurain angelica control medicinal material 0.1g, and 60～90 ℃ add sherwood oil 10ml, floods 30 minutes, and jolting is constantly left standstill, and supernatant is medicinal material solution in contrast; Get Imperatorin, Isomperatorin reference substance again, add ethyl acetate and make the solution that every 1ml contains 1mg, in contrast product solution; An appendix VI of Chinese Pharmacopoeia version in 2005 B draws each 4 μ l of above-mentioned solution according to the thin-layered chromatography test, puts respectively on same silica gel g thin-layer plate, with ratio is that 17: 3 normal hexane-ethyl acetates are developping agent, launches, and takes out, dry, put under the 254nm ultraviolet lamp and inspect; In the test sample chromatogram, with reference substance chromatogram and the corresponding position of control medicinal material chromatogram on, show the fluorescence spot of same color;
(2) get this product 5g, pulverize, the 30ml sonicated that adds diethyl ether 30min filters, and filtrate volatilizes ether, adds ethyl acetate 1ml and makes dissolving, as need testing solution; Other gets the Ligusticum wallichii control medicinal material, and each 1g of Radix Angelicae Sinensis control medicinal material makes control medicinal material solution respectively with method; 2005 editions appendix VIB of Chinese Pharmacopoeia draw each 5 μ L of above-mentioned three kinds of solution according to the thin-layered chromatography test, put respectively on same silica gel g thin-layer plate, with the ratio is that 9:1 normal hexane-ethyl acetate is developping agent, launches, and takes out, dry, put under the 365nm uviol lamp and inspect; In the test sample chromatogram with control medicinal material chromatogram relevant position on, show the fluorescence spot of same color;
The inspection of content, step is:
Check that an appendix I of Chinese Pharmacopoeia version in 2005 A should meet every regulation relevant under the pill item composition that contains is carried out assay, step is:
Assay, Chinese Pharmacopoeia version appendix in 2005 VII is according to high effective liquid chromatography for measuring;
Chromatographic condition and system suitability test are filling agent with octadecylsilane chemically bonded silica; With the acetonitrile is mobile phase A, is Mobile phase B with water, and the regulation in the according to the form below is carried out gradient elution; The detection wavelength is 203nm; Number of theoretical plate calculates by the ginsenoside Rg1 peak should be not less than 4000; Column temperature: 25 ℃;
Time mobile phase A Mobile phase B
0～22 minute 20～40% 80～60%
The preparation precision of reference substance solution takes by weighing the ginsenoside Rg1, the Rb1 reference substance is an amount of, adds methyl alcohol and makes the solution that every 1ml contains 0.8mg, promptly;
This product under the weight differential item is got in the preparation of need testing solution, and porphyrize is got 1.50g, and accurate the title decides, the accurate methyl alcohol 20ml that adds, claim decide weight, reflux 2 hours is put coldly, and weight decided in title again, supply with methyl alcohol and to subtract weight loss, shake up, filter with 0.45 μ m miillpore filter, promptly;
Accurate respectively reference substance solution and each the 10 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, promptly;
The every gram of this product contains the total amount of pseudo-ginseng in ginsenoside Rb1 and ginsenoside Rg1, must not be less than 9.3mg.
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| CN108896500A (en) * | 2018-07-02 | 2018-11-27 | 张家敏 | A kind of screening and extracting method of white Chinese actinidia root anti-tumor active substance |
| CN110376316A (en) * | 2019-08-28 | 2019-10-25 | 广西国际壮医医院 | The method of quality control of Calusena lansium root herb |
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| Title |
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| 中华人民共和国卫生部药品标准中药成方制剂第20册. 中华人民共和国卫生部药典委员会，第359页. 1998 |
| 中华人民共和国卫生部药品标准中药成方制剂第20册. 中华人民共和国卫生部药典委员会，第359页. 1998 * |
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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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