CN102100807B - Chinese medicine composition for regulating qi, widening chest and relieving pain as well as detection method thereof - Google Patents
Chinese medicine composition for regulating qi, widening chest and relieving pain as well as detection method thereof Download PDFInfo
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Abstract
The invention discloses a Chinese medicine composite for regulating qi, widening chest and relieving pain and for treating stenocardia and abdominal distending pain as well as a quality control method thereof. The Chinese medicine composite is a pill made from raw medicinal materials of storax, borneol, frankincense, agilawood and radix aucklandiae. The quality control method comprises the steps of thin-layer identification of the frankincense and the borneol and content determination of the borneol and can more comprehensively control the quality of drugs in qualitative and quantitative aspects. Pharmacodynamics tests show that the Chinese medicine composite provided by the invention has better treatment effect on treating the stenocardia and the abdominal distending pain.
Description
The present invention is for dividing an application, and the original bill application number is 200810102915.8, and the original bill applying date is on March 28th, 2008, and the original bill name is called a kind of Chinese medicine composition and method of quality control thereof of regulate the flow of vital energy wide chest, pain relieving.
Technical field
The present invention relates to a kind of Chinese medicine composition and method of quality control thereof, relate in particular to a kind of Chinese medicine composition of wide chest, pain relieving and method of quality control of this Chinese medicine composition of regulating the flow of vital energy, belong to technical field of traditional Chinese medicines.
Background technology
Angina pectoris is coronary insufficiency, rapid, temporary transient ischemic of cardiac muscle and the caused clinical syndrome of anoxic.Its characteristics are paroxysmal shirtfront squeezing property pain perception, can be with other symptoms, and pain mainly is positioned at the breastbone rear portion, can be radiated to pareordia and left upper extremity, often betides work or when excited, continues several minutes, has a rest or with disappearing behind the nitrate preparations.This disease is more common in the male sex; Most patients are more than 40 years old; Tired, excited, be satiated with food, catch cold, rainy weather, acute circulatory failure etc. are common inducement, this disease is because the incidence of disease is high, mortality ratio is high; The healthy of the mankind in serious harm, thereby b referred to as " the first human killers ".Treatment such as clinical nitrate esters medicine commonly used, calcium ion antagonist, beta-blocker and control angina pectoris attacks, but these drug side-effects are big and be difficult to reach the purpose of basic treatment.
The traditional Chinese medical science thinks that this disease is that internal damage by the excessive seven emotions causes the strongly fragrant resistance of qi and blood, the thick greasy living phlegm of overfeeding delicious food wet and stop phlegm and stop drink, the excessive impairment of QI-blood of internal lesion caused by overexertion and cause deficiency of qi and blood to cause sending out, should dialectical opinion control, employing two methods of taking stopgap measures and effect a permanent cure.Taking stopgap measures, mainly use in the pain phase, is main with " leading to ", invigorates blood circulation, stagnation resolvation, method such as regulate the flow of vital energy, activate yang, reduce phlegm; Effect a permanent cure, generally use in the paracmasis, with adjustment negative and positive, internal organs, qi and blood be the master, yang-tonifying, enriching yin arranged, fill blood, method such as conditioning viscera.Wherein commonly used with " promoting blood circulation and removing blood stasis " method and " aromatic herbs activating yang " method.At present Chinese medicine is being developed some effectively medicines aspect this type of disease of treatment, like compound danshen dripping pills etc., continues performance traditional Chinese medicine characteristics, develops multipotency more and enough effectively treats the Chinese medicine composition of coronary heart disease and be necessary.
Summary of the invention
The Chinese medicine composition that the purpose of this invention is to provide a kind of regulate the flow of vital energy wide chest, pain relieving.
Another object of the present invention provides the method for quality control of this Chinese medicine composition.
The 3rd purpose of the present invention is the application of this Chinese medicine composition in treatment angina pectoris, belly distending pain.
The objective of the invention is to realize through following technical scheme:
Chinese medicine composition with regulate the flow of vital energy wide chest, analgesic effect according to the invention is made up of following weight portion bulk drug:
Storax 50～100 weight portions, borneol 100～150 weight portions, frankincense (system) 80～120 weight portions, agalloch eaglewood 150～200 weight portions, the banksia rose 200～250 weight portions.
Above-mentioned raw materials medicine optimum ratio is:
Storax 60～70 weight portions, borneol 120～130 weight portions, frankincense (system) 90～100 weight portions, agalloch eaglewood 160～170 weight portions, the banksia rose 230～240 weight portions.
Above-mentioned raw materials medicine optimum ratio is:
Storax 65 weight portions, borneol 125 weight portions, frankincense (system) 95 weight portions, agalloch eaglewood 165 weight portions, the banksia rose 235 weight portions.
Storax can be used muscone's replacement of 30～40 weight portions in the traditional Chinese medicinal composition raw materials of the present invention, and agalloch eaglewood can be used the santal replacement of identical weight part, and the banksia rose can be used identical weight part elecampane or root of three-nerved spicebush replacement.
Composition of the present invention can add auxiliary material by common process and process clinical acceptable forms such as tablet, capsule, oral liquid, dripping pill, spray, granule; Said auxiliary material comprises solvent, disintegrant, flavouring, antiseptic, colorant, bonding agent, lubricant, matrix etc.
The preparation method of Chinese medicine composition pill of the present invention is:
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extracted volatile oil 6 hours, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and Macrogol 6000 matrix 220 weight portions, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed dripping pill, promptly gets.
Weight portion/parts by volume is corresponding with g/ml in the composition of the present invention.
Pharmaceutical composition method of quality control of the present invention comprises one or more in following discrimination method and/or the assay:
(1) get dripping pill 1g of the present invention, put in the mortar, the 5～10ml that adds diethyl ether grinds, and filters, and filtrating is put in the evaporating dish, flings to ether, and the covering surfaces ware is put in the water-bath and heated, and collects sublimate, adds ethanol 1ml and makes dissolving, as need testing solution; Other gets the borneol reference substance, adds ethanol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to " each 2～5 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; With cyclohexane: ethyl acetate is 5～10: 1～3 developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get 4 of dripping pills of the present invention and put in the bottle of tool plug, add absolute ethyl alcohol 1～5ml and put and be heated to pill in about 40～70 ℃ water-bath and dissolve, shake up, cool slightly to there being a little deposition to separate out, filter with the syringe-type filter membrane, filtrating is as need testing solution; Other gets frankincense control medicinal material 0.1g, adds absolute ethyl alcohol 2ml, floods 1～2 hour, and supernatant is as control medicinal material solution; According to " each 3～8 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; The sherwood oil that with the boiling point is 60-90 ℃ is a developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast is heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
(3) according to " appendix a VI of Chinese pharmacopoeia version in 2005 E gas chromatography determination; Chromatographic condition and system suitability test are stationary phase with the carbowax-20M, and coating concentration is 10%; 140 ℃ of column temperatures;
It is an amount of that correction factor mensuration precision takes by weighing n-pentadecane, adds ethyl acetate and process the solution that every 1ml contains 5mg, as inner mark solution; Other gets borneol reference substance 10mg, accurate claims surely, puts in the 5ml measuring bottle, adds inner mark solution 1ml and makes dissolving and add ethyl acetate and be diluted to scale, shakes up, and draws 2-4 μ l, inject gas chromatograph, the calculation correction factor;
Assay method gets that dripping pill 0.5g of the present invention is accurate to be claimed surely, and add water 8～15ml and make dissolving, with ethyl acetate extraction 3-5 time, constant volume 25ml volumetric flask; Precision measure 5ml add in mark 1ml shake up, draw 2-4 μ l, inject gas chromatograph is measured, and promptly gets.
In preferred following discrimination method of pharmaceutical composition method of quality control of the present invention and/or the assay one or more:
(1) get dripping pill 1g of the present invention, put in the mortar, the 5～10ml that adds diethyl ether grinds, and filters, and filtrating is put in the evaporating dish, flings to ether, and the covering surfaces ware is put in the water-bath and heated, and collects sublimate, adds ethanol 1ml and makes dissolving, as need testing solution; Other gets the borneol reference substance, adds ethanol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to " each 3 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; With cyclohexane: ethyl acetate is 8: 2 a developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get 4 of dripping pills of the present invention and put in the bottle of tool plug, add absolute ethyl alcohol 2ml and put and be heated to pill in about 50 ℃ water-bath and dissolve, shake up, cool slightly to there being a little deposition to separate out, filter with the syringe-type filter membrane, filtrating is as need testing solution; Other gets frankincense control medicinal material 0.1g, adds absolute ethyl alcohol 2ml, floods 1 hour, and supernatant is as control medicinal material solution; According to " each 5 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; With boiling point 60-90 ℃ sherwood oil is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast is heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
(3) according to " appendix a VI of Chinese pharmacopoeia version in 2005 E gas chromatography determination;
Chromatographic condition and system suitability test are stationary phase with the carbowax-20M, and coating concentration is 10%; 140 ℃ of column temperatures.
It is an amount of that correction factor mensuration precision takes by weighing n-pentadecane, adds ethyl acetate and process the solution that every 1ml contains 5mg, as inner mark solution; Other gets borneol reference substance 10mg, accurate claims surely, puts in the 5ml measuring bottle, adds inner mark solution 1ml and makes dissolving and add ethyl acetate and be diluted to scale, shakes up, and draws 2-4 μ l, inject gas chromatograph, the calculation correction factor;
It is fixed that assay method is got the accurate title of dripping pill 0.5g of the present invention, adds water 10ml and make dissolving, with ethyl acetate extraction (8ml, 5ml, 5ml, 5ml), constant volume 25ml volumetric flask.Precision measure 5ml add in mark 1ml shake up, draw 2-4 μ l, inject gas chromatograph is measured, and promptly gets.
Above-mentioned method of quality control can be used for various preparations, and during the different dosage form quality control, need testing solution prepares selected amount of formulation and all is converted into identical raw material dose.
The method of quality control of Chinese medicine composition provided by the present invention; Be through obtaining behind the creative experiment sieving of big measuring; Through the screening to sample treatment, the selection of developping agent makes and differentiates that specificity is fine in the discrimination method; And method is economic and practical, the result is quick, and can both use different thin layer plates.Pass through screening in the content assaying method to sample, test sample disposal route; The selection of developping agent; Make content assaying method effectivelyly to carry out quality control, and will compare more stable that product that additive method measures shows on pharmacological effect with the product that this method is measured to product.
Embodiment
Following experimental example and embodiment are used to further specify but are not limited to the present invention.
Pharmacodynamics test:
1.1 medicine medicine of the present invention is the pill according to embodiment 1 preparation; The positive control medicine is a storax pill for treating coronary heart disease.
1.2 reagent and instrument
Soda lime, Shanghai the May 4th chemical reagent factory, lot number: 990830.MDA kit and NO kit, Nanjing build up bio-engineering research institute, lot number: 20030423.SOD kit, Nanjing gather Lik-Sang thing engineering in medicine research institute, lot number: 011029.TXB and 6 one Keto-PGF, kit, Beijing North biotechnology research institute, lot number: 030501.
WT/1001 type electronic balance, Jiangsu ten thousand gets balance equipment factory.WFZ800--D3B type ultraviolet-visible pectrophotometer, the Beijing Rayleigh Analytical Instrument Co.,Ltd.FJ one 2021 type radio-immunity counters, Plant No. 262.LD
Z4-0.8 hydro-extractor: Beijing Medical Centrifugal Machine Factory.The KENZ-ECG electrocardiograph, Japan can anti-company.
2 methods and result
2.1 to mouse normal pressure hypoxia endurance test: get 60 of Kunming mouses, male and female half and half, body weight (20 ± 2) g is divided into 4 groups at random; The difference gastric infusion, salt solution group, small dose group (1.95g/kg), heavy dose of group (3.9g/kg), storax pill for treating coronary heart disease group (2.7g/kg), the administration volume is all 0.6mL/10g; Dosage is equivalent to 10 times, 20 times, 10 times of people's consumption respectively, behind the administration 30min, mouse is put into the airtight wide-necked bottle of 8 same volumes (250mL) respectively; Adorn soda lime 20g respectively in the bottle, be lined with filter paper on the soda lime, bottleneck is coated with vaseline; Put into behind the mouse and to pick up counting bottle is airtight, examine dead mouse, the record death time.Test findings is seen table 1.
Table 1 medicine of the present invention is to the influence of the anti-anoxic of mouse normal pressure (X ± s)
| Group | n | Death time of animal (s) |
| The salt solution group | 15 | 34.2±6.62 |
| Medicine small dose group of the present invention | 15 | 40.0±9.43△ |
| The heavy dose of group of medicine of the present invention | 15 | 46.3±10.65△△* |
| The storax pill for treating coronary heart disease group | 15 | 37.3±5.90 |
Annotate: the physiological saline group compares, △ P＜0.05, △ △ P＜0.01; Compare * P＜0.01 with the storax pill for treating coronary heart disease group.
Test shows, medicine ability significant prolongation anoxia in mice death time of the present invention, low dose of P＜0.05, heavy dose of P＜0.01.Under the clinical equivalent amount, medicine of the present invention is superior to storax pill for treating coronary heart disease, and heavy dose of group relatively has significant differences with the storax pill for treating coronary heart disease group.
2.2 to mice plasma TXB2 and 6-Keto-PGF
1aInfluence get 40 of Kunming mouses, male and female half and half, body weight (20 ± 2) g is divided into 4 groups at random: salt solution group, small dose group, heavy dose of group, storax pill for treating coronary heart disease group; Dosage, method are the same, and every day 1 time, successive administration is after 1 week; The abdomen cardinal vein is got blood, and syringe soaks into EDTA, gets 0.6mL for every; Blood placed add 0.1mL EDTA in vitro, after having got it is shaken up, 15min is centrifugal for the room temperature held; 3500r/min, 10min gets blood plasma 0.2mL by specification mensuration program and does the TXB2 ria-determination.Other gets 0.2mL blood plasma, and by specification mensuration program is 6-Keto-PCF
1aMeasure, the result sees table 2.
Table 2 medicine of the present invention is to TXB2 and 6-Keto-PCF
1aInfluence (X ± S)
| Group | n | PCF 1a(pg/ml) | TXB2(pg/ml) | PGF 1a/TXB2 |
| NS | 10 | 97±37.8 | 114±34.6 | 0.85±0.22 |
| Medicine small dose group of the present invention | 10 | 111±55.5 | 98±37.2 | 1.13±0.32△△ |
| The heavy dose of group of medicine of the present invention | 10 | 121±65.7 | 89±25.4 | 1.36±0.43△△ |
| The storax pill for treating coronary heart disease group | 10 | 109±51.3 | 101±46.5 | 1.08±0.26△ |
Annotate: compare △ P＜0.05, △ △ P＜0.01 with the physiological saline group.
Test shows that medicine of the present invention can make 6-Keto-PCF
1aContent raises, and makes TXB2 content reduce single statistics unknown significance difference, 6-Keto-PGF
1a/ TXB2 obviously raises, and relatively has significant differences with the physiological saline group.
2.3 medicine of the present invention is to the influence of serum MDA, NO, SOD content
Get 40 of Kunming mouses, male and female half and half, body weight (20 ± 2) g; Be divided into 4 groups at random: salt solution group, small dose group, heavy dose of group, storax pill for treating coronary heart disease group, administration every day 1 time, dosage is the same; Successive administration is after 1 week, and the abdomen cardinal vein is got blood 1mL, and centrifuging goes out serum.Get serum 0.1mL, measure procedure operation, 532nm place test sample article absorbance with reference to MDA.Other gets serum 0.1mL in clean glass test tube, presses NO and measures procedure operation, and the 550nm place surveys respectively manages absorbance, calculates NO content according to typical curve.Other gets serum 0.1mL, adds 0.4ml physiological saline, after the dilution in 1: 5, gets 30 μ L, presses SOD and measures program determination SOD content.The result sees table 3.
Table 3 medicine of the present invention is to the influence of mice serum MDA, NO, SOD content (X ± s)
| Group | n | MDA(nmol/L) | NO(μmol/L) | SOD (OD) value |
| NS | 10 | 2.55±0.56 | 46.34±19.6 | 0.069±0.009 |
| Medicine small dose group of the present invention | 10 | 2.11±0.27△ | 58.88±22.4△ | 0.078±0.004△ |
| The heavy dose of group of medicine of the present invention | 10 | 1.88±0.11△△ | 74.12±25.6△△ | 0.082±0.005△△ |
| The storax pill for treating coronary heart disease group | 10 | 2.11±0.22△ | 65.76±19.3△ | 0.084±0.001△ |
Annotate: compare △ P＜0.05, △ △ P＜0.01 with physiological saline.
Medicine of the present invention raises SOD content, significantly improves to remove oxygen radical, oxidation resistance.
2.4 resisting myocardial ischemia property test
Get 40 of rats, male and female half and half, body weight (250 ± 20) g, random packet: salt solution group, heavy dose of group (2.7g/kg; Be equivalent to 20 times of people's consumption), small dose group (1.35g/kg is equivalent to 10 times of people's consumption), storax pill for treating coronary heart disease group (1.86g/kg is equivalent to 10 times of people's consumption), fixing under waking state; Record II lead electrocardiogram is measured the normal II electrograph that leads, successive administration 7 days before the medicine; 30min after the administration in the 8th day, every rat is anaesthetized with urethane, and measures the rat cardiogram; The cardiogram of contrast rat this moment is the normal cardiogram of rat with changing little person before the medicine, claims back sublingual vein injection of pituitrin 0.2u/kg; Finish in the 10s injection, the cardiogram of record injection back 1min, 5min is judged the rat heart ischemia.Cardiogram criterion: positive criterion (cardiac muscle is ischemic obviously): sT section horizontal-shift, skew＞0.1mV up or down; The T wave height is alarmmed, and surpasses with leading 1/2 of R ripple; The T wave height is alarmmed and is shifted with the sT section.Negative criterion (myocardial ischemia is not obvious): the oblique skew of ST section, or horizontal-shift＜0.1mV; The T ripple is low or two-way, inversion＜0.1mV.Height with sT field offset baseline is an index.Through the mV number average value of the summation (∑ ST) of every group of ST field offset baseline height index as the treating myocardial ischemia damage degree.The result sees table 4.
Table 4 medicine of the present invention is to rat heart muscle ischemic test findings
Annotate:, compare △ P＜0.05, △ △ P＜0.01 with the physiological saline group through check; Compare * P＜0.05 with the storax pill for treating coronary heart disease group.
Test findings shows that medicine of the present invention can obviously reduce rat heart muscle ischemic animal number, significantly improves the degree of rat heart muscle ischemic.
2.5 medicine of the present invention is to the hemorheological influence of immune rat
Get 40 of rats, male and female half and half are divided into 4 groups at random, 10 every group; Medication, dosage are with the test of resisting myocardial ischemia property, and 1 week of successive administration is behind the last administration 1h; Every subcutaneous rat is annotated adrenal gland rope 0.09mg/100g, and injection back 2h puts into 6 ℃ of cold water with rat, takes out behind the 5min and injects the adrenal gland rope once more; The shallow fiber crops of ether are got 4mL from the abdomen cardinal vein behind the 2h, the EDTA anti-freezing; With FASC-3031 type viscosity instrumentation hemorheology index, with the deformability of RBC deformeter mensuration RBC, test findings is seen table 5.
Table 5 medicine of the present invention is to the hemorheological influence of immune rat (X ± s)
Annotate: compare △ P＜0.05, △ △ P＜0.01 with model group.
Test findings shows that medicine of the present invention can significantly reduce rat plasma viscosity, improves ED, reduce the erythrocyte sedimentation rate value.
2.6 acetic acid twisting method analgesic experiment
Body weight 18～24g mouse, the male and female dual-purpose is divided into 4 groups at random.Medicine high dose group of the present invention, low agent dose group, storax pill for treating coronary heart disease group and honey aqueous solution group.Fasting 16h before the experiment, gastric infusion, control group give with the volume honey aqueous solution.30min after the administration, the aqueous acetic acid of mouse peritoneal injection 0.7%, dosage is 0.1ml/10g.With hind leg stretching, extension, belly contraction and body distortion is the pain index, interior pain number of times and the pain inhibition percent of 10min behind the record mouse peritoneal notes acetic acid.The result sees table 6.
The throe effect of table 6 medicine Dichlorodiphenyl Acetate of the present invention induced mice pain
Annotate: compare △ P＜0.05, △ △ P＜0.01 with the hydromel group; Compare * P＜0.05 with the storax pill for treating coronary heart disease group.
Test findings shows that medicine of the present invention can significantly suppress the pain of acetic acid induced mice, and the effect of medicine of the present invention is superior to the positive control medicine.
(2) technical study test
1, extract the test of volatile oil distillation time:
Press three parts of medicinal materials of embodiment 1 prescription configuration, every part contains frankincense (system) 105g, agalloch eaglewood 210g, banksia rose 210g distillation time and is respectively: 4 hours, 6 hours, 8 hours is index with the oil mass of volatilizing, and confirms distillation time.The result sees table 7.
The test of table 7 distillation time
According to above data, can find out that distilled 6 hours, volatile oil extracts complete basically, distillation time is 6 hours in the actual production.
2, refluxing extraction alcohol adding amount test
It is a to press embodiment 1 recipe quantity configuration medicinal material, and the distillation back dregs of a decoction are divided into three parts, and every part of dregs of a decoction distillation back adds 4 times of amounts of alcohol for first group, and second group adds 6 times of amounts of alcohol, and the 3rd group adds 8 times of amounts of alcohol, is index with the paste volume, confirms alcohol adding amount.The result sees table 8.
Table 8 alcohol adding amount test findings
With the paste-forming rate is index, can find out that adding 4 times of amounts of alcohol extracts fully basically, and can practice thrift cost, selects the 4 times of amounts of alcohol that add in therefore producing for use.
(3) method of quality control development test
(1) thin layer of borneol is differentiated
Standard items source borneol reference substance is purchased lot number: the 743-8902 in Nat'l Pharmaceutical & Biological Products Control Institute
The preparation of need testing solution: get these article 1g, put in the mortar, the 5～10ml that adds diethyl ether grinds, and filters, and filtrating is put in the evaporating dish, flings to ether, and the covering surfaces ware is put in the water-bath and heated, and collects sublimate, adds ethanol 1ml and makes dissolving, as need testing solution.
The preparation of reference substance solution: get the borneol reference substance, add ethanol and process the solution that every 1ml contains 1mg, as reference substance solution.
The preparation of negative control article solution: prepare the negative control article that lack borneol according to the test sample preparation method, the preparation method according to need testing solution prepares negative control article solution then.
The selection of A, developping agent
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 3 μ l of above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate; With the different proportioning mixed liquors of cyclohexane-ethyl acetate is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing.Compare test sample and the expansion effect of reference substance on thin layer plate, the result sees the following form:
The test findings that table 9 developping agent is selected
Can find out that from last table select cyclohexane: ethyl acetate is the developping agent of 8: 2 ratios, each spot launches effective, the Pass Test requirement.
B, blank test
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 3 μ l of above-mentioned need testing solution, reference substance solution and negative control article solution, put respectively on same silica gel g thin-layer plate; With cyclohexane-ethyl acetate (8: 2) is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color, negative control is noiseless.
(2) thin layer of frankincense is differentiated
Standard items source frankincense reference substance is purchased lot number: the 0970-200202 in Nat'l Pharmaceutical & Biological Products Control Institute
The preparation of need testing solution: get 4 of these article and put in the bottle of tool plug, add absolute ethyl alcohol 2ml and put and be heated to pill in about 50 ℃ water-bath and dissolve, shake up, cool slightly to there being a little deposition to separate out, filter with the syringe-type filter membrane, filtrating is as need testing solution.
The preparation of control medicinal material solution: get frankincense control medicinal material 0.1g, add absolute ethyl alcohol 2ml, flooded 1 hour, supernatant is as control medicinal material solution.
The preparation of negative control article solution: prepare the fragrant negative control article of hypogalactia according to the test sample preparation method, the preparation method according to need testing solution prepares negative control article solution then.
The selection of A, developping agent
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l of above-mentioned need testing solution and reference substance solution, put respectively on same silica gel g thin-layer plate; With sherwood oil (60-90 ℃) is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast is heated to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
The test findings that table 10 developping agent is selected
Can find out that from last table developping agent is with sherwood oil (60-90 ℃), each spot launches effective, and it is clear to develop the color, the Pass Test requirement.
B, blank test
According to thin-layered chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate; With sherwood oil (60-90 ℃) is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast is heated to the spot colour developing.In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color, negative control is noiseless.
(3) assay of borneol
Detecting instrument (room temperature detection): Agilent 4890 type gas chromatographs
Producer: Agilent Techologies Anjelen Sci. & Tech. Inc (China)
Stationary phase: carbowax-20M coating concentration: 10%
Column temperature: 170-200 ℃ of carrier: Chromaxorbw (Aw-Dmcs)
The reference substance source: borneol is purchased lot number: the 743-8902 in Nat'l Pharmaceutical & Biological Products Control Institute
N-pentadecane is purchased lot number: the 0970-200202 in Nat'l Pharmaceutical & Biological Products Control Institute
Assay method: it is fixed to get the accurate title of these article 0.5g, adds water 10ml and makes dissolving, with ethyl acetate extraction (8ml, 5ml, 5ml, 5ml), constant volume 25ml volumetric flask.Precision measure 5ml add in mark 1ml shake up, draw 2-4 μ l, inject gas chromatograph is measured, and promptly gets.
1. content assaying method is investigated:
(1) stability test need testing solution respectively at preparing the back 0,2,4,6,12,24 hour, is measured in accordance with the law, and the result shows that it is basicly stable in 24 hours, and the result sees the following form:
Table 11 stability test result
(2) linear relationship is investigated outfit borneol reference substance concentration and is respectively 0.3912mg/ml, 0.8150mg/ml, 1.6300mg/ml, 2.4450mg/ml, 3.2600mg/ml; The accurate respectively 2 μ l inject gas chromatographs of drawing; Measure peak area; The result sees the following form, and shows that borneol is linear between 0.7824 μ g-6.52 μ g, and its regression equation is:
y＝0.3422x+0.0054(r＝0.9998)
Table 12 linear relationship is investigated the result
(3) the accurate need testing solution 2-4 μ l that draws of precision test repeats sample introduction 5 times, tries to achieve relative standard deviation＜2%,
The result sees the following form:
Table 13 Precision test result
(4) the text method is pressed in reappearance test, gets same lot number and prepares 5 duplicate samples and measure, and tries to achieve relative standard deviation＜2%, and the result sees the following form:
Table 14 Precision test result
(5) the recovery test precision takes by weighing the sample 0.25g of the same a collection of medicine of the present invention (according to embodiment 1 preparation) of known content; Add borneol reference substance 16mg, press preparation method's operation of text need testing solution, measure its content; And calculate its recovery, measure the result and see the following form:
Table 15 recovery test result
Can find out that from above methodological study result the content of borneol in the medicine can be stablized, effectively controlled to method of quality control of the present invention.
Following examples all can realize above test effect.
Embodiment 1
Take by weighing following weight portion (g) bulk drug:
Storax 65g, borneol 125g, frankincense (system) 95g, agalloch eaglewood 165g, banksia rose 235g
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and Macrogol 6000 matrix 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 450g dripping pill, promptly gets.
Embodiment 2
Take by weighing following weight portion (g) bulk drug:
Muscone 35g, borneol 125g, frankincense (system) 95g, santal 165g, elecampane 235g
The above five tastes, except that muscone, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and Macrogol 6000 matrix 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 430g dripping pill, promptly gets.
Embodiment 3
Take by weighing following weight portion (g) bulk drug:
Storax 65g, borneol 125g, frankincense (system) 95g, santal 165g, elecampane 235g
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and Macrogol 6000 matrix 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 450g dripping pill, promptly gets.
Embodiment 4
Take by weighing following weight portion (g) bulk drug:
Storax 65g, borneol 125g, frankincense (system) 95g, santal 165g, root of three-nerved spicebush 235g
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and polyethylene glycol groups 6000 matter 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 450g dripping pill, promptly gets.
Embodiment 5
Take by weighing following weight portion (g) bulk drug:
Storax 50g, borneol 100g, frankincense (system) 120g, agalloch eaglewood 200g, banksia rose 200g.
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and Macrogol 6000 matrix 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 420g dripping pill, promptly gets.
Embodiment 6
Take by weighing following weight portion (g) bulk drug:
Storax 100g, borneol 150g, frankincense (system) 80g, agalloch eaglewood 150g, banksia rose 250g.
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and Macrogol 6000 matrix 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 500g dripping pill, promptly gets.
Embodiment 7
Take by weighing following weight portion (g) bulk drug:
Storax 60g, borneol 130g, frankincense (system) 90g, agalloch eaglewood 160g, banksia rose 240g
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and polyglycol matrix 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 450g dripping pill, promptly gets.
Embodiment 8
Take by weighing following weight portion (g) bulk drug:
Storax 70g, borneol 120g, frankincense (system) 100g, agalloch eaglewood 170g, banksia rose 230g
The above five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extract volatile oil, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively; Each 2 hours, filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density; Drying is ground into fine powder, adds storax, borneol and polyglycol matrix 220g, is heated to dissolving; Add volatile oil such as above-mentioned frankincense again, mixing is processed the 450g dripping pill, promptly gets.
Embodiment 9
According to embodiment 1 identical method and consumption, 3 batches of dripping pills of the present invention of middle trial production.
Embodiment 10
Method of quality control of the present invention:
(1) get the dripping pill 1g of embodiment 1, put in the mortar, the 5～10ml that adds diethyl ether grinds, and filters, and filtrating is put in the evaporating dish, flings to ether, and the covering surfaces ware is put in the water-bath and heated, and collects sublimate, adds ethanol 1ml and makes dissolving, as need testing solution; Other gets the borneol reference substance, adds ethanol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to " each 3 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; With cyclohexane: ethyl acetate=8: 2 is a developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get 4 of the dripping pills of embodiment 1, put in the bottle of tool plug, add absolute ethyl alcohol 2ml and put and be heated to pill in about 50 ℃ water-bath and dissolve, shake up, cool slightly to there being a little deposition to separate out, filter with the syringe-type filter membrane, filtrating is as need testing solution; Other gets frankincense control medicinal material 0.1g, adds absolute ethyl alcohol 2ml, floods 1 hour, and supernatant is as control medicinal material solution; According to " each 5 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; With boiling point 60-90 ℃ sherwood oil is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast is heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
(3) according to " appendix a VIE of Chinese pharmacopoeia version in 2005 gas chromatography determination;
Chromatographic condition and system suitability test are stationary phase with the carbowax-20M, and coating concentration is 10%; 140 ℃ of column temperatures.
It is an amount of that correction factor mensuration precision takes by weighing n-pentadecane, adds ethyl acetate and process the solution that every 1ml contains 5mg, as inner mark solution; Other gets borneol reference substance 10mg, accurate claims surely, puts in the 5ml measuring bottle, adds inner mark solution 1ml and makes dissolving and add ethyl acetate and be diluted to scale, shakes up, and draws 2-4 μ l, inject gas chromatograph, the calculation correction factor;
Assay method is got the dripping pill 0.5g precision of embodiment 1 and is claimed to add water 10ml and make dissolving, with ethyl acetate extraction (8ml, 5ml, 5ml, 5ml), constant volume 25ml volumetric flask calmly.Precision measure 5ml add in mark 1ml shake up, draw 2-4 μ l, inject gas chromatograph is measured, and promptly gets.The every gram of these article contains borneol (C
10H
18O) must not be less than 40mg.
Embodiment 11
The assay result of 3 batches of dripping pills of the present invention that embodiment 9 is produced:
Lot number content (mg/g)
101 74.186
202 76.021
303 71.408
Claims (3)
1. the detection method of the Chinese medicine composition of regulate the flow of vital energy wide chest, pain relieving is characterized in that this method comprises following discrimination method and content assaying method:
(1) get 4 of this Chinese traditional medicine composition composition dropping pills and put in the bottle of tool plug, add and be heated to pill in the water-bath that absolute ethyl alcohol 1～5ml puts 40～70 ℃ and dissolve, shake up, cool slightly to there being a little deposition to separate out, filter with the syringe-type filter membrane, filtrating is as need testing solution; Other gets frankincense control medicinal material 0.1g, adds absolute ethyl alcohol 2ml, floods 1～2 hour, and supernatant is as control medicinal material solution; According to " each 3～8 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; The sherwood oil that with the boiling point is 60-90 ℃ is a developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast is heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
(2) according to " appendix a VI of Chinese pharmacopoeia version in 2005 E gas chromatography determination;
Chromatographic condition and system suitability test are stationary phase with the carbowax-20M, and coating concentration is 10%; 140 ℃ of column temperatures; It is an amount of that correction factor mensuration precision takes by weighing n-pentadecane, adds ethyl acetate and process the solution that every 1ml contains 5mg, as inner mark solution; Other gets borneol reference substance 10mg, accurate claims surely, puts in the 5ml measuring bottle, adds inner mark solution 1ml and makes dissolving and add ethyl acetate and be diluted to scale, shakes up, and draws 2-4 μ l, inject gas chromatograph, the calculation correction factor;
Assay method gets that this Chinese traditional medicine composition composition dropping pills 0.5g is accurate to be claimed surely, and add water 8～15ml and make dissolving, with ethyl acetate extraction 3-5 time, constant volume 25ml volumetric flask; Precision measure 5ml add in mark 1ml shake up, draw 2-4 μ l, inject gas chromatograph is measured, and promptly gets;
Wherein, above-mentioned Chinese medicine composition is made up of following weight portion bulk drug:
Storax 50～100 weight portions, borneol 100～150 weight portions, frankincense 80～120 weight portions, agalloch eaglewood 150～200 weight portions, the banksia rose 200～250 weight portions.
2. the detection method of the Chinese medicine composition of regulate the flow of vital energy wide chest, pain relieving is characterized in that this method comprises following discrimination method and content assaying method:
(1) get this Chinese traditional medicine composition composition dropping pills 1g, put in the mortar, the 5～10ml that adds diethyl ether grinds, and filters, and filtrating is put in the evaporating dish, flings to ether, and the covering surfaces ware is put in the water-bath and heated, and collects sublimate, adds ethanol 1ml and makes dissolving, as need testing solution; Other gets the borneol reference substance, adds ethanol and processes the solution that every 1ml contains 1mg, as reference substance solution; According to " each 3 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; With cyclohexane: ethyl acetate is 8: 2 a developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast blows to the spot colour developing; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
(2) get 4 of this Chinese traditional medicine composition composition dropping pills and put in the bottle of tool plug, add and be heated to pill in the water-bath that absolute ethyl alcohol 2ml puts 50 ℃ and dissolve, shake up, cool slightly to there being a little deposition to separate out, filter with the syringe-type filter membrane, filtrating is as need testing solution; Other gets frankincense control medicinal material 0.1g, adds absolute ethyl alcohol 2ml, floods 1 hour, and supernatant is as control medicinal material solution; According to " each 5 μ l of above-mentioned two kinds of solution are drawn in the test of 2005 editions one appendix VI B of Chinese pharmacopoeia thin-layered chromatography, put respectively on same silica gel g thin-layer plate; With boiling point 60-90 ℃ sherwood oil is developping agent; Launch, take out, dry; Spray is with 5% vanillic aldehyde sulfuric acid solution, and it is clear that hot blast is heated to the spot colour developing; In the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
(3) according to " appendix a VI of Chinese pharmacopoeia version in 2005 E gas chromatography determination;
Chromatographic condition and system suitability test are stationary phase with the carbowax-20M, and coating concentration is 10%; 140 ℃ of column temperatures.
It is an amount of that correction factor mensuration precision takes by weighing n-pentadecane, adds ethyl acetate and process the solution that every 1ml contains 5mg, as inner mark solution; Other gets borneol reference substance 10mg, accurate claims surely, puts in the 5ml measuring bottle, adds inner mark solution 1ml and makes dissolving and add ethyl acetate and be diluted to scale, shakes up, and draws 2-4 μ l, inject gas chromatograph, the calculation correction factor;
Assay method gets that this Chinese traditional medicine composition composition dropping pills 0.5g is accurate to be claimed surely, and add water 10ml and make dissolving, with 8ml, 5ml, 5ml, 5ml ethyl acetate extraction four times, constant volume 25ml volumetric flask; Precision measure 5ml add in mark 1ml shake up, draw 2-4 μ l, inject gas chromatograph is measured, and promptly gets;
Wherein, above-mentioned Chinese medicine composition is made up of following weight portion bulk drug:
Storax 50～100 weight portions, borneol 100～150 weight portions, frankincense 80～120 weight portions, agalloch eaglewood 150～200 weight portions, the banksia rose 200～250 weight portions.
3. according to claim 1 or claim 2 the detection method of Chinese medicine composition is characterized in that the preparation method of said composition pill in the detection method is:
Following storax, borneol, frankincense, agalloch eaglewood, the banksia rose five tastes, except that storax, borneol, three flavors such as all the other frankincenses add 10 times of water gagings and extracted volatile oil 6 hours, and the dregs of a decoction extract secondary with 4 times of amount 80% alcohol heating reflux respectively, and each 2 hours,
Filter, filtrate recycling ethanol is 1.25～1.30 thick paste to not having the alcohol flavor, being evaporated to relative density, drying; Be ground into fine powder, add storax, borneol and Macrogol 6000 matrix 220 weight portions, be heated to dissolving, add volatile oil such as above-mentioned frankincense again; Mixing is processed dripping pill, promptly gets.
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| CN1362196A (en) * | 2001-01-02 | 2002-08-07 | 杨孟君 | Nano Guanxinsuhe medicine and its preparation |
| CN1626138A (en) * | 2003-12-11 | 2005-06-15 | 天津天士力制药股份有限公司 | Medication for treating coronary heart disease and angina |
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| CN1362196A (en) * | 2001-01-02 | 2002-08-07 | 杨孟君 | Nano Guanxinsuhe medicine and its preparation |
| CN1626138A (en) * | 2003-12-11 | 2005-06-15 | 天津天士力制药股份有限公司 | Medication for treating coronary heart disease and angina |
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| 中华人民共和国卫生部药典委员会.冠心苏合滴丸.《中华人民共和国卫生部药品标准中药成方制剂第12册》.1997,146. * |
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