CN1751608A - Traditional Chinese medicine additive for cigarette, its prepn. method and quality control method - Google Patents
Traditional Chinese medicine additive for cigarette, its prepn. method and quality control method Download PDFInfo
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Abstract
A Chinese-medicinal additive of cigarette for promoting blood circulation and preventing coronary heart disease and angina pectoris is prepared from Chuan-xiong rhizome, red peony root, giant knotweed rhizome, cinnamon twig and borneol. Its preparing process and quality control method are also disclosed.
Description
Technical field
The present invention relates to a kind of cigarette Chinese medicine additive and preparation method thereof and method of quality control, particularly a kind of cigarette Chinese medicine additive that is used to have function of promoting blood circulation to disperse blood clots and preparation method thereof and method of quality control.
Background technology
The harm of smoking human health.The scientific evidence that is accumulated from phase early 1950s has shown have the disease more than 25 kinds to be sure of or extremely suspect to be to be caused by smoking.Because of burning and sucking annual nearly 2,500,000 people of the dead number of tobacco, wherein the death rate of angiocardiopathy and lung cancer is the highest.Thereby the promotion smoking cessation has become must taking action of world trends and human self-protection.Although but harm of smoking is widely known by the people, the activity of inner control tobacco produces little effect in the world, and global cigarette consumption figure has turned over some in the period of 1967～1992.Smoker's number of China also rises to more than 300,000,000, and the tendency that becomes younger, and women smoker also increases year by year.Therefore smoking is remaining part crowd's social life hobby at present, so we when conducting vigorous propaganda smoking cessation, should adopt modern science and technology to develop a kind of compound type cigarette with Chinese herb feed additive.It both can improve the sanitary condition of smoking, reduce the harm of smoking to human body, improve the security of smoking, can satisfy the demand in market again, and prediction is along with the raising of people's quality of life, the enhancing of self health consciousness and will have the bigger vitality and the market competitiveness to this product of pursuit of smoking security, Chinese herb feed additive can lower or improve the smoker to tar on the other hand, most Gu Ding etc. inhale the pursuit of flavor, thereby realize substituting smoking cessation gradually, China's traditional chinese medicine is the treasure-house of a greatness, Chinese medicine with special efficacy added to make hypotoxicity in the pipe tobacco, health cigarette replaces regular-size cigarette, both can improve security of products, simultaneously with health role, can meet the need of market again, this is that present production of cigarettes and product are practical, effective improved route, also symbol country is to the action plan of cigarette product technological innovation.
Summary of the invention
One object of the present invention is to disclose a kind of cigarette Chinese medicine additive; Another object of the present invention is to disclose a kind of cigarette Chinese medicine additive that is used to have function of promoting blood circulation to disperse blood clots; The 3rd purpose of the present invention is to disclose a kind of preparation method of cigarette Chinese medicine additive, and the 4th purpose of the present invention is to disclose a kind of method of quality control of cigarette Chinese medicine additive.
The raw material of cigarette Chinese medicine additive of the present invention is formed and proportioning following (by weight):
Ligusticum wallichii 280-380 weight portion radix paeoniae rubrathe 140-190 weight portion tiger battle 140-190 weight portion
Cassia twig 70-95 weight portion borneol 5-10 weight portion
It is (by weight) that the raw material of cigarette Chinese medicine additive of the present invention is formed optimum ratio:
The Ligusticum wallichii 370 weight portion radix paeoniae rubrathe 145 weight portions tiger battle 185 weight portions
Cassia twig 75 weight portion borneols 9 weight portions
It is (by weight) that the raw material of cigarette Chinese medicine additive of the present invention is formed optimum ratio:
The Ligusticum wallichii 290 weight portion radix paeoniae rubrathe 185 weight portions tiger battle 145 weight portions
Cassia twig 90 weight portion borneols 6 weight portions
It is (by weight) that the raw material of cigarette Chinese medicine additive of the present invention is formed optimum ratio:
The Ligusticum wallichii 330 weight portion radix paeoniae rubrathe 165 weight portions tiger battle 165 weight portions
Cassia twig 82 weight portion borneols 8 weight portions
The preparation method of this cigarette Chinese medicine additive:
With Ligusticum wallichii, the radix paeoniae rubrathe, tiger battle, cassia twig is cataclasm, the ethanolic solution that wash quickly is placed on 60-80% only covered the medicinal material surface and got final product, and soaked 18-36 hour in 40～45 ℃ of temperature; With the immersion liquid of 3-5 layer filtered through gauze, obtain filtrate V1, dregs of a decoction squeezing, pressed liquor obtains filtrate V2 with 3-5 layer filtered through gauze, merges V1 and V2 airtight preservation in container; The dregs of a decoction are with the alcohol reflux of the 60-80% of 2-4 times of weight 2-4 time, and each 0.5-1.5 hour, all use 3-5 layer filtered through gauze after each the backflow, merge and filter gained filtrate; Backflow gained filtrate obtains concentrate V3 in decompression recycling ethanol below 60 ℃; The take a morsel amalgamation liquid of V1 and V2 adds borneol, and stirring and dissolving is made borneol liquid; Concentrate V3 is under agitation merged with V1, V2, borneol liquid is under agitation added amalgamation liquid very slowly, filter, sterilize, promptly get this Chinese medicine additive soup.
The method of quality control of this cigarette Chinese medicine additive contains one or more in following discriminating and/or the content assaying method, and discriminating in the method for quality control of the present invention and content assaying method are:
Discrimination method is selected from one or more in the following method:
A, get this Chinese medicine additive soup 10ml, add water 20ml, with extracted by ether 2 times, each 20m1 merges ether extracted liquid, waves most ether for 50 ℃, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution; Other gets Ligusticum wallichii control medicinal material meal 1g, the 20ml that adds diethyl ether, and backflow 15-30 minute, filter, filtrate evaporate to dryness, residue add ethyl acetate 2ml makes dissolving, as shining medicinal material solution; Test according to thin-layered chromatography (appendix VIB), draw each 2ul of above-mentioned solution, put respectively in-be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, intoxicated with the n-hexane-acetic acid second of 8-9:1-2 ratio is solvent, launches, and takes out, dry, put under the ultraviolet lamp (365nm) and inspect, the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
B, get this Chinese medicine additive soup 10ml, add water 20ml, with ether 20ml washing, the aqueous solution extracts 2 times with water-saturated n-butanol again, each 20ml merges n-butanol liquid, water bath method, and residue dissolves with small amount of ethanol, add neutral alumina 2g, mix thoroughly, evaporate to dryness, be contained in post (200～300 orders, 1g, the internal diameter 10mm of neutral alumina, dry column-packing) on, uses the 40ml methanol-eluted fractions, collect eluent, put evaporate to dryness in the water-bath, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the Paeoniflorin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw each 5ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 42-48: 4-6: 8-12: the chloroform-ethyl acetate of 0.1-0.3 ratio-methyl alcohol-formic acid is solvent, launches, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
C, get this Chinese medicine additive soup 10ml, put and steam in the water-bath, add 2.5mol/1, sulfuric acid solution 20ml to there not being the alcohol flavor, heating hydrolysis 20-40 minute, put cold, with extracted by ether 2 times, each 20ml, merge ether solution, evaporate to dryness, residue add absolute ethyl alcohol 2ml makes dissolving, as need testing solution; Other gets archen and Physcion reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw need testing solution and medicinal material solution and medicinal material 10ul, each 2ul of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 12-18: 3-6: the benzinum of 1-2 ratio (30～60 ℃)-Ethyl formate-formic acid is solvent, launch, take out, dry, put in the ammonia steam smoked after, inspect under the daylight, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
D, get and differentiate that need testing solution is differentiated need testing solution as this under a item; Other gets the cinnaldehydrum reference substance, adds ethanol and makes the solution that every 1ml contains 1ul, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw above-mentioned need testing solution 4ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 12-18: 3-6: the benzinum of 1-2 ratio (30～60 ℃)-Ethyl formate-formic acid is solvent, launches, and takes out, dry, spray is with dinitrophenylhydrazine ethanol test solution; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
E, get and differentiate that need testing solution is differentiated need testing solution as this under a item; Other gets the borneol reference substance, adds ethanol and makes the solution that every 1ml contains 10mg, in contrast product solution; Draw each 3ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 15-18: the cyclohexane-ethyl acetate of 2-5 ratio is a solvent, launch, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
Content assaying method is:
Get the about 5mg of archen reference substance, the accurate title, decide, and puts in the 50ml measuring bottle, adds methyl alcohol to scale, shakes up, and promptly gets reference substance solution; Precision is measured this Chinese medicine additive soup 2ml, put in the 100ml round-bottomed flask, ethanol is flung in the water-bath heating, adds 2.5mol/1 sulfuric acid solution 20ml, adds hot reflux 0.5-2 hour, cold slightly, add the about 30ml of chloroform, continue backflow 1-3 hour, cooling, move in the separatory funnel, use the minimum of chloroform washing container, washing lotion is incorporated in the separatory funnel, divides and gets in the chloroform stratification 50ml measuring bottle, acid solution is extracted 2 times with chloroform, each about 8ml, chloroform solution is incorporated in the 50ml measuring bottle, adds chloroform to scale, shake up, promptly get need testing solution; Precision is measured reference substance solution 2ml and 3ml, flings to methyl alcohol; Precision is measured need testing solution 5ml, evaporate to dryness in addition; Each accurate mixed in equal amounts solution 20ml that adds 2% ammonia solution and 5% sodium hydroxide solution of above-mentioned three parts of residues makes dissolving, filter, get subsequent filtrate, with reagent is blank, wavelength place at 520nm measures trap respectively, calculate this Chinese medicine additive soup and contain general anthraquinone, must not be less than 0.1% (1mg/ml) in archen (C15H10O50).
Cigarette Chinese medicine additive soup of the present invention after the tobacco leaf chopping, adding during reinforced perfuming, soup is 0.1～1% to the ratio of tobacco leaf, the oven dry pipe tobacco can use.Add that cigarette of the present invention has that blood-activating and qi-promoting, stagnation resolvation are promoted blood circulation, the effect of promoting qi circulation and relieving pain, nourishing qi and blood, the flue gas pharmacological tests of pharmacodynamics test and medicine pipe tobacco shows: the product that this cigarette Chinese medicine additive adds behind the cigarette can reduce whole blood adhesiveness and antiplatelet adhesiveness, help improving ischemic myocardium blood supply oxygen supply, can play the effect that improves coronary heart disease due to the blood-vessel obstructive, angina pectoris syndrome.
Cigarette product (the feudal dynasty medicine cigarette) pharmacodynamics that adds behind this cigarette Chinese medicine additive is partly carried out Primary Study, experimental studies results proves: 1～3/day of rat inhalation cigarette, 0.5～1/day of mouse inhalation cigarette, continuous 12 days, have function of promoting blood circulation to disperse blood clots, visible following index changes:
1, improves hemorheology index: big mouse cruor time extending; Reduce the rat erythrocyte aggregation index, reduce the high, medium and low viscosity of cutting of whole blood;
2, suppress thrombosis: the dry weight of rat arteriovenous thrombus loop thrombus, weight in wet base are reduced;
3, suppress platelet aggregation: the platelet aggregation that ADP is induced has obvious inhibitory action, reduces PAR;
4, isoprel is caused rats with myocardial ischemia protective effect is arranged: reduce the generation of lipid peroxide, improve electrocardiogram (suppressing the rising of T ripple and the rising of S-T section).
Following experimental example is used to further specify but does not limit the present invention:
1. medicine:
Feudal dynasty medicine cigarette, feudal dynasty board cigarette: cigar mill provides by the South Sea, Guangdong
Feudal dynasty medicine cigarette aqueous extract (self-control): 5 medicine cigarette decoctings boil to 200ml.
2. animal:
The ICR mouse, male, 16-18g is provided by Beijing Vital River Experimental Animals Technology Co., Ltd.,
The quality certification number: SCDK (capital) 2002-0003.
3. instrument:
The miniature artificial respirator of gulf, river I type (teaching material section of The 2nd Army Medical College product) is lighted smoking apparatus through transforming as; Big drier.
The miniature artificial respirator of gulf, river I type (teaching material section of The 2nd Army Medical College product) is lighted smoking apparatus through transforming as; The glass closed box.
RBC distortion/gathering tester, model LG-B-190, Beijing generation Supreme Being scientific instrument company product; The blood viscosity instrument, model R-80, Beijing generation Supreme Being scientific instrument company product; The 400R refrigerated centrifuge, German Heraeus product.
AEG-220 type electronic analytical balance, day island proper Tianjin instrument company product; Df-206 type air dry oven, west city, Beijing medical apparatus and instruments factory product.
LG-PABER-1 type platelet aggregation/agglutometer, Beijing generation Supreme Being scientific instrument company product; The 400R refrigerated centrifuge, German Heraeus product.
722 type spectrophotometers, Shanghai the 3rd analytical instrument factory product; The 400R refrigerated centrifuge, German Heraeus product.
MedLab physiological signal acquisition system, Meiyi Science ﹠ Technology Co., Ltd., Nanjing's product, MedLab-U/4c
Experimental example 1: feudal dynasty medicine cigarette sucks the influence to clotting time of mice
1. grouping and administration
Animal is divided into five groups at random, i.e. control group, 1/day of inhalation, 0.5/day group, 1.5/day of gastric infusions, 0.75/day group.Successive administration 12 days was surveyed the clotting time after the last administration in one hour.Inhalation is lighted cigarette with lung ventilator, is blown in the big drier, and mouse kept in the drier 30 minutes.Other gets feudal dynasty medicine cigarette aqueous extract 0.2ml/10g and irritates stomach once every day, and promptly 1.5/day/kg dilutes one times of i.e. 0.75/day/kg.Control group gives the equivalent drinking water.
2. coagulation time test
The last administration was measured the clotting time with capillary tube method after one hour.
3. result
The results are shown in Table 1
Table 1, feudal dynasty medicine cigarette are to the influence of clotting time of mice
| Group | Method of administration | Dosage | Number of animals | Clotting time |
| Medicine cigarette group feudal dynasty control group feudal dynasty medicine cigarette extract | -suck and irritate stomach filling stomach | 0.75/day/kg of-1/day 0.5/day 1.5/day/kg | 14 13 14 12 14 | 44.93±14.24 110±39.46** 91±45.13** 56.75±16.52 46.07±25.75 |
Annotate: compare * * p＜0.01 with control group
The result shows: feudal dynasty medicine cigarette inhalation can obviously prolong the clotting time of mouse, and be certain dose-effect relationship, (comparing p＜0.01 with control group), feudal dynasty medicine cigarette water extract gastric infusion prolongs the DeGrain (comparing p＞0.05 with control group) of clotting time of mice.Presentation of results, the active ingredient in the medicine cigarette is better than the alimentary canal administration through the inhalation effect.
Experimental example 2: feudal dynasty medicine cigarette is to the influence in rat clotting time
1. grouping and administration
Animal is divided into six groups at random, i.e. control group, feudal dynasty board cigarette group (sucking 3/day of feudal dynasty board cigarettes), feudal dynasty medicine cigarette group (sucking 3,2,1/day of feudal dynasty medicine cigarettes respectively) group, compound injection of red sage root group (1.5ml/kg/ days).Feudal dynasty board cigarette group, feudal dynasty medicine cigarette group inhalation with lung ventilator, suck cigarette, are blown in the glass closed box, and rat kept in the glass closed box 30 minutes, successive administration 12 days.Compound injection of red sage root intraperitoneal injection 3 days, 1 time/day, control group does not deal with.
2. coagulation time test
The last administration was measured the clotting time with capillary tube method after one hour.
3. result
See Table 2
Table 2, feudal dynasty medicine cigarette are to the influence in rat clotting time
| Group | Dosage | Number of animals | Clotting time (s) |
| Board cigarette group feudal dynasty control group feudal dynasty medicine cigarette group compound injection of red sage root | -3/day 3/day 2/day 1/day 1.5ml/kg | 13 12 16 16 16 16 | 139.46±49.12 135.58±23.98 160.44±21.89** 158.25±24.94* 168.63±29.87** 163.60±31.68* |
Annotate: compare * p＜0.05, * * p＜0.01 with feudal dynasty board cigarette
The result shows: each dosage group inhalation of feudal dynasty medicine cigarette is the prolong rats clotting time (comparing p＜0.01, p＜0.05 with feudal dynasty board cigarette group) obviously, and feudal dynasty board cigarette does not have obvious influence to the rat clotting time.
Experimental example 3: feudal dynasty medicine cigarette is to the influence of hemorheology of rat
1. grouping and administration
Animal is divided into six groups at random, i.e. control group, feudal dynasty board cigarette group (sucking 3/day of feudal dynasty board cigarettes), feudal dynasty medicine cigarette group (sucking 3,2,1/day of feudal dynasty medicine cigarettes respectively) group, compound injection of red sage root group (1.5ml/kg/ days).Feudal dynasty board cigarette group, feudal dynasty medicine cigarette group inhalation with lung ventilator, suck cigarette, are blown in the glass closed box, and rat kept in the glass closed box 30 minutes, successive administration 12 days.Compound injection of red sage root intraperitoneal injection 3 days, 1 time/day, control group does not deal with.One hour capable arteria carotis intubation is got blood, anticoagulant heparin after the last administration.
2. the mensuration of RCD and aggregation
Get anticoagulation 40 μ l and add RBC deformation liquid 1ml, mixing, sampling 0.8ml is with RBC deformation/gathering tester test, with red blood cell maximum distortion index (MAXDI) expression RCD; Other gets anticoagulation 0.8ml and tests with RBC deformation/gathering tester, with the maximum aggregate index of red blood cell (MAXD) expression erythrocyte aggregation.The result relatively, carries out the t check between organizing, and the results are shown in Table 3.
3. blood Viscosity Determination
Get anticoagulation 0.8ml and detect with blood viscosity instrument, with height cut (200S-1), in cut (30S-1) and low when cutting (5S-1) blood viscosity represent WBV; Other gets anticoagulation and leaves heart 8min with 2000, and its supernatant is blood plasma, the plasma viscosity when getting 0.8ml blood plasma with blood viscosity instrument test 100S-1.The result relatively, carries out the t check between organizing, and the results are shown in Table 4,5.
4. result
The results are shown in Table 3,4
Table 3 feudal dynasty medicine cigarette is to the influence of rat RCD and aggregation (X ± SD)
| Group | Dosage | Number of animals | Deformable index | Erythrocyte aggregation index |
| Board cigarette group feudal dynasty control group feudal dynasty medicine cigarette group compound injection of red sage root group | -3/day 3/day 2/day 1/day 1.5ml/kg | 13 12 16 16 16 16 | 0.79±0.03 0.79±0.02 0.78±0.02 0.77±0.03 0.77±0.03 0.78±0.05 | 0.39±0.12 0.42±0.08 0.33±0.10* 0.36±0.10 0.30±0.08** 0.39±0.09 |
Annotate: compare * * p＜0.01, * p＜0.05 with feudal dynasty board cigarette group
The result shows: feudal dynasty medicine cigarette can reduce the rat erythrocyte aggregation index, and wherein large and small dosage group has been compared significant difference (p＜0.01, p＜0.05) with feudal dynasty board cigarette group.
Table 4 feudal dynasty medicine cigarette is to the influence of rat WBV (X ± SD)
| Group | Dosage | n | WBV | ||
| Height is cut (200S-1) | In cut (30S-1) | Low cut (5S-1) | |||
| Board cigarette group feudal dynasty control group feudal dynasty medicine cigarette group compound injection of red sage root group | -3/day 3/day 2/day 1/day 1.5ml/kg | 13 12 16 16 16 16 | 3.91±0.45 4.11±0.64 3.89±0.48 3.64±0.44* 3.73±0.48 3.77±0.32 | 5.40±0.55 5.75±0.92 5.40±0.72 5.23±0.75 5.14±0.56* 5.28±0.58 | 9.89±1.24 10.72±1.92 9.97±1.77 10.13±2.13 9.36±0.93* 9.86±1.66 |
Annotate: compare * p＜0.05 with feudal dynasty board cigarette group
The result shows: dosage can obviously reduce rat whole blood height and cuts viscosity in the feudal dynasty medicine cigarette, and low dose can obviously reduce in the rat whole blood, the low viscosity (comparing p＜0.05 with feudal dynasty board cigarette group) of cutting.
Experimental example 4: feudal dynasty medicine cigarette is to the influence of rat artery-vein bypass thrombus
1. grouping and administration
Animal is divided into six groups at random, i.e. control group, feudal dynasty board cigarette group (sucking 3/day of feudal dynasty board cigarettes), feudal dynasty medicine cigarette group (sucking 3,2,1/day of feudal dynasty medicine cigarettes respectively), compound injection of red sage root group (1.5ml/kg/ days).Feudal dynasty board cigarette group, feudal dynasty medicine cigarette group inhalation with lung ventilator, suck cigarette, are blown in the glass closed box, and rat kept in the glass closed box 30 minutes, successive administration 12 days.Compound injection of red sage root intraperitoneal injection 3 days, 1 time/day, control group does not deal with.
2. modeling method
Get experiment after the last administration in one hour and use rat, lumbar injection 10% chloraldurate 0.35ml/100g anesthesia, dorsal position is fixed, operation, separation RCCA and left vena jugularis externa.Put into No. 0 surgical thread of a long 8cm who weighs in advance in the long polyethylene pipe stage casing of 10cm, be full of with normal saline solution, two client links are about the intubate that 3cm is full of normal saline solution.After one end of this pipe inserted left vena jugularis externa, the other end inserted RCCA.Blood flow in the polyethylene pipe from right carotid, backflows into left vena jugularis externa again, constitutes the loop blood flow.Clinopodium polycephalum in behind the 10min, removal of thromboses is weighed rapidly, and this weight deducts the silk thread weight, paper heavily is wet weight of thrombus; Put into 60 ℃ of dry 24h of baking oven, removal of thromboses is weighed, and this weight deducts the silk thread weight, paper heavily is the thrombus dry weight.Each organizes equal computation of mean values, standard error.Adopt the t-check to compare between group.
3. result
The results are shown in Table 5
Table 5, feudal dynasty medicine cigarette are to the inhibitory action of rat arteriovenous loop thrombus (X ± SD)
| Group | Dosage | n | Wet weight of thrombus (mg) | Thrombus dry weight (mg) |
| Feudal dynasty board cigarette group control group feudal dynasty medicine cigarette group compound injection of red sage root group | 3/day 1/day 2/day 3/day 1.5ml/kg | 9 12 9 12 10 9 | 179.8±91.1 155.3±63.4 80.1±32.9*## 85.8±32.3**## 101.7±51.4* 110.6±50.5 | 35.8±19.1# 30.8±14.3* 13.1±7.2## 14.7±8.0## 18.0±12.7*# 19.7±11.9* |
Annotate: compare * * p＜0.01, * p＜0.05 with feudal dynasty board cigarette group; Compare ##p＜0.01 with control group, #p＜0.05
The result shows: feudal dynasty board cigarette group rat suppository dry weight obviously increases (comparing p＜0.05 with control group), but each dosage group of feudal dynasty medicine cigarette can obviously reduce rat suppository weight in wet base (comparing p＜0.05 with feudal dynasty board cigarette group), and low dose can obviously reduce rat suppository dry weight (comparing p＜0.05 with feudal dynasty board cigarette group).Compare in the feudal dynasty medicine cigarette with control group, small dose group rat suppository weight in wet base also has obvious reduction (comparing p＜0.01 with control group); Each dosage group rat suppository dry weight also has obvious reduction (comparing p＜0.01 with control group, p＜0.05).
Experimental example 5: feudal dynasty medicine cigarette is to the influence of ADP and collagen-induced rat platelet aggregation
1. grouping and administration
Animal is divided into six groups at random, i.e. negative control group, feudal dynasty board cigarette group (sucking 3/day of feudal dynasty board cigarettes), feudal dynasty medicine cigarette group (sucking 3,2,1/day of feudal dynasty medicine cigarettes respectively), compound injection of red sage root group (1.5ml/kg/ days).Feudal dynasty board cigarette group, feudal dynasty medicine cigarette group inhalation with lung ventilator, suck cigarette, are blown in the glass closed box, and rat kept in the glass closed box 30 minutes, successive administration 12 days.Compound injection of red sage root intraperitoneal injection 3 days, 1 time/day, negative control group does not deal with.Surveyed the clotting time in one hour after the last administration.
2. collagen preparation
Get one on rat tail, peel crust, strike off scale and fat inside, and shred.Weigh, ground down at 4 ℃ behind the adding physiological saline by 1: 9, to milky, 4 ℃ of centrifugal 10min of 1500g get i.e. 10% collagen of supernatant.
3. the mensuration (Born turbidimetry) of modeling and ADP and collagen-induced platelet aggregation
The arteria carotis communis bloodletting, with 3.8% sodium citrate (V/V is 1: 9) anti-freezing, the centrifugal 10min of 150g, supernatant are platelet rich plasma (PRP), residue blood plasma continues with the centrifugal 10min of 1500g, supernatant is platelet poor plasma (PPP), with the PPP zeroing, gets PRP 300 μ l and adds opacity tube, 37 ℃ of incubation 5min, add the ADP 5 μ l of derivant 20 μ mol/L and 10% collagen 30 μ l respectively, assemble 5min, 10min respectively, the record MA.The results are shown in Table 6.
4. result
The results are shown in Table 6
Table 6 feudal dynasty medicine cigarette is to the influence of ADP and collagen-induced rat platelet aggregation (X ± SD)
| Group | Dosage | n | COL(％) | ADP(％) |
| Feudal dynasty board cigarette group negative control group feudal dynasty medicine cigarette group compound injection of red sage root group | 3/day-1/day 2/day 3/day 0.6ml/kg | 11 15 15 16 16 15 | 66.7±15.1 55.0±14.1 59.8±20.5 53.9±19.7 65.7±15.2 66.0±14.7 | 44.0±7.4# 36.7±8.1* 42.5±11.6 38.2±8.3 31.1±15.1* 33.8±10.7* |
Annotate: compare * * p＜0.01 with feudal dynasty board cigarette group, #p＜0.05 is compared in * p＜0.05 with negative control group
The result shows: the platelet aggregation that feudal dynasty medicine cigarette heavy dose is induced ADP has obvious inhibitory action (comparing p＜0.05 with feudal dynasty board cigarette group).Compound injection of red sage root can obviously suppress the platelet aggregation (comparing p＜0.05 with feudal dynasty board cigarette group) that ADP induces.Feudal dynasty board cigarette group is compared the platelet aggregation that ADP is induced and is obviously strengthened (comparing p＜0.05 with negative control group) with negative control group.
Experimental example 6: feudal dynasty medicine cigarette causes the influence of rats with myocardial ischemia cardiac muscle biochemical indicator to isoprel
1. grouping and administration
Animal is divided into six groups at random, 16 every group; Be control group, feudal dynasty board cigarette group (sucking 3/day of feudal dynasty board cigarettes), feudal dynasty medicine cigarette group (sucking 3,2,1/day of feudal dynasty medicine cigarettes respectively) group, compound injection of red sage root 1.5ml/kg.Feudal dynasty board cigarette group, feudal dynasty medicine cigarette group inhalation with lung ventilator, suck cigarette, are blown in the glass closed box, and rat kept in the glass closed box 30 minutes, successive administration 12 days.Compound injection of red sage root intraperitoneal injection 3 days, 1 time/day, control group does not deal with.One hour begins to test after the last administration.
2. modeling
Rat is used in experiment, hypodermic injection hydrochloric acid isoproterenol parenteral solution 1m/kg twice, once/day.Last was injected back 24 hours, put to death animal and got left compartment muscle.Add 9 times of physiological saline and be prepared into 10% homogenate, it is standby to be diluted to 2%, 1% homogenate again.
3. protein quantification
With 1% tissue homogenate, the centrifugal 10min of 4000rpm gets supernatant 50 μ l, measures protein content with Coomassie brilliant blue.Calculate the content that contains SOD in every g albumen.
4. the mensuration of lactic acid (LD)
With 10% tissue homogenate, the centrifugal 10min of 4000rpm gets supernatant 20 μ l, presses LD and measures kit explanation mensuration LD content.The results are shown in Table 7.
5. the mensuration of lactic dehydrogenase (LDH)
Tissue homogenate with 2%, the centrifugal 10min of 4000rpm gets supernatant 10 μ l, presses LDH and measures kit explanation mensuration LDH content.The results are shown in Table 7.
6. the mensuration of superoxide dismutase (SOD)
Tissue homogenate with 1%, the centrifugal 10min of 4000rpm gets supernatant 20 μ l, presses SOD and measures kit explanation mensuration SOD content.The results are shown in Table 7.
7. the mensuration of lipid peroxide (LPO)
With the centrifugal 10min of 10% tissue homogenate 4000rpm, get supernatant 100 μ l, press MDA and measure kit explanation mensuration MDA content.The results are shown in Table 7.
Table 7 feudal dynasty medicine cigarette causes the influence of rats with myocardial ischemia cardiac muscle LD, LDH to isoprel
| Group | Dosage | n | LDH (u/mgprot) | LD (mmol/gprot) |
| Board cigarette group compound injection of red sage root group feudal dynasty control group feudal dynasty medicine cigarette group | 3/day 2/day 1/day of 3/day 1.5ml/kg | 17 9 11 10 12 10 | 750.26±167.77** 977.71±112.05 848.09±63.85** 961.97±77.93 889.24±113.36 887.03±136.59 | 0.23±0.08 0.25±0.10 0.21±0.04 0.24±0.09 0.18±0.06 0.21±0.07 |
Annotate: compare * * p＜0.01, * p＜0.05 with feudal dynasty board cigarette group
The result shows: after the modeling, feudal dynasty board cigarette group LDH, LD content are all apparently higher than control group, and feudal dynasty medicine cigarette each dosage LDH, LD all are lower than feudal dynasty board cigarette group.
Table 8 feudal dynasty medicine cigarette causes the influence of rats with myocardial ischemia SOD of heart tissue, MDA to isoprel
| Group | Dosage | n | SOD (NU/mgprot) | MDA (nmol/mgprot) |
| Board cigarette group compound injection of red sage root group feudal dynasty control group feudal dynasty medicine cigarette group | 3/day 2/day 1/day of 3/day 1.5ml/kg | 17 9 11 10 12 10 | 837.76±183.38 921.37±212.20 844.06±123.82 1055.79±133.12 915.13±183.05 869.81±151.90 | 0.70±0.33** 1.23±0.34 0.85±0.27* 0.96±0.25 0.88±0.27* 0.72±0.25** |
Annotate: compare * * p＜0.01, * p＜0.05 with feudal dynasty board cigarette group
The result shows: after the modeling, feudal dynasty board cigarette group MDA content is all apparently higher than control group (p＜0.01), each dosage MDA content of feudal dynasty medicine cigarette all is starkly lower than feudal dynasty board cigarette group, wherein in, small dose group effect the most obvious (comparing p＜0.05, p＜0.01) with feudal dynasty board cigarette group.
Experimental example 7: feudal dynasty medicine cigarette causes the Electrocardiographic influence of rats with myocardial ischemia to isoprel
1. grouping and administration
Animal is divided into six groups at random, 16 every group; Be control group, feudal dynasty board cigarette group (sucking 3/day of feudal dynasty board cigarettes), feudal dynasty medicine cigarette group (sucking 3,2,1/day of feudal dynasty medicine cigarettes respectively), compound injection of red sage root group (1.5ml/kg/ days).Feudal dynasty board cigarette group, feudal dynasty medicine cigarette group inhalation with lung ventilator, suck cigarette, are blown in the glass closed box, and rat kept in the glass closed box 30 minutes, successive administration 12 days.Compound injection of red sage root intraperitoneal injection 3 days, 1 time/day, control group does not deal with.One hour begins to test after the last administration.
2. experimental technique
Rat use in experiment, lumbar injection 10% chloraldurate 0.35ml/100g anesthesia, dorsal position is fixed, and connects instrument, traces electrocardiogram, treat steadily after, sublingual vein is injected hydrochloric acid isoproterenol parenteral solution 1m/kg.Trace electrocardiogram 30min continuously, before the record modeling, after the modeling 5,10,15,20,25,30min electrocardiogram T amplitude, the intersegmental phase changing value of S-T (after the modeling before parameter-modeling parameter)
3. result
The results are shown in Table 9,10
The result shows: after the modeling, each is organized the T wave amplitude and all obviously raises at each time point, and feudal dynasty each dosage of medicine cigarette all can suppress the rising of T wave amplitude, and has compared obvious significant difference (p＜0.05) at a plurality of time points with feudal dynasty board cigarette group.After the modeling, feudal dynasty board cigarette group S-T section all raises at each time point, in the feudal dynasty medicine cigarette, the low dose of rising that all can suppress the S-T section, and has compared obvious significant difference (p＜0.05) at a plurality of time points with feudal dynasty board cigarette group.
Table 9 feudal dynasty medicine cigarette causes the influence of rats with myocardial ischemia ECG T wave changes in amplitude to isoprel
| Group | Dosage | n | 5min | 10min | 15min | 20min | 25min | 30min |
| Board cigarette group feudal dynasty feudal dynasty medicine cigarette group compound injection of red sage root group control group | 3/day 3/day 2/day 1/day 1.5ml/kg- | 11 11 12 11 11 8 | 0.08±0.05 0.01±0.09 0.04±0.11 0.00±0.11* -0.01±0.12* 0.01±0.04** | 0.10±0.05 0.03±0.09* 0.03±0.08* 0.04±0.09 0.04±0.09 0.01±0.02*** | 0.10±0.04 0.04±0.08 0.04±0.09 0.03±0.09* 0.01±0.15 -0.02±0.08** | 0.10±0.04 0.03±0.08* 0.03±0.09* 0.04±0.07* 0.02±0.16 -0.01±0.09** | 0.10±0.04 0.05±0.08 0.04±0.10 0.05±0.07* 0.02±0.14 0.01±0.05** | 0.08±0.04 0.05±0.07 0.04±0.10 0.05±0.06 0.08±0.08 0.03±0.04* |
Annotate: compare * * p＜0.01, * p＜0.05 with feudal dynasty board cigarette group
Table 10 feudal dynasty medicine cigarette causes the influence that rats with myocardial ischemia electrocardiogram S-T section changes to isoprel
| Group | Dosage | n | 5min | 10min | 15min | 20min | 25min | 30min |
| Board cigarette group feudal dynasty feudal dynasty medicine cigarette group compound injection of red sage root group control group | 3/day 3/day 2/day 1/day 1.5ml/kg- | 11 11 12 11 11 8 | 0.03±0.07 0.01±0.03 0.00±0.02 0.01±0.02 0.00±0.03 0.01±0.01 | 0.01±0.03 0.01±0.03 0.00±0.03 0.00±0.03 -0.01±0.03 0.01±0.01 | 0.02±0.04 0.00±0.02 0.00±0.03 -0.01±0.01* 0.00±0.05 0.01±0.01 | 0.03±0.05 0.01±0.01 0.01±0.03 -0.01±0.02* -0.01±0.04 0.01±0.01 | 0.03±0.04 0.00±0.02 -0.01±0.02* -0.01±0.01* -0.01±0.03* 0.01±0.02 | 0.02±0.03 0.00±0.02 0.01±0.03 -0.01±0.02 0.00±0.04 0.01±0.01 |
Annotate: compare * * p＜0.01, * p＜0.05 with feudal dynasty board cigarette group
Experimental example 8: Study on extraction and result
1, now ethanol reflux extraction is carried out the optimization of process conditions test:
(1) list of references method, fix two factors earlier: 1. medicinal material is cataclasm, and cold soaking 1 hour is refluxing extraction again; 2. the refluxing extraction number of times is 3 times.
(2) orthogonal test: with concentration of alcohol, solvent load, return time is the investigation factor, and each factor is got three levels, is evaluation index with dry extract yield and Paeoniflorin, carries out L9 (34) orthogonal test.Methods of marking: adopt the weighted comprehensive point system: the test full marks are 100 minutes, and wherein the Paeoniflorin recovery rate accounted for 70 fens, and recovery rate is lower than at 55% o'clock and counts 0 fen, and recovery rate is higher than at 90% o'clock and counts 70 fens; Dried cream yield accounted for 30 fens, considered from the effective extract angle, set dried cream yield and was at 40% o'clock and count 0 fen, and dried cream yield is to count 30 fens at 10% o'clock.Recovery rate and dried cream yield sum are this number test score.Interpretation of result:
(1) level quality: A
2＞A
1＞A
3, B
2＞B
3＞B
1, C
2＞C
1＞C
3
(2) factor primary and secondary: by extreme difference R as can be seen, influence factor is A＞C＞B, and the A factor is to the extraction effect significance, and the C factor is taken second place, B factor affecting minimum.
(3) optimum extraction conditions is: A
2B
2C
2, promptly concentration of alcohol is 70%, and the ethanol consumption is 10 times, and return time is each 1 hour.
Embodiment 1:
Ligusticum wallichii 370g radix paeoniae rubrathe 145g tiger battle 185g cassia twig 75g borneol 9g
The above five tastes are made 1000 milliliters of soups according to conventional method.Soup is after the tobacco leaf chopping, and soup is 0.15% to the ratio of tobacco leaf, adding when feeding in raw material perfuming, and the oven dry pipe tobacco gets final product.
Embodiment 2:
Ligusticum wallichii 290g radix paeoniae rubrathe 185g tiger battle 145g cassia twig 90g borneol 6g
The above five tastes are made 1000 milliliters of cigarette Chinese medicine additive soups according to conventional method.Soup after the tobacco leaf chopping, adding during reinforced perfuming, soup is 0.75% to the ratio of tobacco leaf, the oven dry pipe tobacco gets final product.
Embodiment 3:
Ligusticum wallichii 330g radix paeoniae rubrathe 165g tiger battle 165g cassia twig 82g borneol 8g
The above five tastes are made 1000 milliliters of cigarette Chinese medicine additive soups according to conventional method.Soup after the tobacco leaf chopping, adding during reinforced perfuming, soup is 0.25% to the ratio of tobacco leaf, the oven dry pipe tobacco gets final product.
Embodiment 4:
Ligusticum wallichii 370g radix paeoniae rubrathe 145g tiger battle 185g cassia twig 75g borneol 9g
With Ligusticum wallichii, the radix paeoniae rubrathe, tiger battle, cassia twig is suitably cataclasm, wash quickly is placed in 80% the ethanol only, (solution covered the medicinal material surface and get final product, write down consumption of ethanol) soaked 20 hours in 40～45 ℃ of temperature; With 5 layers of filtered through gauze immersion liquid, obtain filtrate V1, dregs of a decoction squeezing, pressed liquor obtains filtrate V2 with 3 layers of filtered through gauze, merges V1 and V2 airtight preservation in container; The dregs of a decoction are with 60% alcohol reflux of 4 times of weight 4 times, and each 0.5 hour, all use 5 layers of filtered through gauze after each the backflow, merge and filter gained filtrate; Backflow gained filtrate obtains concentrate V3 in decompression recycling ethanol below 60 ℃; The take a morsel amalgamation liquid of V1 and V2 adds borneol, and stirring and dissolving is made borneol liquid; Concentrate V3 is under agitation merged with V1, V2, borneol liquid is under agitation added amalgamation liquid very slowly, filter, sterilize, add absolute ethyl alcohol, promptly get this cigarette Chinese medicine additive soup to 1000ml.Soup after the tobacco leaf chopping, adding during reinforced perfuming, soup is 0.35% to the ratio of tobacco leaf, the oven dry pipe tobacco gets final product.
Embodiment 5:
Ligusticum wallichii 290g radix paeoniae rubrathe 185g tiger battle 145g cassia twig 90g borneol 6g
With Ligusticum wallichii, the radix paeoniae rubrathe, tiger battle, cassia twig is suitably cataclasm, wash quickly is placed in 65% the ethanol only, (solution covered the medicinal material surface and get final product, write down consumption of ethanol) soaked 32 hours in 40～45 ℃ of temperature; With 3 layers of filtered through gauze immersion liquid, obtain filtrate V1, dregs of a decoction squeezing, pressed liquor obtains filtrate V2 with 5 layers of filtered through gauze, merges V1 and V2 airtight preservation in container; The dregs of a decoction are with 80% alcohol reflux of 2 times of weight 2 times, and each 1.5 hours, all use 3 layers of filtered through gauze after each the backflow, merge and filter gained filtrate; Backflow gained filtrate obtains concentrate V3 in decompression recycling ethanol below 60 ℃; The take a morsel amalgamation liquid of V1 and V2 adds borneol, and stirring and dissolving is made borneol liquid; Concentrate V3 is under agitation merged with V1, V2, borneol liquid is under agitation added amalgamation liquid very slowly, filter, sterilize, add absolute ethyl alcohol, promptly get cigarette Chinese medicine additive soup to 1000ml.Soup after the tobacco leaf chopping, adding during reinforced perfuming, soup is 0.45% to the ratio of tobacco leaf, the oven dry pipe tobacco gets final product.
Embodiment 6:
Ligusticum wallichii 330g radix paeoniae rubrathe 165g tiger battle 165g cassia twig 82g borneol 8g
With Ligusticum wallichii, the radix paeoniae rubrathe, tiger battle, cassia twig is suitably cataclasm, wash quickly is placed in 70% the ethanol only, (solution covered the medicinal material surface and get final product, write down consumption of ethanol) soaked 24 hours in 40～45 ℃ of temperature; With 4 layers of filtered through gauze immersion liquid, obtain filtrate V1, dregs of a decoction squeezing, pressed liquor obtains filtrate V2 with 4 layers of filtered through gauze, merges V1 and V2 airtight preservation in container; The dregs of a decoction are with 70% alcohol reflux of 3 times of weight 3 times, and each 1 hour, all use 4 layers of filtered through gauze after each the backflow, merge and filter gained filtrate; Backflow gained filtrate obtains concentrate V3 in decompression recycling ethanol below 60 ℃; The take a morsel amalgamation liquid of V1 and V2 adds borneol, and stirring and dissolving is made borneol liquid; Concentrate V3 is under agitation merged with V1, V2, borneol liquid is under agitation added amalgamation liquid very slowly, filter, sterilize, add absolute ethyl alcohol, promptly get the Chinese medicine additive soup to 1000ml.Soup after the tobacco leaf chopping, adding during reinforced perfuming, soup is 0.25% to the ratio of tobacco leaf, the oven dry pipe tobacco gets final product.
Embodiment 7:The discrimination method of this cigarette Chinese medicine additive:
Get this Chinese medicine additive soup 10ml, add water 20ml, with extracted by ether 2 times, each 20ml merges ether extracted liquid, waves most ether for 50 ℃, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution; Other gets Ligusticum wallichii control medicinal material meal 1g, and the 20ml that adds diethyl ether refluxed 20 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 2ml makes dissolving, as shining medicinal material solution; Test according to thin-layered chromatography (appendix VIB), draw each 2ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, intoxicated with the n-hexane-acetic acid second of 9:1 ratio is solvent, launches, and takes out, dry, put under the ultraviolet lamp (365nm) and inspect, the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
Embodiment 8:The discrimination method of this cigarette Chinese medicine additive:
Get this Chinese medicine additive soup 10ml, add water 20ml, with ether 20ml washing, the aqueous solution extracts 2 times with water-saturated n-butanol again, each 20ml merges n-butanol liquid, water bath method, and residue dissolves with small amount of ethanol, add neutral alumina 2g, mix thoroughly, evaporate to dryness, be contained in post (200～300 orders, 1g, the internal diameter 10mm of neutral alumina, dry column-packing) on, uses the 40ml methanol-eluted fractions, collect eluent, put evaporate to dryness in the water-bath, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the Paeoniflorin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw each 5ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder, with 0.3% sodium carboxymethylcellulose with 45: 5: 10: the chloroform-ethyl acetate of 0.2 ratio-methyl alcohol-formic acid is solvent, launches, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment 9:The discrimination method of this cigarette Chinese medicine additive:
Get this Chinese medicine additive soup 10ml, put and steam in the water-bath, add 2.5mol/1, sulfuric acid solution 20ml to there not being the alcohol flavor, heating hydrolysis 30 minutes, put cold, with extracted by ether 2 times, each 20ml, merge ether solution, evaporate to dryness, residue add absolute ethyl alcohol 2ml makes dissolving, as need testing solution; Other gets archen and Physcion reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw need testing solution and medicinal material solution and medicinal material 10ul, each 2ul of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, benzinum (30～60 ℃)-Ethyl formate-formic acid with 15: 5: 1 ratios is solvent, launch, take out, dry, put in the ammonia steam smoked after, inspect under the daylight, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment 10:The discrimination method of this cigarette Chinese medicine additive:
Get 7 following need testing solutions of embodiment and differentiate need testing solution as this; Other gets the cinnaldehydrum reference substance, adds ethanol and makes the solution that every 1ml contains 1ul, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw above-mentioned need testing solution 4ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, benzinum (30～60 ℃)-Ethyl formate-formic acid with 15: 5: 1 ratios is solvent, launches, and takes out, dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment 11:The discrimination method of this cigarette Chinese medicine additive:
Get 7 following need testing solutions of embodiment and differentiate need testing solution as this; Other gets the borneol reference substance, adds ethanol and makes the solution that every 1ml contains 10mg, in contrast product solution; Draw each 3ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, cyclohexane-ethyl acetate with the 17:3 ratio is a solvent, launch, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment 12:The discrimination method of this cigarette Chinese medicine additive:
A, get this Chinese medicine additive soup 10ml, add water 20ml, with extracted by ether 2 times, each 20m1 merges ether extracted liquid, waves most ether for 50 ℃, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution; Other gets Ligusticum wallichii control medicinal material meal 1g, and the 20ml that adds diethyl ether refluxed 20 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 2ml makes dissolving, as shining medicinal material solution; Test according to thin-layered chromatography (appendix VIB), draw each 2ul of above-mentioned solution, put respectively in-be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, intoxicated with the n-hexane-acetic acid second of 9: 1 ratios is solvent, launches, and takes out, dry, put under the ultraviolet lamp (365nm) and inspect, the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
B, get this Chinese medicine additive soup 10ml, add water 20ml, with ether 20ml washing, the aqueous solution extracts 2 times with water-saturated n-butanol again, each 20ml merges n-butanol liquid, water bath method, and residue dissolves with small amount of ethanol, add neutral alumina 2g, mix thoroughly, evaporate to dryness, be contained in post (200～300 orders, 1g, the internal diameter 10mm of neutral alumina, dry column-packing) on, uses the 40ml methanol-eluted fractions, collect eluent, put evaporate to dryness in the water-bath, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the Paeoniflorin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw each 5ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder, with 0.3% sodium carboxymethylcellulose with 45: 5: 10: the chloroform-ethyl acetate of 0.2 ratio-methyl alcohol-formic acid is solvent, launches, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
C, get this cigarette Chinese medicine additive soup 10ml, put and steam in the water-bath, add 2.5mol/1, sulfuric acid solution 20ml to there not being the alcohol flavor, heating hydrolysis 30 minutes, put cold, with extracted by ether 2 times, each 20ml, merge ether solution, evaporate to dryness, residue add absolute ethyl alcohol 2ml makes dissolving, as need testing solution; Other gets archen and Physcion reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw need testing solution and medicinal material solution and medicinal material 10ul, each 2ul of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, benzinum (30～60 ℃)-Ethyl formate one formic acid with 15: 5: 1 ratios is solvent, launch, take out, dry, put in the ammonia steam smoked after, inspect under the daylight, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
D, get under a item need testing solution and differentiate need testing solution as this; Other gets the cinnaldehydrum reference substance, adds ethanol and makes the solution that every 1ml contains 1ul, in contrast product solution; Test according to thin-layered chromatography (appendix VIB), draw above-mentioned need testing solution 4ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, benzinum (30～60 ℃)-Ethyl formate-formic acid with 15: 5: 1 ratios is solvent, launches, and takes out, dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatogram chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
E, get under a item need testing solution and differentiate need testing solution as this; Other gets the borneol reference substance, adds ethanol and makes the solution that every 1ml contains 10mg, in contrast product solution; Draw each 3ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, cyclohexane-ethyl acetate with 17: 3 ratios is a solvent, launch, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
Embodiment 13:The content assaying method of this cigarette Chinese medicine additive:
Get the about 5mg of archen reference substance, the accurate title, decide, and puts in the 50ml measuring bottle, adds methyl alcohol to scale, shakes up, and promptly gets reference substance solution; Precision is measured this Chinese medicine additive soup 2ml, puts in the 100ml round-bottomed flask, and ethanol is flung in the water-bath heating, adds 2.5mol/1 sulfuric acid solution 20ml, added hot reflux 1 hour, cold slightly, add the about 30ml of chloroform, continue to reflux 2 hours, cooling moves in the separatory funnel, use the minimum of chloroform washing container, washing lotion is incorporated in the separatory funnel, divides and gets in the chloroform stratification 50ml measuring bottle, acid solution is extracted 2 times with chloroform, and about at every turn 8ml, chloroform solution incorporate in the 50ml measuring bottle, add chloroform to scale, shake up, promptly get need testing solution; Precision is measured reference substance solution 2ml and 3ml, flings to methyl alcohol; Precision is measured need testing solution 5ml, evaporate to dryness in addition; Each accurate mixed in equal amounts solution 20ml that adds 2% ammonia solution and 5% sodium hydroxide solution of above-mentioned three parts of residues makes dissolving, filtering, get subsequent filtrate, is blank with reagent, wavelength place at 520nm measures trap respectively, calculates this Chinese medicine additive soup and contains general anthraquinone with archen (C
15H
10O
50) meter, must not be less than 0.1% (1mg/ml).
Embodiment 14:The method of quality control of this cigarette Chinese medicine additive:
1, discrimination method
A, get this Chinese medicine additive soup 10ml, add water 20ml, with extracted by ether 2 times, each 20m1 merges ether extracted liquid, waves most ether for 50 ℃, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution.Other gets Ligusticum wallichii control medicinal material meal 1g, and the 20ml that adds diethyl ether refluxed 20 minutes, filters, and filtrate evaporate to dryness, residue add ethyl acetate 2ml makes dissolving, as shining medicinal material solution.Test according to thin-layered chromatography (appendix VIB), draw each 2ul of above-mentioned solution, put respectively in-be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with n-hexane-acetic acid second intoxicated (9: 1) is solvent, launches, and takes out, dry, put under the ultraviolet lamp (365nm) and inspect, the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the spot of same color.
B, get this Chinese medicine additive soup 10ml, add water 20ml, with ether 20ml washing, the aqueous solution extracts 2 times with water-saturated n-butanol again, each 20ml merges n-butanol liquid, water bath method, and residue dissolves with small amount of ethanol, add neutral alumina 2g, mix thoroughly, evaporate to dryness, be contained in post (200～300 orders, 1g, the internal diameter 10mm of neutral alumina, dry column-packing) on, uses the 40ml methanol-eluted fractions, collect eluent, put evaporate to dryness in the water-bath, residue adds methyl alcohol 2ml makes dissolving, as need testing solution.Other gets the Paeoniflorin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution.Test according to thin-layered chromatography (appendix VIB), draw each 5ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with chloroform-ethyl acetate-methyl alcohol-formic acid (45: 5: 10: 0.2) be solvent, launch, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
C, get this cigarette Chinese medicine additive soup 10ml, put and steam in the water-bath, add 2.5mol/1, sulfuric acid solution 20ml to there not being the alcohol flavor, heating hydrolysis 30 minutes, put cold, with extracted by ether 2 times, each 20m1, merge ether solution, evaporate to dryness, residue add absolute ethyl alcohol 2ml makes dissolving, as need testing solution.Other gets archen and Physcion reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, in contrast product solution.Test according to thin-layered chromatography (appendix VIB), draw need testing solution and medicinal material solution and medicinal material 10ul, each 2ul of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with benzinum (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is solvent, launch, take out, dry, put in the ammonia steam smoked after, inspect under the daylight, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
D, get and differentiate that need testing solution is differentiated need testing solution as this under a item.Other gets the cinnaldehydrum reference substance, adds ethanol and makes the solution that every 1ml contains 1ul, in contrast product solution.Test according to thin-layered chromatography (appendix VIB), draw above-mentioned need testing solution 4ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with benzinum (30～60 ℃)-Ethyl formate-formic acid (15: 5: 1) is solvent, launches, and takes out, dry, spray is with dinitrophenylhydrazine ethanol test solution.In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color.
E, get and differentiate that need testing solution is differentiated need testing solution as this under a item.Other gets the borneol reference substance, adds ethanol and makes the solution that every 1ml contains 10mg, in contrast product solution.Draw each 3ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with cyclohexane-ethyl acetate (17: 3) is solvent, launch, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
2, content assaying method
Get the about 5mg of archen reference substance, the accurate title, decide, and puts in the 50ml measuring bottle, adds methyl alcohol to scale, shakes up, and promptly gets reference substance solution; Precision is measured this Chinese medicine additive soup 2ml, puts in the 100ml round-bottomed flask, and ethanol is flung in the water-bath heating, adds 2.5mol/1 sulfuric acid solution 20ml, added hot reflux 1 hour, cold slightly, add the about 30ml of chloroform, continue to reflux 2 hours, cooling moves in the separatory funnel, use the minimum of chloroform washing container, washing lotion is incorporated in the separatory funnel, divides and gets in the chloroform stratification 50ml measuring bottle, acid solution is extracted 2 times with chloroform, and about at every turn 8ml, chloroform solution incorporate in the 50ml measuring bottle, add chloroform to scale, shake up, promptly get need testing solution; Precision is measured reference substance solution 2ml and 3ml, flings to methyl alcohol; Precision is measured need testing solution 5ml, evaporate to dryness in addition; Each accurate mixed in equal amounts solution 20ml that adds 2% ammonia solution and 5% sodium hydroxide solution of above-mentioned three parts of residues makes dissolving, filtering, get subsequent filtrate, is blank with reagent, wavelength place at 520nm measures trap respectively, calculates this Chinese medicine additive soup and contains general anthraquinone with archen (C
15H
10O
50) meter, must not be less than 0.1% (1mg/ml).
Claims (10)
1, a kind of cigarette Chinese medicine additive is characterized in that this Chinese medicine additive is to be made by the raw material of following weight parts:
Ligusticum wallichii 280-380 weight portion radix paeoniae rubrathe 140-190 weight portion tiger battle 140-190 weight portion
Cassia twig 70-95 weight portion borneol 5-10 weight portion.
2, cigarette Chinese medicine additive as claimed in claim 1 is characterized in that this Chinese medicine additive is to be made by the raw material of following weight parts:
The Ligusticum wallichii 330 weight portion radix paeoniae rubrathe 165 weight portions tiger battle 165 weight portions
Cassia twig 82 weight portion borneols 8 weight portions.
3, the preparation method of cigarette Chinese medicine additive as claimed in claim 1 or 2 is characterized in that this method is:
With Ligusticum wallichii, the radix paeoniae rubrathe, tiger battle, cassia twig is cataclasm, wash quickly is placed in the ethanol of 60-80% only, soaks 18-36 hour in 40～45 ℃ of temperature; With the immersion liquid of 3-5 layer filtered through gauze, obtain filtrate V1, dregs of a decoction squeezing, pressed liquor obtains filtrate V2 with 3-5 layer filtered through gauze, merges V1 and V2 airtight preservation in container; The dregs of a decoction are with the alcohol reflux of the 60-80% of 2-4 times of weight 2-4 time, and each 0.5-1.5 hour, all use 3-5 layer filtered through gauze after each the backflow, merge and filter gained filtrate; Backflow gained filtrate obtains concentrate V3 in decompression recycling ethanol below 60 ℃; The take a morsel amalgamation liquid of V1 and V2 adds borneol, and stirring and dissolving is made borneol liquid; Concentrate V3 is under agitation merged with V1, V2, borneol liquid is under agitation added amalgamation liquid very slowly, filter, sterilize, promptly.
4, the preparation method of cigarette Chinese medicine additive as claimed in claim 3 is characterized in that this method is:
With Ligusticum wallichii, the radix paeoniae rubrathe, tiger battle, cassia twig is cataclasm, wash quickly is placed in 70% the ethanol only, soaks 24 hours in 40～45 ℃ of temperature; With 4 layers of filtered through gauze immersion liquid, obtain filtrate V1, dregs of a decoction squeezing, pressed liquor obtains filtrate V2 with 4 layers of filtered through gauze, merges V1 and V2 airtight preservation in container; The dregs of a decoction are with 70% alcohol reflux of 3 times of weight 3 times, and each 1 hour, all use 4 layers of filtered through gauze after each the backflow, merge and filter gained filtrate; Backflow gained filtrate obtains concentrate V3 in decompression recycling ethanol below 60 ℃; The take a morsel amalgamation liquid of V1 and V2 adds borneol, and stirring and dissolving is made borneol liquid; Concentrate V3 is under agitation merged with V1, V2, borneol liquid is under agitation added amalgamation liquid very slowly, filter, sterilize, promptly.
5, the method for quality control of cigarette Chinese medicine additive as claimed in claim 1 or 2 is characterized in that comprising in this method in the following discrimination method one or more:
A, get this Chinese medicine additive soup 10ml, add water 20ml, with extracted by ether 2 times, each 20ml merges ether extracted liquid, waves most ether for 50 ℃, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution; Other gets Ligusticum wallichii control medicinal material meal 1g, the 20ml that adds diethyl ether, and backflow 15-30 minute, filter, filtrate evaporate to dryness, residue add ethyl acetate 2ml makes dissolving, as shining medicinal material solution; Test according to thin-layered chromatography, draw each 2ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 8-9: the n-hexane of 1-2 ratio-acetic acid second is intoxicated to be solvent, launches, and takes out, dry, put under the ultraviolet lamp and inspect, the test sample chromatogram with the corresponding position of control medicinal material chromatogram on, show the spot of same color;
B, get this Chinese medicine additive soup 10ml, add water 20ml, with ether 20ml washing, the aqueous solution extracts 2 times with water-saturated n-butanol again, and each 20ml merges n-butanol liquid, water bath method, residue dissolves with small amount of ethanol, adds neutral alumina 2g, mix thoroughly, evaporate to dryness is contained on the post of neutral alumina, use the 40ml methanol-eluted fractions, collect eluent, put evaporate to dryness in the water-bath, residue adds methyl alcohol 2ml makes dissolving, as need testing solution; Other gets the Paeoniflorin reference substance, adds methyl alcohol and makes the solution that every 1ml contains 2mg, in contrast product solution; Test according to thin-layered chromatography, draw each 5ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 42-48: 4-6: 8-12: the chloroform-ethyl acetate of 0.1-0.3 ratio-methyl alcohol-formic acid is solvent, launches, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, and it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
C, get this Chinese medicine additive soup 10ml, put and steam in the water-bath, add 2.5mol/l, sulfuric acid solution 20ml to there not being the alcohol flavor, heating hydrolysis 20-40 minute, put cold, with extracted by ether 2 times, each 20ml, merge ether solution, evaporate to dryness, residue add absolute ethyl alcohol 2ml makes dissolving, as need testing solution; Other gets archen and Physcion reference substance, adds methyl alcohol respectively and makes the solution that every 1ml contains 1mg, in contrast product solution; Test according to thin-layered chromatography, draw need testing solution and medicinal material solution and medicinal material 10ul, each 2ul of reference substance solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 12-18: 3-6: the benzinum-Ethyl formate of 1-2 ratio-formic acid is solvent, launch, take out, dry, put in the ammonia steam smoked after, inspect under the daylight, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color;
D, get and differentiate that need testing solution is differentiated need testing solution as this under a item; Other gets the cinnaldehydrum reference substance, adds ethanol and makes the solution that every 1ml contains 1ul, in contrast product solution; Test according to thin-layered chromatography, draw above-mentioned need testing solution 4ul, reference substance solution 2ul, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 12-18: 3-6: the benzinum-Ethyl formate of 1-2 ratio-formic acid is solvent, launches, and takes out, dry, spray is with dinitrophenylhydrazine ethanol test solution; In the test sample chromatogram chromatogram, with the corresponding position of reference substance chromatogram on, show the spot of same color;
E, get and differentiate that need testing solution is differentiated need testing solution as this under a item; Other gets the borneol reference substance, adds ethanol and makes the solution that every 1ml contains 10mg, in contrast product solution; Draw each 3ul of above-mentioned solution, put respectively in same be on the silica gel g thin-layer plate of binder with 0.3% sodium carboxymethylcellulose, with 15-18: the cyclohexane-ethyl acetate of 2-5 ratio is a solvent, launch, take out, dry, spray is with 5% vanillic aldehyde ethanol solution of sulfuric acid, it is clear to be heated to spot colour developing at 105 ℃, the test sample chromatogram with the corresponding position of reference substance chromatogram on, show the spot of same color.
6, the method for quality control of cigarette Chinese medicine additive as claimed in claim 5 is characterized in that comprising in this method following content assaying method:
Get the about 5mg of archen reference substance, the accurate title, decide, and puts in the 50ml measuring bottle, adds methyl alcohol to scale, shakes up, and promptly gets reference substance solution; Precision is measured this Chinese medicine additive soup 2ml, put in the 100ml round-bottomed flask, ethanol is flung in the water-bath heating, adds 2.5mol/l sulfuric acid solution 20ml, adds hot reflux 0.5-2 hour, cold slightly, add the about 30ml of chloroform, continue backflow 1-3 hour, cooling, move in the separatory funnel, use the minimum of chloroform washing container, washing lotion is incorporated in the separatory funnel, divides and gets in the chloroform stratification 50ml measuring bottle, acid solution is extracted 2 times with chloroform, each about 8ml, chloroform solution is incorporated in the 50ml measuring bottle, adds chloroform to scale, shake up, promptly get need testing solution; Precision is measured reference substance solution 2ml and 3ml, flings to methyl alcohol; Precision is measured need testing solution 5ml, evaporate to dryness in addition; Each accurate mixed in equal amounts solution 20ml that adds 2% ammonia solution and 5% sodium hydroxide solution of above-mentioned three parts of residues makes dissolving, filter, get subsequent filtrate, with reagent is blank, wavelength place at 520nm measures trap respectively, calculate this Chinese medicine additive soup and contain general anthraquinone, must not be less than 0.1% in archen.
7, cigarette Chinese medicine additive as claimed in claim 1 or 2 has function of promoting blood circulation to disperse blood clots in preparation, the application in treatment coronary heart disease, the anginal cigarette.
8, application as claimed in claim 7 is characterized in that the described hemorheology index that improves is meant the prolongation clotting time, reduces erythrocyte aggregation index or reduces the high, medium and low viscosity of cutting of whole blood; Described inhibition thrombosis is meant dry weight, the weight in wet base that reduces arteriovenous thrombus loop thrombus; The described myocardial ischemia that improves is meant the generation that reduces lipid peroxide, improves Electrocardiographic effect.
9, cigarette Chinese medicine additive as claimed in claim 1 or 2, this Chinese medicine additive is made cigarette, it is characterized in that the ratio of Chinese medicine additive soup and pipe tobacco is 0.1～1% in the cigarette.
10, cigarette Chinese medicine additive as claimed in claim 8, this Chinese medicine additive is made cigarette, it is characterized in that the ratio of Chinese medicine additive soup and pipe tobacco is 0.25% in the cigarette.
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| CNB2005100934411A CN100482112C (en) | 2005-08-23 | 2005-08-30 | Traditional Chinese medicine additive for cigarette, its prepn. method and quality control method |
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| CNB2005100934411A CN100482112C (en) | 2005-08-23 | 2005-08-30 | Traditional Chinese medicine additive for cigarette, its prepn. method and quality control method |
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| CN100482112C CN100482112C (en) | 2009-04-29 |
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| CN111356469A (en) * | 2017-10-27 | 2020-06-30 | 韩国韩医药振兴院 | Antithrombotic composition comprising rhizoma Polygoni Cuspidati and cortex Cinnamomi |
| JP2021501207A (en) * | 2017-10-27 | 2021-01-14 | 韓國韓醫藥振興院Ｎａｔｉｏｎａｌ Ｉｎｓｔｉｔｕｔｅ ｆｏｒ Ｋｏｒｅａｎ Ｍｅｄｉｃｉｎｅ Ｄｅｖｅｌｏｐｍｅｎｔ | Antithrombotic composition containing Japanese knotweed and cinnamon |
| CN111356469B (en) * | 2017-10-27 | 2022-05-27 | 韩国韩医药振兴院 | Composition comprising rhizoma Polygoni Cuspidati root and cortex Cinnamomi for resisting thrombi |
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| CN109932469A (en) * | 2019-04-12 | 2019-06-25 | 安徽中医药大学第一附属医院 | The discrimination method of borneol in a kind of hemorrhoid complicated by anal fistula lotion |
| CN109932470A (en) * | 2019-04-12 | 2019-06-25 | 安徽中医药大学第一附属医院 | The alkalization method of silica G plate in a kind of traditional Chinese medicine of licorice root preparation indentification by TLC |
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