CN102266364A - Traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and preparation method thereof - Google Patents
Traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and preparation method thereof Download PDFInfo
- Publication number
- CN102266364A CN102266364A CN 201110235878 CN201110235878A CN102266364A CN 102266364 A CN102266364 A CN 102266364A CN 201110235878 CN201110235878 CN 201110235878 CN 201110235878 A CN201110235878 A CN 201110235878A CN 102266364 A CN102266364 A CN 102266364A
- Authority
- CN
- China
- Prior art keywords
- preparation
- extract
- extracting solution
- cardiovascular
- chinese medicine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000003814 drug Substances 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 208000026106 cerebrovascular disease Diseases 0.000 title claims abstract description 22
- 208000024172 Cardiovascular disease Diseases 0.000 title claims abstract description 20
- 230000002526 effect on cardiovascular system Effects 0.000 title claims abstract description 20
- 239000013078 crystal Substances 0.000 claims abstract description 30
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007788 liquid Substances 0.000 claims abstract description 22
- 229940079593 drug Drugs 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 5
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000004615 ingredient Substances 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 23
- 238000000605 extraction Methods 0.000 claims description 14
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000284 extract Substances 0.000 abstract description 33
- -1 inhalation Substances 0.000 abstract description 4
- 239000007924 injection Substances 0.000 abstract description 4
- 238000002347 injection Methods 0.000 abstract description 4
- 208000029078 coronary artery disease Diseases 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000008187 granular material Substances 0.000 abstract description 2
- 239000007921 spray Substances 0.000 abstract description 2
- 239000003826 tablet Substances 0.000 abstract description 2
- 244000061520 Angelica archangelica Species 0.000 abstract 2
- 235000001287 Guettarda speciosa Nutrition 0.000 abstract 2
- 241000112528 Ligusticum striatum Species 0.000 abstract 2
- 239000008188 pellet Substances 0.000 abstract 1
- 239000007901 soft capsule Substances 0.000 abstract 1
- 208000023516 stroke disease Diseases 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 24
- IQVQXVFMNOFTMU-FLIBITNWSA-N (Z)-ligustilide Chemical compound C1CC=CC2=C1C(=C/CCC)/OC2=O IQVQXVFMNOFTMU-FLIBITNWSA-N 0.000 description 23
- IQVQXVFMNOFTMU-DHZHZOJOSA-N Z-ligustilide Natural products C1CC=CC2=C1C(=C/CCC)\OC2=O IQVQXVFMNOFTMU-DHZHZOJOSA-N 0.000 description 23
- KSEBMYQBYZTDHS-HWKANZROSA-M (E)-Ferulic acid Natural products COC1=CC(\C=C\C([O-])=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-M 0.000 description 16
- KSEBMYQBYZTDHS-HWKANZROSA-N ferulic acid Chemical compound COC1=CC(\C=C\C(O)=O)=CC=C1O KSEBMYQBYZTDHS-HWKANZROSA-N 0.000 description 16
- 229940114124 ferulic acid Drugs 0.000 description 16
- KSEBMYQBYZTDHS-UHFFFAOYSA-N ferulic acid Natural products COC1=CC(C=CC(O)=O)=CC=C1O KSEBMYQBYZTDHS-UHFFFAOYSA-N 0.000 description 16
- 235000001785 ferulic acid Nutrition 0.000 description 16
- QURCVMIEKCOAJU-UHFFFAOYSA-N trans-isoferulic acid Natural products COC1=CC=C(C=CC(O)=O)C=C1O QURCVMIEKCOAJU-UHFFFAOYSA-N 0.000 description 16
- 241000700159 Rattus Species 0.000 description 11
- 229930006000 Sucrose Natural products 0.000 description 10
- 239000005720 sucrose Substances 0.000 description 10
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 9
- 210000004369 blood Anatomy 0.000 description 7
- 239000008280 blood Substances 0.000 description 7
- 238000004821 distillation Methods 0.000 description 6
- 239000012634 fragment Substances 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 239000000341 volatile oil Substances 0.000 description 6
- 102000019197 Superoxide Dismutase Human genes 0.000 description 5
- 108010012715 Superoxide dismutase Proteins 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000001256 steam distillation Methods 0.000 description 5
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 4
- 206010061216 Infarction Diseases 0.000 description 4
- 208000002193 Pain Diseases 0.000 description 4
- 206010008118 cerebral infarction Diseases 0.000 description 4
- 230000007574 infarction Effects 0.000 description 4
- 239000012567 medical material Substances 0.000 description 4
- 201000006474 Brain Ischemia Diseases 0.000 description 3
- 208000007536 Thrombosis Diseases 0.000 description 3
- 230000014759 maintenance of location Effects 0.000 description 3
- 208000010125 myocardial infarction Diseases 0.000 description 3
- 210000002966 serum Anatomy 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 208000006820 Arthralgia Diseases 0.000 description 2
- HJXMNVQARNZTEE-UHFFFAOYSA-N Butylphthalide Chemical compound C1=CC=C2C(CCCC)OC(=O)C2=C1 HJXMNVQARNZTEE-UHFFFAOYSA-N 0.000 description 2
- 206010008089 Cerebral artery occlusion Diseases 0.000 description 2
- 206010008120 Cerebral ischaemia Diseases 0.000 description 2
- 206010008190 Cerebrovascular accident Diseases 0.000 description 2
- WSMYVTOQOOLQHP-UHFFFAOYSA-N Malondialdehyde Chemical compound O=CCC=O WSMYVTOQOOLQHP-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- 208000006011 Stroke Diseases 0.000 description 2
- 229960000583 acetic acid Drugs 0.000 description 2
- 239000004480 active ingredient Substances 0.000 description 2
- 239000003146 anticoagulant agent Substances 0.000 description 2
- 230000017531 blood circulation Effects 0.000 description 2
- 150000001720 carbohydrates Chemical class 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000012362 glacial acetic acid Substances 0.000 description 2
- 235000001727 glucose Nutrition 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000004128 high performance liquid chromatography Methods 0.000 description 2
- 239000007791 liquid phase Substances 0.000 description 2
- 238000001819 mass spectrum Methods 0.000 description 2
- 201000007309 middle cerebral artery infarction Diseases 0.000 description 2
- 230000003188 neurobehavioral effect Effects 0.000 description 2
- JPXMTWWFLBLUCD-UHFFFAOYSA-N nitro blue tetrazolium(2+) Chemical compound COC1=CC(C=2C=C(OC)C(=CC=2)[N+]=2N(N=C(N=2)C=2C=CC=CC=2)C=2C=CC(=CC=2)[N+]([O-])=O)=CC=C1[N+]1=NC(C=2C=CC=CC=2)=NN1C1=CC=C([N+]([O-])=O)C=C1 JPXMTWWFLBLUCD-UHFFFAOYSA-N 0.000 description 2
- 230000000144 pharmacologic effect Effects 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- QEVHRUUCFGRFIF-MDEJGZGSSA-N reserpine Chemical compound O([C@H]1[C@@H]([C@H]([C@H]2C[C@@H]3C4=C(C5=CC=C(OC)C=C5N4)CCN3C[C@H]2C1)C(=O)OC)OC)C(=O)C1=CC(OC)=C(OC)C(OC)=C1 QEVHRUUCFGRFIF-MDEJGZGSSA-N 0.000 description 2
- 238000004809 thin layer chromatography Methods 0.000 description 2
- UIAGMCDKSXEBJQ-IBGZPJMESA-N 3-o-(2-methoxyethyl) 5-o-propan-2-yl (4s)-2,6-dimethyl-4-(3-nitrophenyl)-1,4-dihydropyridine-3,5-dicarboxylate Chemical compound COCCOC(=O)C1=C(C)NC(C)=C(C(=O)OC(C)C)[C@H]1C1=CC=CC([N+]([O-])=O)=C1 UIAGMCDKSXEBJQ-IBGZPJMESA-N 0.000 description 1
- 201000001320 Atherosclerosis Diseases 0.000 description 1
- 206010008111 Cerebral haemorrhage Diseases 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 206010019233 Headaches Diseases 0.000 description 1
- 206010063837 Reperfusion injury Diseases 0.000 description 1
- 208000025747 Rheumatic disease Diseases 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 230000002785 anti-thrombosis Effects 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 206010003119 arrhythmia Diseases 0.000 description 1
- 230000006793 arrhythmia Effects 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 210000000481 breast Anatomy 0.000 description 1
- 229950005197 butylphthalide Drugs 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001647 drug administration Methods 0.000 description 1
- 230000000857 drug effect Effects 0.000 description 1
- 238000009297 electrocoagulation Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 150000002304 glucoses Chemical class 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 231100000869 headache Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002607 hemopoietic effect Effects 0.000 description 1
- 238000000589 high-performance liquid chromatography-mass spectrometry Methods 0.000 description 1
- 238000000338 in vitro Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 208000037906 ischaemic injury Diseases 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 208000031225 myocardial ischemia Diseases 0.000 description 1
- 210000004165 myocardium Anatomy 0.000 description 1
- 229960000715 nimodipine Drugs 0.000 description 1
- 231100000862 numbness Toxicity 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000013641 positive control Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 230000003716 rejuvenation Effects 0.000 description 1
- 230000010410 reperfusion Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000000552 rheumatic effect Effects 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 125000000185 sucrose group Chemical group 0.000 description 1
- 239000000829 suppository Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 230000008542 thermal sensitivity Effects 0.000 description 1
Images
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and a preparation method thereof. The preparation method comprises the following steps: weighing 1g of angelica or Ligusticum wallichii or a mixture of angelica and Ligusticum wallichii in any proportion, crushing, extracting with 1-100 ml of 50-100wt% ethanol solvent 1-3 times and 0.5-4.0 hours each time, and filtering to obtain an extract; concentrating the extract to 0.1-5.0 g crude drug per milliliter of drug liquid, and standing at the temperature of 0-30 DEG C for 1-100 days to precipitate colorless to light yellow crystal; and removing the crystals and concentrating the drug liquid into an extract so as to obtain the required traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases. The traditional Chinese medicine effective part prepared by the preparation method disclosed by the invention can be made into tablets, soft capsules, granules, pellets, oral liquid, injection, inhalation, sprays, patches, drops and the like, and can be used in preparation of drugs for treating stroke and coronary heart disease.
Description
Technical field
The present invention relates to a kind of effective ingredient in Chinese preparation field, specifically is a kind of treatment cardiovascular and cerebrovascular disease effective ingredient in Chinese and preparation method thereof.
Background technology
Apoplexy and coronary heart disease are the regular incidences of world population and are tending towards rejuvenation, have a strong impact on patient's Health and Living quality, also are one of first causes that causes the human mortality.Radix Angelicae Sinensis and Rhizoma Chuanxiong be clinical commonly used enrich blood invigorate blood circulation, the blood stasis removing pain relieving to medicine, also be the common important Chinese medicine of treatment cardiovascular and cerebrovascular disease.
Radix Angelicae Sinensis have enrich blood invigorate blood circulation, the analgesic effect, be used for all cards of blood deficiency and cards such as blood stasis is had a pain, arthralgia pain numbness; From the modern medicine angle, has arrhythmia, atherosclerosis, anticoagulant, effects such as antithrombotic and enhancing hemopoietic function; Rhizoma Chuanxiong has the effect of blood-activating and qi-promoting, wind-expelling pain-stopping, is used for the twinge of the breast side of body, headache, rheumatic arthralgia.Current have Radix Angelicae Sinensis injection, Rhizoma Chuanxiong injection, FUFANG DANGGUI ZHUSHEYE etc. to make in clinical.Radix Angelicae Sinensis, the effective ingredient of Rhizoma Chuanxiong treatment cardiovascular and cerebrovascular disease is mainly ferulic acid, comprises volatile ingredient ligustilide, butylphthalide etc. in addition.
Containing the conventional extracting method of Radix Angelicae Sinensis, Rhizoma Chuanxiong medicine is to adopt vapor distillation to obtain volatile oil, remerges water decoction, makes preparation.Yet this method has following shortcoming:
(1), carry the volatile oil yield very low, volatile ingredient extracts not exclusively, influences drug effect; And, be difficult to mention volatile oil completely because the equipment of suitability for industrialized production is limit, be Aromatic water under a lot of situations;
(2), vapor distillation extracts the volatile oil time and grow (common more than 4 hours), thermal sensitivity composition (as effective composition ligustilide) easily decomposes, the long-time decoction, the medicinal residues thickness is difficult to be filtered, and causes loss of active ingredients;
(3), filter water decoction in contain impurity such as a large amount of useless polysaccharide and micromolecule saccharide, cause the increase of drug administration dosage.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of effective ingredient in Chinese for the treatment of cardiovascular and cerebrovascular disease and preparation method thereof is provided, the present invention combines Chinese medicine and the modern purification techniques that extracts, and fully extracts the middle pharmaceutically active ingredient of treatment cardiovascular and cerebrovascular disease: ferulic acid and volatile ingredient ligustilide.
Realize the technical scheme that the object of the invention adopted:
A kind of preparation method for the treatment of the effective ingredient in Chinese of cardiovascular and cerebrovascular disease, comprise the steps: weighting raw materials: Radix Angelicae Sinensis or Rhizoma Chuanxiong or both press any one in the blended mixture of arbitrary proportion, pulverizing the back, to add mass percent be to extract 1～3 time in 50～100% the ethanol, wherein extracting the required ethanol of every 1g crude drug is 1～100ml, each extraction time is 0.5～4.0 hour, filter, obtain extracting solution, this extracting solution is concentrated into 0.1～5.0g crude drug/ml medicinal liquid, and left standstill 1～100 day at 0～30 ℃, separate out colourless to pale yellow crystals, behind the reject crystal, medicinal liquid is condensed into extractum, can obtains the effective ingredient in Chinese of required treatment cardiovascular and cerebrovascular disease.
Described alcohol solvent consumption is 5～10ml, and mass percent is 90～100%, and described each extraction time is 2 hours, and described extracting solution is concentrated into 1.0～1.5g crude drug/ml medicinal liquid, and described dwell temperature is 0～8 ℃, and time of repose is 3～8 days.
Compared with prior art, the advantage and the beneficial effect that have of the present invention is as follows:
(1) extracts as solvent with ethanol, though do not relate to the volatile oil leaching process of vapor distillation, but can obtain promptly to contain ferulic acid simultaneously, the effective site that contains the volatile ingredient ligustilide again, avoided in the conventional extracting method volatile oil yield low, extracted not exclusively and shortcoming such as industrial applications difficulty.
(2) extracting solution leaves standstill at 0～30 ℃ and can separate out pale yellow crystals in 1～100 day, this crystal is an impurity sucrose, the Chinese herbal and crude drugs preparations that gets final product requiredly behind the reject, this method is utilized the sucrose melted by heating, this character is separated out in cooling, and is simple to operation, avoided also will adopting macroporous adsorbent resin technology to remove the last handling process of saccharide impurity after the conventional extracting method extraction, avoided the further loss of effective ingredient, this also is the original innovation part of the present invention.
(3) the extraction efficiency height of effective ingredient ferulic acid and ligustilide among the present invention reaches 2 times and 6 times of conventional steam distillation respectively, thereby can reduce dosage, and is easy to use.
(4) effective site of the inventive method acquisition can further be made tablet, capsule, granule, micropill, oral liquid, injection, inhalant, spray, patch, suppository and drop etc., uses in medicine for preparing prevention and treatment apoplexy, coronary heart disease and health product.
Description of drawings
Fig. 1 is the improve design sketch of the effective site of the inventive method preparation to the focal cerebral hemorrhage focus of infarct of rat;
Fig. 2 is that extract of the present invention is separated out crystalline thin-layer chromatogram; Wherein 1 represents sucrose, 2 expression glucoses, the crystal that Radix Angelicae Sinensis extracting solution is separated out in 3 expression the inventive method, the crystal that the Rhizoma Chuanxiong extracting solution is separated out in 4 expression the inventive method, the crystal that Radix Angelicae Sinensis and Rhizoma Chuanxiong extracting solution are separated out in 5 expression the inventive method;
Fig. 3 is that extracting solution is separated out crystalline infrared spectrum in the inventive method;
Fig. 4 is that the present invention extracts the ferulic acid sign high-efficient liquid phase chromatogram that obtains; Wherein A figure is the ferulic acid standard substance, and B figure is the Radix Angelicae Sinensis effective site that the embodiment of the invention 1 makes, and C figure is the Rhizoma Chuanxiong effective site that the embodiment of the invention 2 makes;
Fig. 5 is that the present invention extracts the ligustilide sign high-efficient liquid phase chromatogram that obtains; Wherein A figure is the ligustilide reference substance, and B figure is the effective site that contains Radix Angelicae Sinensis and Rhizoma Chuanxiong that the embodiment of the invention 3 makes;
Fig. 6 is that the present invention extracts the ligustilide mass spectrum that obtains.
The specific embodiment
Below in conjunction with specific embodiment the present invention is described in further detail, but embodiments of the present invention are not limited thereto, the technological parameter for not indicating especially can carry out with reference to routine techniques.
Get Radix Angelicae Sinensis 400g, being ground into the fragment about 1cm, is that 90% ethanol 2000ml extracts 3 times with mass percent, and each extraction time is 2 hours, extracting the back filters, obtain extracting solution, this extracting solution is concentrated into 1.0g crude drug/ml medicinal liquid, left standstill 8 days at 0 ℃, separate out colourless to pale yellow crystals, the reject crystal, medicinal liquid is condensed into extractum, and the cardiovascular and cerebrovascular disease that obtains medical treatment mainly contains the effective ingredient in Chinese of ferulic acid and ligustilide.
Get Rhizoma Chuanxiong 400g, being ground into the fragment about 1cm, is that 92% ethanol 2000ml extracts 2 times with mass percent, and each extraction time is 2 hours, extracting the back filters, obtain extracting solution, this extracting solution is concentrated into 1.3g crude drug/ml medicinal liquid, left standstill 8 days at 1 ℃, separate out colourless to pale yellow crystals, the reject crystal, medicinal liquid is condensed into extractum, and the cardiovascular and cerebrovascular disease that obtains medical treatment mainly contains the effective ingredient in Chinese of ferulic acid and ligustilide.
Get Radix Angelicae Sinensis 200g, Rhizoma Chuanxiong 200g, the medical material gross weight is 400g, and be ground into fragment about 1cm, and be that 99% ethanol 2000ml extracts 1 time with mass percent, extraction time is 2 hours, extracting the back filters, obtain extracting solution, this extracting solution is concentrated into 1.4g crude drug/ml medicinal liquid, left standstill 5 days at 5 ℃, separate out colourless to pale yellow crystals, the reject crystal, medicinal liquid is condensed into extractum, and the cardiovascular and cerebrovascular disease that obtains medical treatment mainly contains the effective ingredient in Chinese of ferulic acid and ligustilide.
Get Radix Angelicae Sinensis 100g, Rhizoma Chuanxiong 300g, the medical material gross weight is 400g, and be ground into fragment about 1cm, and be that 95% ethanol 2000ml extracts 3 times with mass percent, each extraction time is 2 hours, extracting the back filters, obtain extracting solution, this extracting solution is concentrated into 1.3g crude drug/ml medicinal liquid, left standstill 4 days at 7 ℃, separate out colourless to pale yellow crystals, the reject crystal, medicinal liquid is condensed into extractum, and the cardiovascular and cerebrovascular disease that obtains medical treatment mainly contains the effective ingredient in Chinese of ferulic acid and ligustilide.
Get Radix Angelicae Sinensis 100g, Rhizoma Chuanxiong 300g, the medical material gross weight is 400g, and be ground into fragment about 1cm, and be that 50% ethanol 2000ml extracts 1 time with mass percent, extraction time is 4 hours, extracting the back filters, obtain extracting solution, this extracting solution is concentrated into 0.1g crude drug/ml medicinal liquid, left standstill 1 day at 25 ℃, separate out colourless to pale yellow crystals, the reject crystal, medicinal liquid is condensed into extractum, and the cardiovascular and cerebrovascular disease that obtains medical treatment mainly contains the effective ingredient in Chinese of ferulic acid and ligustilide.
Embodiment 6
Get Radix Angelicae Sinensis 100g, Rhizoma Chuanxiong 300g, the medical material gross weight is 400g, and be ground into fragment about 1cm, with mass percent is that 100% ethanol 2000ml extracts 1 time, and each extraction time is 0.5 hour, extracts after-filtration and falls medicinal residues and obtain extracting solution, this extracting solution is concentrated into 5.0g crude drug/ml medicinal liquid, left standstill 100 days at 30 ℃, separate out pale yellow crystals after, the reject crystal, medicinal liquid is condensed into extractum, and the cardiovascular and cerebrovascular disease that obtains medical treatment mainly contains the effective ingredient in Chinese of ferulic acid and ligustilide.
The effective ingredient in Chinese of the inventive method preparation is carried out following pharmacological evaluation:
1, the influence that focal cerebral ischemia in rats is damaged
Adopt bolt collimation method blocking-up intraluminal middle cerebral artery occlusion in rats, the focal brain ischemia-reperfusion injury model that causes.Irritate respectively and feed effective site (EE) and the nimodipine positive control drug (NP) that adopts the inventive method preparation with dosage, the result is as follows: compare with model group (M), the effective site group rat focus of infarct that this law obtains obviously dwindles, as shown in Figure 1.Give the effective site of this law preparation, the neurobehavioral obstacle of animal obviously alleviates behind the cerebral infarction, and activity of SOD in serum obviously increases, and MDA content obviously descends.The matched group (NP) that is better than use with every index of dosage.
Adopt electrocoagulation blocking-up intraluminal middle cerebral artery occlusion in rats, the focal cerebral ischemia in rats model that causes.Irritate respectively to feed and adopt the effective site of this law preparation and the extract of steam distillation preparation with dosage, result and model group are relatively, this effective site group rat focus of infarct obviously dwindles, the neurobehavioral obstacle of animal obviously alleviates behind the cerebral infarction, activity of SOD in serum obviously increases, and MDA content obviously descends.The matched group that is better than the extract that uses the preparation of vapor distillation method with every index of dosage.
2, to the influence of rat heart muscle ischemic injuries
Myocardial infarction model due to the employing rat myocardial ischemia and reperfusion, nitro blue tetrazolium (N-BT) is a stain.Observation is adopted the influence of the extract of the effective site of this law preparation and steam distillation preparation to myocardial infarction degree and superoxide dismutase (SOD) and malonaldehyde (MDA) with dosage, this effective site group (EE) myocardial infarction degree has obviously and alleviates as a result, infarct size reduces, infarcted region weight saving, infarcted region accounts for ventricle and heart percentage ratio reduces, and with model group significant difference (P＜0.05～P＜0.01) is arranged relatively.The activity of SOD in serum that can raise relatively has significant difference (P＜0.05) with model group; Be better than the extract that adopts the preparation of vapor distillation method with each index of dosage.
3, to the influence of rats in vitro thrombosis and blood viscosity.
Irritated hello administration in continuous 7 days for rat and adopt the effective site of this law preparation and the extract of steam distillation preparation with dosage, the result is as follows: this effective site obviously shortens thrombosis length (P＜0.01), alleviates wet weight of thrombus and dry weight (P＜0.01 ~ 0.001); Obviously reduce shear rate 150S
-1, 60S
-1, 5S
-1Under whole blood viscosity (P＜0.05 ~ 0.001); Be better than the extract that adopts the preparation of vapor distillation method with each index of dosage.
Be effective ingredient in the effective site of determining this law preparation, carried out following sign experiment
:
1, separating out crystal is sucrose, and its sign is as follows:
1) separates out crystal and carry out thin layer chromatography (TLC) inspection knowledge, compare with glucose, sucrose, as Fig. 2.
The crystal Rf value of separating out in this method Radix Angelicae Sinensis extracting solution, Rhizoma Chuanxiong extracting solution, Radix Angelicae Sinensis and the Rhizoma Chuanxiong extracting solution is identical with sucrose, and the crystal that visible cold preservation is separated out is sucrose (impurity).
2) carry out infrared test to separating out crystal, as shown in Figure 3:
It is consistent with the infrared standard diagram of sucrose that three kinds of extracts are separated out the crystal infared spectrum, and can further determine to adopt the crystal that cold preservation is separated out in the extracting solution of this paper method is sucrose (impurity).
2, the HPLC chromatograph of ferulic acid characterizes
Chromatographic condition: chromatographic column Hypersil ODS C
18(4.6 * 150mm, 5 μ m); Methanol-1% glacial acetic acid 32:68 is a mobile phase; The detection wavelength is 320nm; Column temperature: room temperature.Radix Angelicae Sinensis, Rhizoma Chuanxiong extract all have corresponding that chromatographic peak occurs at ferulic acid retention time place, see Fig. 4.As seen adopt this law to extract in the Radix Angelicae Sinensis of acquisition, the Rhizoma Chuanxiong extract and contain the effective ingredient ferulic acid.
3, the sign of ligustilide
1) the HPLC chromatograph of ligustilide characterizes
Chromatographic condition: chromatographic column Hypersil ODS C
18(4.6 * 150mm, 5 μ m); Methanol-1% glacial acetic acid 58:42 is a mobile phase; The detection wavelength is 280nm; Column temperature: room temperature.As shown in Figure 5.
Radix Angelicae Sinensis, Rhizoma Chuanxiong extract have corresponding chromatographic peak to occur at ligustilide retention time place, contain the ligustilide effective ingredient in visible Radix Angelicae Sinensis, the Rhizoma Chuanxiong extract.
2) the HPLC-MS coupling of ligustilide characterizes
Material under the ligustilide retention time in this law extract is carried out mass spectrometric measurement, and the mass spectrum of extraction is seen Fig. 6, and is consistent with the molecular weight of ligustilide.This shows, contain the ligustilide effective ingredient in Radix Angelicae Sinensis, the Rhizoma Chuanxiong extract.
In summary, this extraction process can leave standstill separates out sucrose impurity, is easy to separate, and the effective site that makes mainly contains ferulic acid and ligustilide effective ingredient.Pharmacological effect is better than with the conventional steam distillation extract of dosage amounts.
The foregoing description is a preferred implementation of the present invention; but embodiments of the present invention are not restricted to the described embodiments; other is any not to deviate from change, the modification made under spirit of the present invention and the principle, substitute, combination, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (3)
1. preparation method for the treatment of the effective ingredient in Chinese of cardiovascular and cerebrovascular disease, it is characterized in that, comprise the steps: weighting raw materials: Radix Angelicae Sinensis or Rhizoma Chuanxiong or both press any one in the blended mixture of arbitrary proportion, pulverizing the back, to add mass percent be to extract 1～3 time in 50～100% the ethanol, wherein extracting the required ethanol of every 1g crude drug is 1～100ml, each extraction time is 0.5～4.0 hour, filter, obtain extracting solution, this extracting solution is concentrated into 0.1～5.0g crude drug/ml medicinal liquid, and left standstill 1～100 day at 0～30 ℃, separate out colourless to pale yellow crystals, behind the reject crystal, medicinal liquid is condensed into extractum, can obtains the effective ingredient in Chinese of required treatment cardiovascular and cerebrovascular disease.
2. preparation method according to claim 1, it is characterized in that, described alcohol solvent consumption is 5～10ml, mass percent is 90～100%, described each extraction time is 2 hours, described extracting solution is concentrated into 1.0～1.5g crude drug/ml medicinal liquid, and described dwell temperature is 0～8 ℃, and time of repose is 3～8 days.
3. an effective ingredient in Chinese for the treatment of cardiovascular and cerebrovascular disease is characterized in that, is prepared from by any method of claim 1 to 2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110235878 CN102266364B (en) | 2011-08-17 | 2011-08-17 | Traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110235878 CN102266364B (en) | 2011-08-17 | 2011-08-17 | Traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102266364A true CN102266364A (en) | 2011-12-07 |
| CN102266364B CN102266364B (en) | 2013-03-20 |
Family
ID=45048948
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110235878 Active CN102266364B (en) | 2011-08-17 | 2011-08-17 | Traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102266364B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113797246A (en) * | 2021-10-27 | 2021-12-17 | 首都医科大学附属北京中医医院 | Traditional Chinese medicine composition and preparation method and application thereof |
| CN114469934A (en) * | 2022-02-11 | 2022-05-13 | 天津中新药业集团股份有限公司第六中药厂 | Composition and pharmaceutical preparation thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215265A (en) * | 2008-01-15 | 2008-07-09 | 四川大学 | Method for integrally extracting and purifying ligustrazine, ferulic acid and volatile oil in ligusticum wallichii |
| CN101768073A (en) * | 2010-02-01 | 2010-07-07 | 南京泽朗医药科技有限公司 | Method for preparing ferulic acid from Chinese angelica |
-
2011
- 2011-08-17 CN CN 201110235878 patent/CN102266364B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215265A (en) * | 2008-01-15 | 2008-07-09 | 四川大学 | Method for integrally extracting and purifying ligustrazine, ferulic acid and volatile oil in ligusticum wallichii |
| CN101768073A (en) * | 2010-02-01 | 2010-07-07 | 南京泽朗医药科技有限公司 | Method for preparing ferulic acid from Chinese angelica |
Non-Patent Citations (2)
| Title |
|---|
| 《中成药》 20090220 李新莹等 川芎中主要有效成分的综合提取分离工艺研究 第31卷, 第02期 * |
| 《齐齐哈尔医学院学报》 20071115 刘亚琴等 当归中阿魏酸的提取与分离 第28卷, 第21期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113797246A (en) * | 2021-10-27 | 2021-12-17 | 首都医科大学附属北京中医医院 | Traditional Chinese medicine composition and preparation method and application thereof |
| CN114469934A (en) * | 2022-02-11 | 2022-05-13 | 天津中新药业集团股份有限公司第六中药厂 | Composition and pharmaceutical preparation thereof |
| CN114469934B (en) * | 2022-02-11 | 2023-08-25 | 津药达仁堂集团股份有限公司第六中药厂 | Composition and pharmaceutical preparation thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102266364B (en) | 2013-03-20 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101463061B (en) | Ginseng saponin Rg1 and Rb1 in pseudo-ginseng and preparation of total saponin thereof | |
| CN101040901A (en) | Rosmarinus officinalis extract and its preparing process and application | |
| CN104844723A (en) | Preparation method and application of dendrobium officinale extract | |
| JP2016503040A (en) | Pharmaceutical composition for treating headache and method for preparing the same | |
| CN102274244A (en) | Cassia bark polyphenol extract and preparation method and application thereof | |
| CN1326814C (en) | Process for preparing Erigeron breviscapus active component | |
| CN102266364B (en) | Traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and preparation method thereof | |
| CN101254217B (en) | Preparation of extract of regeneratabl portion of yew and applications of same for preparing oral anti-cancer medicine | |
| CN101849950A (en) | Application of rotundic acid in preparing blood lipid regulating medicines | |
| CN1943569B (en) | Chinese medicine active component composition and its preparing method and use | |
| CN101297823A (en) | Medicament for preventing and treating Alzheimer's disease | |
| CN101703561A (en) | Eucommia bark effective position for treating osteoporosis and preparation method thereof | |
| KR20130130580A (en) | Composition for preventing or treating gout containing mixed medicinal herbs extracts and method of preparing the extracts | |
| KR101719709B1 (en) | Composition for preventing or treating metabolic disorders comprising extracts of Lonicera japonica Thunb. and Rehmannia glutinosa Liboch | |
| CN101612184B (en) | Multiradiate fleabane extract, composition containing same, preparation method and application thereof | |
| CN101856357B (en) | Application of rotundic acid in preparing medicines for preventing and treating cardiovascular and cerebrovascular diseases | |
| CN1321632C (en) | Compound saussurea involucrata capsule and its preparation process | |
| CN102670852A (en) | Spraying agent for resisting inflammatory and relieving pains as well as preparation method and application of spraying agent | |
| US8633332B2 (en) | Efficient isolation of cimiracemate A, and methods of use | |
| CN101843669B (en) | Chinese medicinal effective-part composition for treating coronary heart diseases | |
| CN100486621C (en) | Chinese medicinal composition for treating hemilateral headache and its preparation method | |
| CN102258587B (en) | Preparation method and application of red paeony root active ingredient | |
| CN102293816B (en) | Production method of rheumatism dripping pill | |
| CN103450142B (en) | Chroman compound as well as extracting method and application thereof | |
| CN102379864A (en) | Compound salvianic acid injection for treating cerebral vascular thrombosis diseases and preparation process thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C41 | Transfer of patent application or patent right or utility model | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20170213 Address after: Ji'an City, Jilin province 134200 Lumin Yajiang Bridge Street No. 31 Patentee after: JILIN TONGHUA BOXIANG PHARMACEUTICAL Co.,Ltd. Address before: 510640 Tianhe District, Guangdong, No. five road, No. 381, Patentee before: South China University of Technology |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: Traditional Chinese medicine effective part for treating cardiovascular and cerebrovascular diseases and preparation method thereof Effective date of registration: 20200506 Granted publication date: 20130320 Pledgee: Tonghua Branch of China Everbright Bank Co.,Ltd. Pledgor: JILIN TONGHUA BOXIANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2020980002001 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PC01 | Cancellation of the registration of the contract for pledge of patent right |
Date of cancellation: 20220711 Granted publication date: 20130320 Pledgee: Tonghua Branch of China Everbright Bank Co.,Ltd. Pledgor: JILIN TONGHUA BOXIANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2020980002001 |
|
| PC01 | Cancellation of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: An effective part of traditional Chinese medicine for treating cardiovascular and cerebrovascular diseases and its preparation method Effective date of registration: 20220713 Granted publication date: 20130320 Pledgee: Tonghua Branch of China Everbright Bank Co.,Ltd. Pledgor: JILIN TONGHUA BOXIANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2022220000033 |
|
| PE01 | Entry into force of the registration of the contract for pledge of patent right |