CN1255100C - Soft capsule preparation of Tibet medicine 'unique taste' - Google Patents
Soft capsule preparation of Tibet medicine 'unique taste' Download PDFInfo
- Publication number
- CN1255100C CN1255100C CN 200410031071 CN200410031071A CN1255100C CN 1255100 C CN1255100 C CN 1255100C CN 200410031071 CN200410031071 CN 200410031071 CN 200410031071 A CN200410031071 A CN 200410031071A CN 1255100 C CN1255100 C CN 1255100C
- Authority
- CN
- China
- Prior art keywords
- soft capsule
- add
- radix lamiophlomidis
- lamiophlomidis rotatae
- preparation
- 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.)
- Expired - Lifetime
Links
- 239000007901 soft capsule Substances 0.000 title claims abstract description 89
- 238000002360 preparation method Methods 0.000 title claims abstract description 65
- 239000003814 drug Substances 0.000 title claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 122
- 239000000843 powder Substances 0.000 claims abstract description 118
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 88
- 239000000284 extract Substances 0.000 claims abstract description 77
- 238000000605 extraction Methods 0.000 claims abstract description 34
- 238000000034 method Methods 0.000 claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 17
- 229920005989 resin Polymers 0.000 claims abstract description 17
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- 239000003549 soybean oil Substances 0.000 claims abstract description 13
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 13
- 238000005325 percolation Methods 0.000 claims abstract description 8
- MWDZOUNAPSSOEL-UHFFFAOYSA-N kaempferol Natural products OC1=C(C(=O)c2cc(O)cc(O)c2O1)c3ccc(O)cc3 MWDZOUNAPSSOEL-UHFFFAOYSA-N 0.000 claims description 47
- 239000000243 solution Substances 0.000 claims description 47
- 238000001035 drying Methods 0.000 claims description 46
- 235000009498 luteolin Nutrition 0.000 claims description 42
- IQPNAANSBPBGFQ-UHFFFAOYSA-N luteolin Chemical compound C=1C(O)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(O)C(O)=C1 IQPNAANSBPBGFQ-UHFFFAOYSA-N 0.000 claims description 42
- LRDGATPGVJTWLJ-UHFFFAOYSA-N luteolin Natural products OC1=CC(O)=CC(C=2OC3=CC(O)=CC(O)=C3C(=O)C=2)=C1 LRDGATPGVJTWLJ-UHFFFAOYSA-N 0.000 claims description 41
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- REFJWTPEDVJJIY-UHFFFAOYSA-N Quercetin Chemical compound C=1C(O)=CC(O)=C(C(C=2O)=O)C=1OC=2C1=CC=C(O)C(O)=C1 REFJWTPEDVJJIY-UHFFFAOYSA-N 0.000 claims description 12
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- JLPULHDHAOZNQI-ZTIMHPMXSA-N 1-hexadecanoyl-2-(9Z,12Z-octadecadienoyl)-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCCCCCC\C=C/C\C=C/CCCCC JLPULHDHAOZNQI-ZTIMHPMXSA-N 0.000 claims description 5
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- SYYHBUHOUUETMI-UHFFFAOYSA-N Pennogenin Natural products O1C2CC3C4CC=C5CC(O)CCC5(C)C4CCC3(C)C2(O)C(C)C21CCC(C)CO2 SYYHBUHOUUETMI-UHFFFAOYSA-N 0.000 claims description 3
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- KZNIFHPLKGYRTM-UHFFFAOYSA-N apigenin Chemical compound C1=CC(O)=CC=C1C1=CC(=O)C2=C(O)C=C(O)C=C2O1 KZNIFHPLKGYRTM-UHFFFAOYSA-N 0.000 claims description 3
- XADJWCRESPGUTB-UHFFFAOYSA-N apigenin Natural products C1=CC(O)=CC=C1C1=CC(=O)C2=CC(O)=C(O)C=C2O1 XADJWCRESPGUTB-UHFFFAOYSA-N 0.000 claims description 3
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- 229940117893 apigenin Drugs 0.000 claims description 3
- RPMNUQRUHXIGHK-PYXJVEIZSA-N apigenin 7-O-neohesperidoside Chemical compound O[C@@H]1[C@H](O)[C@@H](O)[C@H](C)O[C@H]1O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=CC(O)=C2C(=O)C=C(C=3C=CC(O)=CC=3)OC2=C1 RPMNUQRUHXIGHK-PYXJVEIZSA-N 0.000 claims description 3
- 229930034861 apigenin-7-O-neohesperidoside Natural products 0.000 claims description 3
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Abstract
The present invention discloses a soft capsule preparation with an extract of the effective part of a Tibetan medicine-lamiophlomis as the main raw material and a preparation method thereof. The extract of the effective part of the soft capsule of the present invention can be obtained by the methods of extraction by boiling with water, ethanol reflux, extraction by percolation, etc., and the extract is separated and purified by the methods of extraction by an organic solvent, adsorption with a macroporous resin, etc.; a suspending agent-beeswax and the fine powder of the extract are added into soybean oil and are uniformly mixed; the mixture is pressed by a colloidal mill to form the soft capsule preparation of the present invention. The soft capsule of the present invention has the preferable functions of alleviating pain and stopping bleeding. The soft capsule can be used for stopping bleeding, alleviating pain, resisting bacteria, relieving inflammation and activating blood circulation to dissipate blood stasis clinically. The soft capsule also has the advantages of quick disintegration in the gastrointestinal track, quick absorption and effect, little dosage, high biological availability, outstanding curative effect, high stability, etc.
Description
Technical field
The present invention relates to a kind of single medicinal material soft capsule preparation and preparation method thereof, particularly relate to soft capsule preparation of a kind of Tibet medicine lamivphlomis root and preparation method thereof, belong to medical technical field.
Background technology
Radix Lamiophlomidis Rotatae Lamiophlomis rotata (Benth.) Kudo is a labiate, belongs to Paraphlomis (Phlomis Linn) originally, has now told to become independently from this genus to belong to, claim Radix Lamiophlomidis Rotatae to belong to, only a kind, have another name called unrivalled leading to, Tibetan language also claims " big bus ", " beating the cloth crust ".Its root and rhizome or herb people medicine are one of national folks such as China Tibetan, illiteracy and Nahsi medical herbs commonly used.Being that Tibetan, illiteracy and Nahsi are among the people flows yellow fluid after being commonly used to treat cutter, gunshot wound, traumatic injury, edema, the medical herbs of illness such as arthritis has the effect of hemostasis and pain-relieving, anti-inflammation, blood circulation promoting and blood stasis dispelling.
The modern pharmacological research Radix Lamiophlomidis Rotatae has following pharmacological action:
Analgesic activity: 10% Radix Lamiophlomidis Rotatae extractum 0.28ml/10g or 0.14ml/10g gives mice lavage, analgesic activity arranged, about 2 hours of persistent period; The analgesic activity of Radix Lamiophlomidis Rotatae extractum 0.19-3.0g/kg is suitable with the aspirin of 0.23g/kg.
Anastalsis: 10% or 5% Radix Lamiophlomidis Rotatae extractum 0.14ml/10g, give mice lavage, the bleeding time by administration before 7.1-7.7 minute, foreshorten to 4.7 and 3.2 minutes respectively (P＜0.01), showing has anastalsis.
Antibacterial action: Radix Lamiophlomidis Rotatae extractum has bacteriostasis to beta hemolytic streptococcus and aerobacteria.Radix Lamiophlomidis Rotatae leaf Saponin all has bacteriostasis to La Shigella, bacillus pyocyaneus, aerobacteria, bacillus subtilis and beta hemolytic streptococcus.
Immunization: Radix Lamiophlomidis Rotatae extractum can improve macrophage phagocytic rate, macrophage phagocytic index, E one garland formation rate and esterase dyeing positive rate, shows that Radix Lamiophlomidis Rotatae has the effect that improves nonspecific immunity and specific cellular immunity.
Tibet medicine lamivphlomis root confirms that through toxicological experiment its toxic and side effects is little, its pain relieving, hemostasis, antibacterial, and the mechanism of action that increases immunity of organisms makes it that use value widely be arranged aspect surgical wound.Surgical clinical can be used for the analgesia of treatment fracture, prolapse of lumbar intervertebral disc, osteoarthritis, rheumatoid arthritis etc.
According to chemistry and the pharmacological experiments to Radix Lamiophlomidis Rotatae, it has outside analgesia preferably and the hemostatic function.Clinically can be used for treating that rotten to the corn hemorrhagic gastritis, digestive ulcerative bleeding, migraine, urinary system infection are hemorrhage, the urinary stone analgesia is hemorrhage, chronic bacterial prostatitis etc.
The effect that Tibet medicine lamivphlomis root also has strengthening the body resistance and improves immunologic function, this medicine also has better curative effect to the side effect that family planning operation causes, particularly to putting the dripping colporrhagia not to the utmost of ring and medicine stream postoperative drop shape, than the Western medicine better efficacy, show that this product is promising Chinese medicine, be worth clinical application.
In addition, Radix Lamiophlomidis Rotatae also contains 17 seed amino acids and 21 kinds of trace element, and the reparation that can be articular cartilage provides enriches the prescribing adequate nutrition material, thereby reaches the purpose of bone and muscle strengthening.
Tibet medicine lamivphlomis root is extensive in clinical practice, and is effective, and toxic and side effects is little, has much clinical value.But pain management, hemorrhage symptom need a kind of can dose for a short time clinically, and rapid-action medicine satisfies the clinical application needs, for abundant exploitation Tibetan medicine resource, increase the Tibetan medicine dosage form, are the important research directions of common lamiophlomis root preparation exploitation.
Summary of the invention
The purpose of this invention is to provide a kind of effective part extract with Tibet medicine lamivphlomis root is the soft capsule preparation of primary raw material; Second purpose of the present invention is that the effective part extract with Tibet medicine lamivphlomis root is the preparation technology of a kind of soft capsule preparation of primary raw material.
Duyiwei soft capsule preparation of the present invention is made by following bulk drugs: Radix Lamiophlomidis Rotatae extract 26 weight portions, vegetable oil 29 weight portions, suspending agent 3 weight portions.
Above-mentioned Duyiwei soft capsule preparation also can be made by following bulk drugs: Radix Lamiophlomidis Rotatae extract 20～30 weight portions, vegetable oil 25～36 weight portions, suspending agent 1～5 weight portion.
Contain liposoluble constituent 14%～21%, flavonoid and glycoside 8%～60%, polysaccharide 25%～65% in the Radix Lamiophlomidis Rotatae extract of above-mentioned Duyiwei soft capsule preparation.Described liposoluble constituent is 5,7,3 ', 4 '-kaempferol, 5,7,3 ', 4 '-first flavonol-7-O-β-D-glucoside, Quercetin, Quercetin-3-O-β-L-arabinose glycosides, 5,7,4 '-trihydroxyflavone-7-O-β-neohesperidoside, the pennogenin glucosides, cupreol and positive tritriacontane; Described flavonoid and glycoside are luteolin, and luteolin-7-O-glucoside, Quercetin, Quercetin-O-can draw uncle's glucosides, apigenin, apigenin-7-O neohesperidoside, cupreol.
All can obtain the above-mentioned Duyiwei soft capsule of the present invention by following technological means:
Process program 1,
1. get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, decoct with water secondary, add the water of 10～30 times of amounts for the first time, decocted 1～2 hour, for the second time add 10～20 times of water gagings, decocted 0.5～1.5 hour, merge medicinal liquid, filter, filtrate is condensed into thick paste, and drying under reduced pressure is ground into fine powder, and it is standby to cross 200 mesh sieves.
2. get vegetable oil and be heated to 80 ℃, add suspending agent, it is dissolved, cool to about 40 ℃, add above-mentioned extractum fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
Process program 2,
1. get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, decoct with water secondary, add the water of 10～30 times of amounts for the first time, decocted 1～2 hour, add 10～20 times of water gagings for the second time, decocted 0.5～1.5 hour, merge medicinal liquid, filtration, concentrated standby.
2. concentrated solution is crossed the macropore resin bed and analysed post, with 30～50 times of distilled water eluting, collect eluent and be condensed into thick paste, drying under reduced pressure is ground into fine powder, and it is standby to cross 200 mesh sieves.
3. get vegetable oil and be heated to 80 ℃, add suspending agent, it is dissolved, cool to about 40 ℃, add above-mentioned extractum fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
Process program 3,
1. get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, add 70%～99% alcohol reflux 2～3 times, add 8～12 times of amounts of ethanol for the first time, refluxed 1～3 hour, add 6～10 times of amounts of ethanol, refluxed 1～2 hour for the 2nd, 3 time.Merge backflow, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the alcohol extraction concentrated solution.
2. after the alcohol extraction concentrated solution adds the water suspendible, use petroleum ether, n-butanol extraction 2～3 times successively, reclaim solvent, drying obtains ligroin extraction A, n-butanol extract B, and extracting remainder is water extract C.
3. merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, it is standby to cross 200 mesh sieves.Get vegetable oil and be heated to 80 ℃, add suspending agent, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
Process program 4,
1. get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, place percolator with 70%～90% soak with ethanol after 12～36 hours, with the speed percolation of 5ml～10ml/min, until effluent till thin layer chromatography detects immaculate.Concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the Radix Lamiophlomidis Rotatae percolate.
2. the Radix Lamiophlomidis Rotatae percolate is added water and left standstill 12～36 hours, obtain precipitate A, drying for standby.Supernatant is crossed the macropore resin bed and is analysed post, uses 30～50 times of distilled water respectively, and 30～50 times of 15%～45% ethanol elution reclaims ethanol, and drying obtains extract B, C.
3. merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, it is standby to cross 200 mesh sieves.Get vegetable oil and be heated to 80 ℃, add suspending agent, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
The used vegetable oil of the present invention can be one or more in soybean oil, salad oil, Oleum Sesami, Oleum Arachidis hypogaeae semen, Semen Maydis oil, almond oil, peach kernel oil, Oleum Gossypii semen, Oleum Helianthi, Oleum Ricini, the olive oil; Described suspending agent can be any one or a few in glycerol, tween 80, Petiolus Trachycarpi oil, aluminum monostearate, soybean lecithin, the Cera Flava etc.
The quality standard control of the invention described above soft capsule:
The thin layer chromatography of [discriminating] Radix Lamiophlomidis Rotatae is differentiated
The present invention is the soft capsule of Radix Lamiophlomidis Rotatae through being processed into, and adopting the TLC method is contrast with the Radix Lamiophlomidis Rotatae control medicinal material, differentiates Radix Lamiophlomidis Rotatae in this product, this method favorable reproducibility, and specificity is strong.
Get this product content 0.3g, add ethanol 5ml, reflux 10 minutes filters, and gets filtrate 2ml, is concentrated into about 1ml, as need testing solution.
Other gets Radix Lamiophlomidis Rotatae control medicinal material 1g, shines medical material solution in pairs with legal system.
According to thin layer chromatography (" Chinese Pharmacopoeia 2000 version one one " appendix VIB) test, draw each 5 μ l of above-mentioned two kinds of solution, put on same silica gel g thin-layer plate respectively and (do not activate), with chloroform-methanol (4: 1) is developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, about 15 minutes of 105 ℃ of heating.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
[assay] adopts high effective liquid chromatography for measuring
The assay of luteolin
(1) chromatographic condition chromatographic column: Hypersil BDS C
18(4.6 * 150mm, 5 μ m)
Mobile phase: methanol-0.2% phosphoric acid solution (40: 60), detect wavelength 350nm, detection sensitivity 0.01AUFS, column temperature: 30 ℃, flow velocity: 1.0ml/min, sample size: 10 μ l.
(2) preparation of contrast solution: it is an amount of that precision takes by weighing the luteolin reference substance, adds methanol and make the solution that every 1ml contains 25 μ g, promptly.
(3) preparation of need testing solution: get each respectively and extract the about 2g of extract powder that tests under the item, the accurate title, decide, put respectively in the 100ml ground tool plug triangular flask, precision adds methanol 25ml and claims to decide weight, supersound process 30 minutes, put cold, claim again to decide weight, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate as need testing solution.
(4) linear relationship: it is an amount of that precision takes by weighing the luteolin reference substance, add methanol and make the solution that every 1ml contains 28.5 μ g, draw this solution 2,5,8,10,12,15 μ l, inject high performance liquid chromatograph, by above-mentioned chromatographic determination luteolin absworption peak area, be A with the integrated value of luteolin absworption peak area, sample size is C, linear regression gets regression equation: A=4 * 10
6C-11414, R=0.9999 (n=6), the result shows that concentration and area are good linear relationship in 0.057 μ g～0.4275 μ g scope.
(5) recovery test: precision takes by weighing the sample 1g of known content, and the accurate luteolin sodium reference substance that adds is an amount of, presses the preparation of need testing solution preparation method, and by above-mentioned chromatographic condition test, average recovery rate is 99.68%, and RSD is 1.21% (n=6).
The content of luteolin in this product Radix Lamiophlomidis Rotatae, the content of every luteolin contains Radix Lamiophlomidis Rotatae in luteolin according to every of measurement result regulation this product in this product sample between 0.8000mg～1.8105mg after measured, must not be less than 0.8000mg.
Duyiwei soft capsule agent provided by the invention means that Radix Lamiophlomidis Rotatae medicinal material extract extract powder is added suitable adjuvant is sealed in the medicament of making in the soft capsule material of sphere, ellipse or other shapes, it has the following advantages: compare with existing dosage form, this dosage form taking dose is little, disintegrate is fast in intestines and stomach, absorb, produce effects is also fast, bioavailability height, determined curative effect, preparation stability strengthens.The Radix Lamiophlomidis Rotatae extract purity height that obtains among the Duyiwei soft capsule agent preparation technology provided by the invention, hemostasis, the analgesic curative effect is clear and definite.
Following experimental example is used to further specify the present invention.
Experimental example 1 Radix Lamiophlomidis Rotatae water is obtained through refining technical study fully
(1), optimum process condition determines
1. the investigation of degree of grinding
Duyiwei soft capsule adopts the decocting cooking method to extract effective ingredient in the Radix Lamiophlomidis Rotatae, and Radix Lamiophlomidis Rotatae is the whole grass medicine, directly decocts the proposition that is unfavorable for effective ingredient, after it is pulverized, increases the specific surface area of medicine, is beneficial to the extraction of effective ingredient.
Get three parts of Radix Lamiophlomidis Rotatae medical materials, each 1000g, pulverize separately becomes coarse powder, and (referring to can be all by a sieve, can be no more than 20% powder by No. three sieves but be mixed with), coarse powder (refers to and can all sieve by No. two, can be no more than 40% powder by No. four sieves but be mixed with), middle powder (refer to and can be no more than 60% powder by No. five sieves but be mixed with) all by No. four sieves, serve as the investigation index with the rate of filtration, the extract powder yield that decocts medicinal liquid, investigate the pulverizing medicinal materials fineness, the results are shown in Table 1.
The fineness test of table 1 pulverizing medicinal materials
| Inventory (g) | Degree of grinding | The rate of filtration | Extract powder yield (%) |
| 1000 1000 1000 | Powder in the coarse powder coarse powder | Slowly very slow rapidly | 25.7 26.4 27.2 |
Result of the test shows, the Radix Lamiophlomidis Rotatae pulverizing medicinal materials is become coarse powder, coarse powder, middle powder are through decocting extract powder yield no significant difference, and that coarse powder decocts medical filtration is rapid, in powder, coarse powder to decoct medical filtration speed slow, operation in being not easy to produce is so selection decocts after Radix Lamiophlomidis Rotatae is ground into coarse powder.
2. the investigation of water absorption rate
Get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, take by weighing three parts, each 1000g adds the water logging bubble 12 hours of 20 times of amounts respectively, and the elimination surplus water divides another name every part of medical material weight again, calculates water absorption rate, the results are shown in Table 2.
Table 2 moisture content test result
| Numbering | Medical material weight (g) before soaking | Soak back medical material heavy (g) | Water absorption rate (%) |
| 123 | 1,000 1,000 1000 | 4,816 4,834 4764 | 381.6% 383.4% 376.4% |
| Average water absorption rate is 380.47%. | |||
3. optimum extraction condition determines
Contained analgesia in the Radix Lamiophlomidis Rotatae, hemostasis effective ingredient are based on flavonoid, glycoside, saccharide etc., and these chemical compounds dissolubility in water is big.In this product Study on Preparation, serve as to investigate index with the content that gets powder rate and luteolin, to the decoction number of times of influence decoction effect, decocting time, amount of water screens, and concrete grammar is as follows.
Decoct number of times to decocting the influence of effect
Get three parts of Radix Lamiophlomidis Rotatae medical materials, every part of 1000g adds 20 times water, decocts respectively 1 time, 2 times, 3 times, filters respectively, and filtrate concentrates, and drying calculates the powder rate and measures the content of luteolin, the results are shown in Table 3.
Table 3 decocts number of times to decocting the influence of effect
| Inventory (g) | Decoct number of times (inferior) | Get powder rate (%) | Content of luteolin (%) |
| 1000 1000 1000 | 1 2 3 | 15.49 21.17 23.24 | 0.021 0.037 0.032 |
The result shows, decocts 2 times and decocts 3 times, and it is approaching to get powder rate and content of luteolin, for reducing production costs, selects to decoct 2 times.
Decocting time is to decocting the influence of effect
Get three parts of Radix Lamiophlomidis Rotatae medical materials, every part of 1000g, the decocting that adds 20 times boils secondary, each decocting time is pressed A (1 hour, 1 hour) respectively, three groups of testing programs of B (1 hour, 0.5 hour) C (1.5 hours, 1 hour) are investigated, calculate the powder rate, and measure the content of luteolin, the results are shown in Table 4.
Table 4 decocting time is to decocting the influence of effect
| Inventory (g) | Decocting time (hour) | Get powder rate (%) | Content of luteolin (%) |
| 1000 1000 1000 | A(1，0.5) B(1，1) C(1.5，1) | 20.08 21.75 25.37. | 0.022 0.029 0.035 |
(annotate: the numerical value in the decocting time bracket is respectively the first time, secondary decocting time).
The result shows: the content that A group testing program gets powder rate and luteolin is minimum, and the content that C group testing program gets powder rate and luteolin is the highest, so select C group testing program, promptly decocts secondary, decocts 1.5 hours for the 1st time, decocts 1 hour for the 2nd time.
Amount of water is to decocting the influence of effect
Get three parts of Radix Lamiophlomidis Rotatae medical materials, every part of 1000g decocts secondary, each 1 hour, each amount of water was pressed A (15 times, 10 times) respectively, and three groups of testing programs of B (20 times, 15 times) C (25 times, 20 times) are investigated, calculate the powder rate and measure the content of luteolin, the results are shown in Table 5.
Table 5 amount of water is to decocting the influence of effect
| Inventory (g) | Amount of water (doubly) | Get powder rate (%) | Content of luteolin (%) |
| 1000 1000 1000 | A(15，10) B(20，15) C(25，20) | 14.51 21.19 23.63 | 0.023 0.037 0.029 |
(annotate: the numerical value in the amount of water bracket is respectively the first time, secondary amount of water).
The result shows: A group testing program get the powder rate and content of luteolin minimum, it is close with C group testing program that B group testing program gets the powder rate, and the relative amount of luteolin is higher than the C group, so in conjunction with curative effect and dose, reduce production costs, select B prescription case, promptly decoct secondary, the water that adds for the first time 20 times of amounts adds the water of 15 times of amounts the second time.
Above result of the test shows that this product optimum extraction process is: Radix Lamiophlomidis Rotatae is ground into coarse powder and decocts with water secondary, adds 20 times of water gagings for the first time, decocts 1.5 hours, and add 15 times of water gagings the second time, decocted 1 hour.
Experimental example 2 Radix Lamiophlomidis Rotatae water are put forward the optimum extraction process demonstration test
Get 10 times of recipe quantity Radix Lamiophlomidis Rotatae medical materials, be ground into coarse powder, take by weighing three parts, every part of 10000g carries out three batch sample process certifications test by said extracted technology respectively, the results are shown in Table 6.
Table 6 optimum extraction process demonstration test
| Lot number | Inventory (g) | Get powder amount (g) | Get powder rate (%) | Content of luteolin (%) |
| 1 2 3 | 10000 10000 10000 | 2448.6 2234.1 2692.5 | 24.49 22.34 26.92 | 0.033 0.031 0.026 |
Experimental example 3 Radix Lamiophlomidis Rotatae water are carried the separation impurity removal process
In order to remove solid particle in the medicinal liquid, use filter method in the production more.Because our Radix Lamiophlomidis Rotatae is very easily well-done in heating process, make medicinal liquid muddiness, thickness, be difficult to filter, and become the extract powder moisture absorption strong.Repetition test proves that medicinal liquid is made filter material with canvas while hot, carries out coarse filtration with filter press, and folder 8 metafiltration paper repeat filter pressing in the filtrate reuse fine canvas, and obtain clear liquid.
Filtrate is crossed the macropore resin bed and is analysed post, and the water eluting can be removed impurity such as vegetable protein, tannin.Investigation to the eluting amount of water sees Table 7.
Table 7 eluting amount of water is to getting the influence of powder rate
| Concentrated filtrate (g) | Eluting amount of water (doubly) | Get powder rate (%) |
| 1000 1000 1000 | A(30) B(40) C(50) | 16.36 19.86 20.13 |
The result shows: it is minimum that A group testing program gets the powder rate, and it is close with C group testing program that B group testing program gets the powder rate, thus consider the problem of production cost, selection B prescription case, promptly filtrate is crossed the macropore resin bed and is analysed behind the post with 40 times of water elutions.
Experimental example 4 Radix Lamiophlomidis Rotatae alcohol reflux condition researchs
In Radix Lamiophlomidis Rotatae ethanol extraction technical study, with the content of powder rate and luteolin serves as to investigate index, to influencing the backflow number of times of extraction effect, return time, concentration of alcohol and amount of alcohol are screened, concrete grammar is as follows:
Get three parts of Radix Lamiophlomidis Rotatae medical materials, every part of 1000g, by different backflow number of times, return time, concentration of alcohol and amount of alcohol concentrate, and drying calculates the powder rate and measures the content of luteolin, the results are shown in Table 8.
The different extraction conditions of table 8 are to the influence of extraction effect
| Inventory (g) | Backflow number of times (inferior) | Concentration of alcohol (%) | Get powder rate (%) | Content of luteolin (%) |
| 1000 | 2 | 75 | 21.41 | 0.022 |
| 85 | 22.58 | 0.026 | ||
| 95 | 23.15 | 0.029 | ||
| 1000 | 3 | 75 | 22.17 | 0.027 |
| 85 | 23.36 | 0.030 | ||
| 95 | 24.87 | 0.034 | ||
| 1000 | 4 | 75 | 23.11 | 0.027 |
| 85 | 24.57 | 0.032 | ||
| 95 | 24.92 | 0.036 |
The result shows, the alcohol reflux with 95% 3 times, and it is the highest to get powder rate and content of luteolin, so select the alcohol reflux with 95% to extract Radix Lamiophlomidis Rotatae 3 times.
Determining of experimental example 5 extract powder fineness
During preparation suspendible body, from sedimentation formula (stock`s formula) V=2r of suspension
2(d
1-d
2) (V is the microgranule sedimentation velocity to g/9 η, and r is a particle radius, d
1Be density of particle, d
2Be disperse medium density, η is the viscosity of disperse medium) can know by inference, reduce granularity, increase dispersion medium viscosity and can reduce sedimentation velocity effectively, guarantee the stability of suspension.So thin more easy more mixing of the granularity of extract dry powder.Now be to investigate the optimum fineness that index is determined extract powder in this product preparation with the settling ratio.
Get three parts of each 50g of Radix Lamiophlomidis Rotatae extract dry powder, pulverize separately became the fine powder of 80 orders, 120 orders, 200 mesh sieves.Get above-mentioned three kinds of each 5g of fine powder and put respectively in the identical 50ml tool plug graduated cylinder of diameter, add same disperse medium (soybean oil: Cera Flava=10: 1), placed 3 hours, measure its settling ratio.3 parts of operation repetitives the results are shown in Table 9.
Settling ratio F=Hu/Ho
Ho is an original height in the formula, the height of Hu for showing through sedimentation after leaving standstill.
The extract powder settling ratio measurement result of table 9 different fineness
| The extract powder fineness | Settling ratio |
| 80 orders, 120 orders, 200 orders | 0.38 0.76 0.92 |
Result of the test showed that the fine powder F value of 200 mesh sieves was maximum, therefore Radix Lamiophlomidis Rotatae extract dry powder was broken into the fine powder of 200 mesh sieves, and the soft capsule content suspendible system of making is the most stable.
The optimization screening of experimental example 6 preparation soft capsule prescriptions and adjuvant
For determining best adjuvant in this product preparation, drafted 4 prescriptions, settling ratio, the content uniformity of finished product, the yield rate with content serves as to investigate index respectively, screens best adjuvant.
The design of prescription
| Prescription 1 | Radix Lamiophlomidis Rotatae extract dry powder salad oil soybean phospholipid | 260g 300g 20g |
| Make | 1000 | |
| Prescription 2 | Radix Lamiophlomidis Rotatae extract dry powder soybean oil Petiolus Trachycarpi oil | 260g 260g 60g |
| Make | 1000 |
| Prescription 3 | Radix Lamiophlomidis Rotatae extract dry powder soybean oil Petiolus Trachycarpi oil soybean phospholipid | 260g 268g 42g 10g |
| Make | 1000 | |
| Prescription 4 | Radix Lamiophlomidis Rotatae extract dry powder soybean oil Cera Flava | 260g 290g 30g |
| Make | 1000 |
1. the mensuration of soft capsule content settling ratio
It is an amount of to get the soft capsule content that above-mentioned different prescription makes, and puts respectively in the identical 50ml tool plug graduated cylinder of diameter, places and measures its settling ratio, 3 parts of operation repetitives in 3 hours.The results are shown in Table 10.
The different prescriptions of table 10 are made soft capsule content settling ratio measurement result
| The prescription number | Settling ratio |
| No. 1 No. 2 No. 3 No. 4 | 0.85 0.54 0.67 0.92 |
2. the investigation of content uniformity and yield rate
Above 4 kinds of different prescriptions are made the soft capsule content uniformity and yield rate is investigated, the results are shown in Table 11.
Inspection of table 11 content uniformity and yield rate are investigated the result
| The prescription number | Content uniformity | Yield rate (%) |
| No. 1 No. 2 No. 3 No. 4 | Qualified | 72.3 65.8 62.2 91.34 |
Result of the test shows that prescription 1,2,3,4 soft capsule contents that make are even, stable, good fluidity, and yield rate height, content uniformity are checked up to specification, and selecting prescription 4 is best prescription.
The pharmacodynamics test of experimental example 7 Radix Lamiophlomidis Rotatae extracts
1, alcohol reflux liquid obtains extract A, B, C respectively with petroleum ether, n-butyl alcohol, water extraction.Investigate extract A, B, C analgesic activity with acetic acid white mice writhing method, investigate the anastalsis of extract A, B, C with white mice tail vein hemostasis trial mice.The results are shown in Table 12.
The analgesia of table 12 extract A, B, C, anastalsis
| Extract | Analgesia percentage rate (%) | Bleeding time shortens (branch) |
| A B C | 85 90 100 | 2.3 4.7 3.8 |
The result shows that extract A, B, C all have certain hemostatic analgesia effect.
2, ethanol percolation liquid obtains extract A with water precipitation, and supernatant is crossed macroporous resin, and water, ethanol elution obtain extract B, C respectively.
Investigate extract A, B, C analgesic activity with acetic acid white mice writhing method, investigate the anastalsis of extract A, B, C with white mice tail vein hemostasis trial mice.The results are shown in Table 13.
The analgesia of table 13 extract A, B, C, anastalsis
| Extract | Analgesia percentage rate (%) | Bleeding time shortens (branch) |
| A B C | 90 100 90 | 3.9 5.2 3.3 |
The result shows that extract A, B, C all have certain hemostatic analgesia effect.
The said extracted thing analyze to be found through thin layer chromatography (TLC): the part of Petroleum ether extraction be liposoluble constituent (5,7,3 ', 4 '-kaempferol, 5,7,3 ', 4 '-first flavonol-7-O-β-D-glucoside, Quercetin, Quercetin-3-O-β-L-arabinose glycosides, 5,7,4 '-trihydroxyflavone-7-O-β-neohesperidoside, the pennogenin glucosides, cupreol and positive tritriacontane etc.), account for 14%～18%; The part of n-butanol extraction is flavonoid and glycoside (luteolin, luteolin-7-O-glucoside, Quercetin, Quercetin-O-galactoside, apigenin, apigenin-7-O neohesperidoside, cupreol etc.), accounts for 8%～22%; The part that water is carried is that polysaccharide accounts for 55%～65%.
Differentiate discovery through thin layer chromatography (TLC), water deposit is similar to ligroin extraction in the macroporous resin partition method, is liposoluble constituent, accounts for 16%～21%; The water elution part is similar to water extract in the alcohol reflux, for the polysaccharide composition, accounts for 25%～30%; Ethanol elution part is similar to the n-butanol extract composition, for flavonoid and glycosides composition account for 45%～60%.
Embodiment 1The preparation of Duyiwei soft capsule (water extraction)
1, gets Radix Lamiophlomidis Rotatae 1000g, be ground into coarse powder, decoct with water secondary, add the water of 20 times of amounts for the first time, decocted 1.5 hours, for the second time add 15 times of water gagings, decocted 1 hour, merge medicinal liquid, filter, filtrate is condensed into thick paste, and drying under reduced pressure is ground into fine powder, and it is standby to cross 200 mesh sieves; Get extract 260g.
2, get soybean oil 290g and be heated to 80 ℃, add Cera Flava 30g, it is dissolved, cool to about 40 ℃, add above-mentioned extractum fine powder, mixing is pressed into soft capsule, and drying is pressed into soft capsule, through washing ball, being drying to obtain 1000 of Duyiwei soft capsules.
Embodiment 2The preparation of Duyiwei soft capsule (water is carried+macroporous resin adsorption)
1, Radix Lamiophlomidis Rotatae medical material 1000g is ground into coarse powder, decocts with water secondary, adds the water of 20 times of amounts for the first time, decocts 1.5 hours, adds 15 times of water gagings for the second time, decocts 1 hour, merges medicinal liquid, filtration, and filtrate is concentrated standby.
2, concentrated solution is crossed the macropore resin bed and analysed post, with 40 times of water elutions, collect eluent and be condensed into thick paste, drying under reduced pressure is ground into fine powder, and it is standby to cross 200 mesh sieves; Get extract 200g.
3, get Semen Maydis oil 270g and be heated to 80 ℃, add soybean lecithin 20g, it is dissolved, cool to about 40 ℃, add above-mentioned extractum fine powder, mixing is pressed into soft capsule, and drying is pressed into soft capsule, through washing ball, being drying to obtain 1000 of Duyiwei soft capsules.
Embodiment 3The preparation of Duyiwei soft capsule (alcohol reflux+organic solvent extraction)
1, gets Radix Lamiophlomidis Rotatae medical material 1000g, be ground into coarse powder, add 95% alcohol reflux 3 times, add 10 times of amounts of ethanol for the first time, refluxed 2 hours, add 8 times of amounts of ethanol, refluxed 1.5 hours for the 2nd, 3 time.Merge backflow, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the alcohol extraction concentrated solution.
2, after the alcohol extraction concentrated solution adds equivalent distilled water mix homogeneously, use equivalent petroleum ether, n-butanol extraction 3 times successively, reclaim solvent, drying obtains ligroin extraction A45g, n-butanol extract B56g, and extracting remainder is water extract C160g.
3, merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, it is standby to cross 200 mesh sieves.Get olive oil 320g and be heated to 80 ℃, add suspending agent Petiolus Trachycarpi oil 65g, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain 1000 of Duyiwei soft capsules.
Embodiment 4The preparation of Duyiwei soft capsule (ethanol percolation+macroporous resin separates)
1, get Radix Lamiophlomidis Rotatae medical material 1000g, be ground into coarse powder, place percolator with 80% soak with ethanol after 24 hours, with the speed percolation of 5mll/min, until effluent till thin layer chromatography detects immaculate.Concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the Radix Lamiophlomidis Rotatae percolate.
2, the Radix Lamiophlomidis Rotatae percolate is added the equivalent distilled water and left standstill 24 hours, obtain precipitate A51g, drying for standby.Supernatant is crossed the macropore resin bed and is analysed post, and earlier with 40 times of distilled water eluting, eluent reclaims drying and obtains extract B 72g, and 40 times of amounts of reuse, 30% ethanol elution reclaims ethanol in the eluent, and drying obtains extract C 137g.
3, merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, it is standby to cross 200 mesh sieves.Get soybean oil 300g and be heated to 80 ℃, add suspending agent Petiolus Trachycarpi oil 30g, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain 1000 of Duyiwei soft capsules.
Embodiment 5The method of quality control of Duyiwei soft capsule
The thin layer chromatography of [discriminating] Radix Lamiophlomidis Rotatae is differentiated
The present invention is the soft capsule of Radix Lamiophlomidis Rotatae through being processed into, and adopting the TLC method is contrast with the Radix Lamiophlomidis Rotatae control medicinal material, differentiates Radix Lamiophlomidis Rotatae in this product, this method favorable reproducibility, and specificity is strong.
Get this product content 0.3g, add ethanol 5ml, reflux 10 minutes filters, and gets filtrate 2ml, is concentrated into about 1ml, as need testing solution.
Other gets Radix Lamiophlomidis Rotatae control medicinal material 1g, shines medical material solution in pairs with legal system.
According to thin layer chromatography (" Chinese Pharmacopoeia 2000 version one one " appendix VIB) test, draw each 5 μ l of above-mentioned two kinds of solution, put on same silica gel g thin-layer plate respectively and (do not activate), with chloroform-methanol (4: 1) is developing solvent, launch, take out, dry, spray is with the phosphomolybdic acid test solution, about 15 minutes of 105 ℃ of heating.In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
[assay] adopts high effective liquid chromatography for measuring
The assay of luteolin
(1) chromatographic condition chromatographic column: Hypersil BDS C
18(4.6 * 150mm, 5 μ m)
Mobile phase: methanol-0.2% phosphoric acid solution (40: 60), detect wavelength 350nm, detection sensitivity 0.01AUFS, column temperature: 30 ℃, flow velocity: 1.0ml/min, sample size: 10 μ l.
(2) preparation of contrast solution: it is an amount of that precision takes by weighing the luteolin reference substance, adds methanol and make the solution that every 1ml contains 25 μ g, promptly.
(3) preparation of need testing solution: get each respectively and extract the about 2g of extract powder that tests under the item, the accurate title, decide, put respectively in the 100ml ground tool plug triangular flask, precision adds methanol 25ml and claims to decide weight, supersound process 30 minutes, put cold, claim again to decide weight, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate as need testing solution.
(4) linear relationship: it is an amount of that precision takes by weighing the luteolin reference substance, add methanol and make the solution that every 1ml contains 28.5 μ g, draw this solution 2,5,8,10,12,15 μ l, inject high performance liquid chromatograph, by above-mentioned chromatographic determination luteolin absworption peak area, be A with the integrated value of luteolin absworption peak area, sample size is C, linear regression gets regression equation: A=4 * 10
6C-11414, R=0.9999 (n=6), the result shows that concentration and area are good linear relationship in 0.057 μ g～0.4275 μ g scope.
(5) recovery test: precision takes by weighing the sample 1g of known content, and the accurate luteolin sodium reference substance that adds is an amount of, presses the preparation of need testing solution preparation method, and by above-mentioned chromatographic condition test, average recovery rate is 99.68%, and RSD is 1.21% (n=6).
The content of luteolin in this product Radix Lamiophlomidis Rotatae, the content of every luteolin contains Radix Lamiophlomidis Rotatae in luteolin according to every of measurement result regulation this product in this product sample between 0.8000mg～1.8105mg after measured, must not be less than 0.8000mg.
Claims (16)
1, a kind of soft capsule preparation of Radix Lamiophlomidis Rotatae is characterized in that this soft capsule is made up of following bulk drugs: Radix Lamiophlomidis Rotatae extract 20～30 weight portions, vegetable oil 25～36 weight portions, suspending agent 1～5 weight portion;
Wherein Radix Lamiophlomidis Rotatae extract is by any one preparation in following four kinds of extracting method:
I, get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, decoct with water secondary, add for the first time the water of 10～30 times of amounts, decocted 1～2 hour, add 10～20 times of water gagings for the second time, decocted 0.5～1.5 hour, merge medicinal liquid, filter, filtrate is condensed into thick paste, drying under reduced pressure, be ground into fine powder, cross 200 mesh sieves, standby;
II, get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, decoct with water secondary, add the water of 10～30 times of amounts for the first time, decocted 1～2 hour, add 10～20 times of water gagings for the second time, decocted 0.5～1.5 hour, merge medicinal liquid, filtration, concentrated standby; Concentrated solution is crossed the macropore resin bed analyse post, with 30～50 times of distilled water eluting, collect eluent and be condensed into thick paste, drying under reduced pressure is ground into fine powder, crosses 200 mesh sieves, and is standby;
III, get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, add 70%～99% alcohol reflux 2～3 times, add 8～12 times of amounts of ethanol for the first time, refluxed 1～3 hour, add 6～10 times of amounts of ethanol, refluxed 1～2 hour for the 2nd, 3 time; Merge backflow, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the alcohol extraction concentrated solution; After the alcohol extraction concentrated solution adds the water suspendible, use petroleum ether, n-butanol extraction 2～3 times successively, reclaim solvent, drying obtains ligroin extraction A, n-butanol extract B, and extracting remainder is water extract C; Merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, cross 200 mesh sieves, standby;
IV, get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, place percolator with 70%～90% soak with ethanol after 12～36 hours, with the speed percolation of 5ml～10ml/min, until effluent till thin layer chromatography detects immaculate; Concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the Radix Lamiophlomidis Rotatae percolate; The Radix Lamiophlomidis Rotatae percolate is added water left standstill 12～36 hours, obtain precipitate A, drying for standby; Supernatant is crossed the macropore resin bed and is analysed post, uses 30～50 times of distilled water respectively, and 30～50 times of 15%～45% ethanol elution reclaims ethanol, and drying obtains extract B, C; Merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, cross 200 mesh sieves, standby.
2, Duyiwei soft capsule preparation as claimed in claim 1 is characterized in that this soft capsule is made up of following bulk drugs: Radix Lamiophlomidis Rotatae extract 26 weight portions, vegetable oil 29 weight portions, suspending agent 3 weight portions.
3. Duyiwei soft capsule preparation is characterized in that this soft capsule made by following bulk drugs: Radix Lamiophlomidis Rotatae extract 26 weight portions, vegetable oil 29 weight portions, suspending agent 3 weight portions.
4,, it is characterized in that containing in the described Radix Lamiophlomidis Rotatae extract liposoluble constituent 14%～21%, flavone compound and glycoside 8%～60%, polysaccharide 25%～65% as the soft capsule preparation of claim 1,2 or 3 described Radix Lamiophlomidis Rotataes.
5, preparation as claimed in claim 4, it is characterized in that the liposoluble constituent that contains in the described Radix Lamiophlomidis Rotatae extract be 5,7,3 ', 4 '-kaempferol, 5,7,3 ', 4 '-first flavonol-7-O-β-D-glucoside, Quercetin, Quercetin-3-O-β-L-arabinose glycosides, 5,7,4 '-trihydroxyflavone-7-O-β-neohesperidoside, pennogenin glucosides, cupreol and positive tritriacontane;
Flavone compound and glycoside are luteolin, luteolin-7-O-glucoside, Quercetin, Quercetin-O-galactoside, apigenin, apigenin-7-O neohesperidoside, cupreol.
6, as the preparation method of Duyiwei soft capsule preparation as described in claim 1 or 3, it is characterized in that this method is:
Radix Lamiophlomidis Rotatae medical material 100 parts by weight of crushed become coarse powder, decoct with water secondary, add the water of 20 times of amounts for the first time, decoct 1.5 hours, for the second time add 15 times of water gagings, decocted 1 hour, merge medicinal liquid, filter, filtrate is condensed into thick paste, and drying under reduced pressure is ground into fine powder, and it is standby to cross 200 mesh sieves; Get soybean oil 29 weight portions and be heated to 80 ℃, add Cera Flava 3 weight portions, it is dissolved, cool to about 40 ℃, add above-mentioned extractum fine powder, mixing is crossed colloid mill, is pressed into soft capsule, and drying is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
7, the preparation method of Duyiwei soft capsule preparation according to claim 1, it is characterized in that this method is: get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, decoct with water secondary, add the water of 10～30 times of amounts for the first time, decocted 1～2 hour, for the second time add 10～20 times of water gagings, decocted 0.5～1.5 hour, merge medicinal liquid, filter, concentrate standby; Concentrated solution is crossed the macropore resin bed analyse post, with 30～50 times of distilled water eluting, collect eluent and be condensed into thick paste, drying under reduced pressure is ground into fine powder, and it is standby to cross 200 mesh sieves; Get vegetable oil and be heated to 80 ℃, add suspending agent, it is dissolved, cool to about 40 ℃, add above-mentioned extractum fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
8, the preparation method of Duyiwei soft capsule preparation as claimed in claim 7 is characterized in that this method is:
The Radix Lamiophlomidis Rotatae medical material is ground into coarse powder, decocts with water secondary, adds the water of 20 times of amounts for the first time, decocts 1.5 hours, adds 15 times of water gagings for the second time, decocts 1 hour, merges medicinal liquid, filtration, and filtrate is concentrated standby; Concentrated solution is crossed the macropore resin bed analyse post, with 40 times of distilled water eluting, collect eluent and be condensed into thick paste, drying under reduced pressure is ground into fine powder, and it is standby to cross 200 mesh sieves; Get soybean oil and be heated to 80 ℃, add Cera Flava, it is dissolved, cool to about 40 ℃, add above-mentioned extractum fine powder, mixing is crossed colloid mill, is pressed into soft capsule, and drying is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
9, the preparation method of Duyiwei soft capsule preparation according to claim 1, it is characterized in that this method is: get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, add 70%～99% alcohol reflux 2～3 times, add for the first time 8～12 times of amounts of ethanol, refluxed 1～3 hour, and added 6～10 times of amounts of ethanol, refluxed 1～2 hour for the 2nd, 3 time; Merge backflow, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the alcohol extraction concentrated solution; After the alcohol extraction concentrated solution adds the water suspendible, use petroleum ether, n-butanol extraction 2～3 times successively, reclaim solvent, drying obtains ligroin extraction A, n-butanol extract B, and extracting remainder is water extract C; Merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, it is standby to cross 200 mesh sieves; Get vegetable oil and be heated to 80 ℃, add suspending agent, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
10, the preparation method of Duyiwei soft capsule preparation as claimed in claim 9 is characterized in that this method is:
Get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, add 95% alcohol reflux 3 times, add 10 times of amounts of ethanol for the first time, refluxed 2 hours, add 8 times of amounts of ethanol, refluxed 1.5 hours for the 2nd, 3 time; Merge backflow, concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the alcohol extraction concentrated solution; The alcohol extraction concentrated solution is used equivalent petroleum ether, n-butanol extraction 3 times after the water gaging suspendible such as adding successively, reclaims solvent, and drying obtains ligroin extraction A, n-butanol extract B, and extracting remainder is water extract C; Merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, it is standby to cross 200 mesh sieves; Get soybean oil and be heated to 80 ℃, add the suspending agent Cera Flava, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
11, the preparation method of Duyiwei soft capsule preparation as claimed in claim 1, it is characterized in that this method is: get the Radix Lamiophlomidis Rotatae medical material, be ground into coarse powder, place percolator with 70%～90% soak with ethanol after 12～36 hours, with the speed percolation of 5ml～10ml/min, until effluent till thin layer chromatography detects immaculate; Concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the Radix Lamiophlomidis Rotatae percolate; The Radix Lamiophlomidis Rotatae percolate is added water left standstill 12～36 hours, obtain precipitate A, drying for standby; Supernatant is crossed the macropore resin bed and is analysed post, uses 30～50 times of distilled water respectively, and 30～50 times of 15%～45% ethanol elution reclaims ethanol, and drying obtains extract B, C; Merge above-mentioned A, B, three kinds of extracts of C, be ground into fine powder, it is standby to cross 200 mesh sieves; Get vegetable oil and be heated to 80 ℃, add suspending agent, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
12, the preparation method of Duyiwei soft capsule preparation as claimed in claim 11 is characterized in that this method is:
Get Radix Lamiophlomidis Rotatae medical material 100 weight portions, be ground into coarse powder, place percolator with 80% soak with ethanol after 24 hours, with the speed percolation of 5ml/min, until effluent till thin layer chromatography detects immaculate; Concentrating under reduced pressure reclaims ethanol to there not being the alcohol flavor, obtains the Radix Lamiophlomidis Rotatae percolate; The Radix Lamiophlomidis Rotatae percolate is added water left standstill 24 hours, obtain precipitate A, drying for standby; Supernatant is crossed the macropore resin bed and is analysed post, uses 40 times of distilled water respectively, and 40 times of 30% ethanol elution reclaims ethanol, and drying obtains extract B, C; Merge above-mentioned A, B, three kinds of extracts of C totally 26 weight portions, be ground into fine powder, it is standby to cross 200 mesh sieves; Get soybean oil 29 weight portions and be heated to 80 ℃, add suspending agent Cera Flava 3 weight portions, it is dissolved, cool to about 40 ℃, add said extracted thing fine powder, mixing is crossed colloid mill, is pressed into soft capsule, through washing ball, being drying to obtain Duyiwei soft capsule.
13,, it is characterized in that used vegetable oil is one or more in soybean oil, salad oil, Oleum Sesami, Oleum Arachidis hypogaeae semen, Semen Maydis oil, almond oil, peach kernel oil, Oleum Gossypii semen, Oleum Helianthi, Oleum Ricini or the olive oil as the preparation method of claim 7,9 or 11 described Duyiwei soft capsule preparations.
14,, it is characterized in that used suspending agent is any one or a few in glycerol, tween 80, Petiolus Trachycarpi oil, aluminum monostearate, soybean lecithin or the Cera Flava etc. as the preparation method of claim 7,9 or 11 described Duyiwei soft capsule preparations.
15,, it is characterized in that content assaying method is in this method as the method for quality control of claim 1,2 or 3 described Duyiwei soft capsule preparations:
High performance liquid chromatography:
Chromatographic condition chromatographic column: Hypersil BDS C
18
Mobile phase: ratio is 40: 60 methanol-0.2% phosphoric acid solution, detects wavelength 350nm, detection sensitivity 0.01AUFS, and column temperature: 30 ℃, flow velocity: 1.0ml/min, sample size: 10 μ l;
The preparation of contrast solution: it is an amount of that precision takes by weighing the luteolin reference substance, adds methanol and make the solution that every 1ml contains 25 μ g, promptly;
The preparation of need testing solution: get each respectively and extract the about 2g of extract powder that tests under the item, the accurate title, decide, put respectively in the 100ml ground tool plug triangular flask, precision adds methanol 25ml and claims to decide weight, supersound process 30 minutes, put cold, claim again to decide weight, add methanol and supply the weight that subtracts mistake, shake up, filter, get subsequent filtrate as need testing solution;
Linear relationship: it is an amount of that precision takes by weighing the luteolin reference substance, adds methanol and make the solution that every 1ml contains 28.5 μ g, draws this solution 2,5,8,10,12,15 μ l, injects high performance liquid chromatograph, by above-mentioned chromatographic determination luteolin absworption peak area; Every contains Radix Lamiophlomidis Rotatae in luteolin in the soft capsule preparation, must not be less than 0.8000mg.
16, the method for quality control of Duyiwei soft capsule preparation as claimed in claim 15 is characterized in that also comprising in this method following discrimination method:
According to thin layer chromatography:
Get soft capsule content 0.3g, add ethanol 5ml, reflux 10 minutes filters, and gets filtrate 2ml, is concentrated into about 1ml, as need testing solution;
Other gets Radix Lamiophlomidis Rotatae control medicinal material 1g, and the same legal system is shone medical material solution in pairs;
Drawing each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, is that 4: 1 chloroform-methanol is developing solvent with ratio, launches, and takes out, and dries, and spray is with the phosphomolybdic acid test solution, about 15 minutes of 105 ℃ of heating;
In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show the speckle of same color.
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| CN103083395A (en) * | 2012-12-31 | 2013-05-08 | 安徽海神寿春药业有限公司 | Preparation method of lamiophlomis rotate dry extract |
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| CN100450502C (en) * | 2004-09-29 | 2009-01-14 | 广州陈李济药厂 | Active extract of lamtophlomis rotata and its preparing method and use |
| CN102218046B (en) * | 2011-06-14 | 2012-03-14 | 贵州地道药业有限公司 | Chinese patent medicine soft capsule ingredients-mixing technology |
| CN104083572B (en) * | 2014-07-30 | 2017-09-26 | 广州白云山星群(药业)股份有限公司 | Compound iron holly bark soft capsule and preparation method thereof |
| CN104083618B (en) * | 2014-07-30 | 2017-09-05 | 广州白云山星群(药业)股份有限公司 | Qinghouyan soft capsule and preparation method thereof |
| CN106769295A (en) * | 2016-12-08 | 2017-05-31 | 成都中医药大学 | The extracting method and detection method of lamiophlomis rotata polysaccharide |
| CN111494455A (en) * | 2020-03-16 | 2020-08-07 | 中国科学院长春应用化学研究所 | Method for extracting flavonoid compounds in lamiophlomis rotata by response surface method |
| CN111358830A (en) * | 2020-04-15 | 2020-07-03 | 重庆心康制药有限公司 | Lamiophlomis rotata pill and preparation method thereof |
| CN115006362A (en) * | 2022-06-14 | 2022-09-06 | 重庆心康制药有限公司 | Lamiophlomis rotata pill |
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| CN103083395A (en) * | 2012-12-31 | 2013-05-08 | 安徽海神寿春药业有限公司 | Preparation method of lamiophlomis rotate dry extract |
| CN103083395B (en) * | 2012-12-31 | 2015-03-25 | 安徽海神寿春药业有限公司 | Preparation method of lamiophlomis rotate dry extract |
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Effective date of registration: 20170503 Address after: 610041 No. 12, No. 1, building 75, little Tianzhu street, 4, Chengdu, Sichuan, Wuhou District Patentee after: Sichuan Hengkang Development Co.,Ltd. Address before: 610041, 11FA-C, Asia Pacific Plaza, 58 KELONG Road North, Sichuan, Chengdu Patentee before: Chengdu Youta Pharmaceutical Co.,Ltd. |
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Effective date of registration: 20180509 Address after: 746500 Wang Yi Industrial Park, Wang Ba, Kang County, Longnan, Gansu Patentee after: KANGXIAN DUYIWEI BIOLOGICAL PHARMACEUTICAL Co.,Ltd. Address before: 610041 4, 12 Building 1, 75 Tianzhu street, Wuhou District, Chengdu, Sichuan. Patentee before: Sichuan Hengkang Development Co.,Ltd. |
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Denomination of invention: Tibetan medicine Duyiwei soft capsule preparation and its preparation method Effective date of registration: 20210201 Granted publication date: 20060510 Pledgee: Kangxian sub branch of industrial and Commercial Bank of China Ltd. Pledgor: KANGXIAN DUYIWEI BIOLOGICAL PHARMACEUTICAL Co.,Ltd. Registration number: Y2021620000002 |
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Date of cancellation: 20230306 Granted publication date: 20060510 Pledgee: Kangxian sub branch of industrial and Commercial Bank of China Ltd. Pledgor: KANGXIAN DUYIWEI BIOLOGICAL PHARMACEUTICAL Co.,Ltd. Registration number: Y2021620000002 |
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Denomination of invention: Tibetan medicine Duyiwei soft capsule preparation and its preparation method Effective date of registration: 20230614 Granted publication date: 20060510 Pledgee: Kangxian sub branch of industrial and Commercial Bank of China Ltd. Pledgor: KANGXIAN DUYIWEI BIOLOGICAL PHARMACEUTICAL Co.,Ltd. Registration number: Y2023620000016 |
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