CN101148441A - Andrographolidi natrii bisulfis and preparation method thereof - Google Patents
Andrographolidi natrii bisulfis and preparation method thereof Download PDFInfo
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- CN101148441A CN101148441A CNA200710110975XA CN200710110975A CN101148441A CN 101148441 A CN101148441 A CN 101148441A CN A200710110975X A CNA200710110975X A CN A200710110975XA CN 200710110975 A CN200710110975 A CN 200710110975A CN 101148441 A CN101148441 A CN 101148441A
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- Prior art keywords
- stirring
- natrii bisulfis
- rographolide
- sodium bisulfite
- preparation
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Links
- 238000002360 preparation method Methods 0.000 title claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 33
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 claims abstract description 9
- 235000010267 sodium hydrogen sulphite Nutrition 0.000 claims abstract description 9
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000010992 reflux Methods 0.000 claims abstract description 7
- 238000001291 vacuum drying Methods 0.000 claims abstract description 7
- 239000012065 filter cake Substances 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims description 22
- 238000000605 extraction Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- JXAZAUKOWVKTLO-UHFFFAOYSA-L sodium pyrosulfate Chemical compound [Na+].[Na+].[O-]S(=O)(=O)OS([O-])(=O)=O JXAZAUKOWVKTLO-UHFFFAOYSA-L 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000000796 flavoring agent Substances 0.000 claims description 6
- 235000019634 flavors Nutrition 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 5
- 230000008025 crystallization Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000010791 quenching Methods 0.000 claims description 5
- 238000000967 suction filtration Methods 0.000 claims description 5
- 230000000694 effects Effects 0.000 abstract description 5
- 238000010438 heat treatment Methods 0.000 abstract description 2
- BOJKULTULYSRAS-OTESTREVSA-N Andrographolide Chemical compound C([C@H]1[C@]2(C)CC[C@@H](O)[C@]([C@H]2CCC1=C)(CO)C)\C=C1/[C@H](O)COC1=O BOJKULTULYSRAS-OTESTREVSA-N 0.000 abstract 4
- ASLUCFFROXVMFL-UHFFFAOYSA-N andrographolide Natural products CC1(CO)C(O)CCC2(C)C(CC=C3/C(O)OCC3=O)C(=C)CCC12 ASLUCFFROXVMFL-UHFFFAOYSA-N 0.000 abstract 4
- 150000001875 compounds Chemical class 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 102000011759 adducin Human genes 0.000 description 5
- 108010076723 adducin Proteins 0.000 description 5
- 238000004587 chromatography analysis Methods 0.000 description 5
- 239000007791 liquid phase Substances 0.000 description 5
- 230000014759 maintenance of location Effects 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000003115 biocidal effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000011084 recovery Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 241000746375 Andrographis Species 0.000 description 1
- 208000004429 Bacillary Dysentery Diseases 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-M Bisulfite Chemical compound OS([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-M 0.000 description 1
- 208000005577 Gastroenteritis Diseases 0.000 description 1
- 206010017915 Gastroenteritis shigella Diseases 0.000 description 1
- 201000008197 Laryngitis Diseases 0.000 description 1
- 206010034038 Parotitis Diseases 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 206010057190 Respiratory tract infections Diseases 0.000 description 1
- 206010046306 Upper respiratory tract infection Diseases 0.000 description 1
- 239000008186 active pharmaceutical agent Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 239000002260 anti-inflammatory agent Substances 0.000 description 1
- 229940124599 anti-inflammatory drug Drugs 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 201000001352 cholecystitis Diseases 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 238000010606 normalization Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 201000005113 shigellosis Diseases 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 206010044008 tonsillitis Diseases 0.000 description 1
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Abstract
The present invention provides one kind of sodium bisulfite andrographolide, which is prepared through adding water solution of sodium bisulfite into alcohol solution of andrographolide, heating to reflux, recovering alcohol, cooling, extracting with chloroform for several times, filtering, vacuum concentrating the filtrate, crystallizing the concentrated solution, suction filtering, and vacuum drying the filter cake to obtain the white sodium bisulfite andrographolide addition compound. The sodium bisulfite andrographolide product has high purity, high stability, high curative effect and wide use.
Description
Technical field
The present invention relates to a kind of pharmacy field, specifically, relate to a kind of antibiosis anti-inflammatory drug rographolidum Natrii Bisulfis and preparation method thereof.
Background technology
Rographolidum Natrii Bisulfis (being Lian Bizhi again) is the active pharmaceutical ingredients that extracts from Chinese medicine Herba Andrographis a kind of---rographolide and bisulfite are received the water-soluble sulfonate that makes after the addition.Pharmacological research and clinical application show to have effects such as antibiotic, antiviral, and clinical have better curative effect to bacillary dysentery, parotitis, laryngitis, tonsillitis, gastro-enteritis, pneumonia, cholecystitis and upper respiratory tract infection etc., is described as the natural antibiotics medicine.
At present, the concrete technology of rographolidum Natrii Bisulfis production is: 1) get rographolide 100g, add 95% ethanol 1500ml heating for dissolving; 2) get the Na of 1mol/L
2SO
4400ml adds 2%H
2SO
4480ml mixes, and adds water to 800ml; 3) pour rographolide solution into step 2) solution in, shake up, reflux added 2%H after 30 minutes
2SO
4Making PH is 6-7, and recovery ethanol is used equal-volume chloroform extraction 3 times to there not being the alcohol flavor, divides water-yielding stratum, and steams water to small volume.Add pure 1000ml, dissolving is also filtered, and filtrate decompression recovery alcohol is to doing, and vacuum-drying gets white affixture.But the Lian Bizhi transfusion of this method preparation is unstable in storage, prevent for some time after pH value have obvious decline, thereby affect the treatment.For this reason, many researchs had once been carried out in this area.For example, application number is 200310111332 and two China's patent application of application number 200310112722, has almost proposed simultaneously by Lian Bizhi is made freeze-dried powder, thereby has solved the problem of preparation stability.
But, though freeze-dried powder is convenient to preservation, improved cost aborning, also increased the difficulty of operation clinically.
Summary of the invention
In view of the problem that background technology exists, one of purpose of the present invention provides that a kind of impurity is few, purity is high, good stability, the preparation method of the rographolidum Natrii Bisulfis that does not lessen the curative effect again.
The present invention has adopted following technical scheme:
A kind of preparation method of rographolidum Natrii Bisulfis may further comprise the steps:
1) get rographolide Akg, 6≤A≤12, preferred 8≤A≤10, more preferably A=10, and add 95% ethanol 120-165L heated and stirred dissolving, and remain on 70～85 ℃;
2) get sodium bisulfite BKg, 2.2≤B≤3.2, preferred B=2.5 adds water to 73L～86L, stirring and dissolving;
3) pour the rographolide ethanolic soln of step 1) into step 2) the sodium pyrosulfate aqueous solution in, uniform mixing also is heated to 65～85 ℃; After refluxing then 23～36 minutes, reclaim ethanol, place 1 ℃～9 ℃ freezer to refrigerate 12～48 hours, and repeatedly with an amount of chloroform extraction until there not being the alcohol flavor, preferred 4 times, after the filtration with the filtrate vacuum concentration;
4) concentrated solution with step 3) places crystallizing pan, adopts the chuck water quench, stirs and leave standstill crystallization under 3 ℃～19 ℃, and suction filtration with filter cake vacuum-drying, gets white rographolidum Natrii Bisulfis affixture again.
Wherein, the crystallizing pan in the step 4) has stirring arm, and wherein said stirring is that stirring arm stirs.
The preparation method of rographolidum Natrii Bisulfis of the present invention, compare with traditional technology, have following technique effect: prepared rographolidum Natrii Bisulfis impurity is few, purity is high, good stability, specifically, the rographolidum Natrii Bisulfis purity of the present invention's preparation is more than 99.5%, and the rographolidum Natrii Bisulfis purity of former technology manufacturing only is below 90%.
Description of drawings
Fig. 1 has shown the color atlas of the rographolidum Natrii Bisulfis that adopts original technology preparation.
Fig. 2 has shown the color atlas of the rographolidum Natrii Bisulfis that one of embodiments of the invention are made.
Embodiment
Below in conjunction with embodiment the present invention is further described, so that to the understanding in more detail of the present invention's do.The following stated only is in order to explain the preferred embodiments of the present invention, is not according to this present invention to be done any pro forma restriction, so every any form of being done on creation spirit of the present invention basis is modified or change, all should belong to protection category of the present invention.
Embodiment 1
Take by weighing rographolide 6kg, and add 95% ethanol 120L, the heated and stirred dissolving, and remain on 70 ℃; Get sodium bisulfite 2.2Kg then, add water to 73L, stirring and dissolving; Pour the rographolide ethanolic soln of step 1) into step 2) the sodium pyrosulfate aqueous solution in, uniform mixing also is heated to 70 ℃; After refluxing then 36 minutes, reclaim ethanol, place 1 ℃～9 ℃ freezer to refrigerate 12～48 hours, and with an amount of chloroform extraction 3 times until there not being the alcohol flavor, after the filtration with the filtrate vacuum concentration; The concentrated solution of step 3) has been placed the stirring arm crystallizing pan, adopted the chuck water quench, stirred and leave standstill crystallization at 3 ℃～19 ℃ following stirring arms, suction filtration with filter cake vacuum-drying, promptly gets white rographolidum Natrii Bisulfis affixture again.Its purity is 99.6% to adopt liquid phase chromatography to measure as can be known.
Take by weighing rographolide 10kg, and add 95% ethanol 145L, the heated and stirred dissolving, and remain on 80 ℃; Get sodium bisulfite 2.5Kg then, add water to 80L, stirring and dissolving; Pour the rographolide ethanolic soln of step 1) into step 2) the sodium pyrosulfate aqueous solution in, uniform mixing also is heated to 85 ℃; After refluxing then 30 minutes, reclaim ethanol, place 1 ℃～9 ℃ freezer to refrigerate 12～48 hours, and with an amount of chloroform extraction 4 times until there not being the alcohol flavor, after the filtration with the filtrate vacuum concentration; The concentrated solution of step 3) has been placed the stirring arm crystallizing pan, adopted the chuck water quench, stirred and leave standstill crystallization at 3 ℃～19 ℃ following stirring arms, suction filtration with filter cake vacuum-drying, gets white rographolidum Natrii Bisulfis affixture again.Its purity is 99.8% to adopt liquid phase chromatography to measure as can be known.
Take by weighing rographolide 12kg, and add 95% ethanol 165L, the heated and stirred dissolving, and remain on 85 ℃; Get sodium bisulfite 3.2Kg then, add water to 86L, stirring and dissolving; Pour the rographolide ethanolic soln of step 1) into step 2) the sodium pyrosulfate aqueous solution in, uniform mixing also is heated to 65 ℃; After refluxing then 36 minutes, reclaim ethanol, place 1 ℃～9 ℃ freezer to refrigerate 12～48 hours, and with an amount of chloroform extraction 4 times until there not being the alcohol flavor, after the filtration with the filtrate vacuum concentration; The concentrated solution of step 3) has been placed the stirring arm crystallizing pan, adopt the chuck water quench, stir and leave standstill crystallization at 3 ℃～19 ℃ following stirring arms, suction filtration again, with filter cake vacuum-drying, get white rographolidum Natrii Bisulfis affixture, its purity was 99.74% (as shown in Figure 2) to adopt liquid phase chromatography to measure as can be known.
By liquid phase chromatography the color atlas of the white rographolidum Natrii Bisulfis of acquisition is tested, test condition is as follows:
Use the instrument type: liquid phase chromatography; Gradient mode: constant current;
Integrative approach: area normalization method; Instrument model: LC-10ATVP;
Detector: ultraviolet; Wavelength: 220nm; Column temperature: 30 ℃;
Post model: Shimpack-VPODS.
Fig. 1 is the color atlas that adopts the rographolidum Natrii Bisulfis of original technology preparation, and its correspondence analysis the results are shown in the table 1.Fig. 2 is the color atlas of the rographolidum Natrii Bisulfis of embodiments of the invention 3 manufacturings, and its correspondence analysis the results are shown in the table 2.By contrasting both as can be known, the highest 77.43% (the retention time) that only are about of rographolidum Natrii Bisulfis purity of reason technology preparation corresponding to 12.915; And the purity of the rographolidum Natrii Bisulfis of the inventive method one embodiment preparation is up to 99.74% (corresponding to identical approximately retention time 12.865).
Table 1 is corresponding to the analytical results of the color atlas of the prepared sodium pyrosulfate rographolide of original technology
The analytical results table
| Peak number | The peak name | Retention time | Peak height | Peak area | Content |
| 1 2 3 4 5 6 7 3 9 10 11 12 13 | 3.298 3.823 4.023 4.973 5.382 5.848 6.465 7.348 9.365 10.815 12.915 15.915 17.648 | 494.067 495.111 997.244 302.333 981.211 471.07 418.456 151.327 125.623 343.145 55485.449 11715.754 188.507 | 7671.100 6711.600 12274.900 3722.061 11919.555 6892.792 6835.531 2392.600 4188.246 7473.151 1562921.625 378540.406 7015.553 | 0.3800 0.3325 0.6081 0.1844 0.5905 0.3415 0.3386 0.1185 0.2075 0.3702 77.4276 18.7530 0.3476 | |
| Amount to | 72169.298 | 2018559.120 | 100.0000 |
Table 2 is corresponding to the analytical results of the color atlas of the prepared sodium pyrosulfate rographolide of embodiments of the invention 3
The analytical results table
| Peak number | The peak name | Retention time | Peak height | Peak area | Content |
| 1 2 | 5.340 12.865 | 382.000 66966.125 | 5205.500 1990887.000 | 0.2608 99.7392 | |
| Amount to | 67348.125 | 1996092.500 | 100.0000 |
Claims (6)
1. the preparation method of a rographolidum Natrii Bisulfis may further comprise the steps:
1) get rographolide Akg, 6≤A≤12, and add the dissolving of 95% ethanol 120-165L heated and stirred, and remain on 70～85 ℃;
2) get sodium bisulfite BKg, 2.2≤B≤3.2 add water to 73L～86L, stirring and dissolving;
3) pour the rographolide ethanolic soln of step 1) into step 2) the sodium pyrosulfate aqueous solution in, uniform mixing also is heated to 65～85 ℃; After refluxing then 23～36 minutes, reclaim ethanol, place 1 ℃～9 ℃ freezer to refrigerate 12～48 hours, and repeatedly with an amount of chloroform extraction until there not being the alcohol flavor, after the filtration with the filtrate vacuum concentration;
4) concentrated solution with step 3) places crystallizing pan, adopts the chuck water quench, stirs and leave standstill crystallization under 8 ℃～19 ℃, and suction filtration with filter cake vacuum-drying, gets white rographolidum Natrii Bisulfis again.
2. the method for claim 1 is characterized in that, the A in the step 1) is 8≤A≤10.
3. method as claimed in claim 2 is characterized in that the A in the step 1) equals 10.
4. as each described method of claim 1-3, it is characterized in that B=2.5.
5. as each described method of claim 1-3, it is characterized in that the chloroform extraction in the step 3) repeatedly is extraction 4 times.
6. as each described method of claim 1-3, it is characterized in that the crystallizing pan described in the step 4) has stirring arm, and wherein said stirring is that stirring arm stirs.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710110975A CN100577655C (en) | 2007-06-12 | 2007-06-12 | Andrographolidi natrii bisulfis and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710110975A CN100577655C (en) | 2007-06-12 | 2007-06-12 | Andrographolidi natrii bisulfis and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101148441A true CN101148441A (en) | 2008-03-26 |
| CN100577655C CN100577655C (en) | 2010-01-06 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507771A (en) * | 2011-10-26 | 2012-06-20 | 无锡济民可信山禾药业股份有限公司 | Novel content detection method for sodium hydrogensulfite andrographolide |
| CN106770774A (en) * | 2016-12-28 | 2017-05-31 | 李宏 | A kind of measuring method of LIANBIZHI ZHUSHEYE |
| CN108853026A (en) * | 2018-08-21 | 2018-11-23 | 无锡正大生物股份有限公司 | A kind of andrographolide for animals is scattered |
| CN110559289A (en) * | 2019-08-09 | 2019-12-13 | 中国中医科学院广安门医院 | Application of andrographolide sodium bisulfite in preparing accelerant for promoting reverse cholesterol transport |
| CN111635383A (en) * | 2020-07-07 | 2020-09-08 | 郑州大学 | Single crystal of 14-dehydroxy-13-dehydroandrographolide-12-calcium sulfonate acetone solvate and preparation method thereof |
| CN113861141A (en) * | 2020-06-30 | 2021-12-31 | 江西青峰药业有限公司 | Preparation method of andrographolide sulfonate for controlling anaphylactic reaction of Chinese medicinal injection |
-
2007
- 2007-06-12 CN CN200710110975A patent/CN100577655C/en active Active
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102507771A (en) * | 2011-10-26 | 2012-06-20 | 无锡济民可信山禾药业股份有限公司 | Novel content detection method for sodium hydrogensulfite andrographolide |
| CN102507771B (en) * | 2011-10-26 | 2016-07-06 | 无锡济民可信山禾药业股份有限公司 | A kind of detection method of content of new andrographolidum Natrii Bisulfis |
| CN106770774A (en) * | 2016-12-28 | 2017-05-31 | 李宏 | A kind of measuring method of LIANBIZHI ZHUSHEYE |
| CN108853026A (en) * | 2018-08-21 | 2018-11-23 | 无锡正大生物股份有限公司 | A kind of andrographolide for animals is scattered |
| CN110559289A (en) * | 2019-08-09 | 2019-12-13 | 中国中医科学院广安门医院 | Application of andrographolide sodium bisulfite in preparing accelerant for promoting reverse cholesterol transport |
| CN113861141A (en) * | 2020-06-30 | 2021-12-31 | 江西青峰药业有限公司 | Preparation method of andrographolide sulfonate for controlling anaphylactic reaction of Chinese medicinal injection |
| CN113861141B (en) * | 2020-06-30 | 2024-03-19 | 江西青峰药业有限公司 | Preparation method of andrographolide sulfonate for controlling anaphylactic reaction of traditional Chinese medicine injection |
| CN111635383A (en) * | 2020-07-07 | 2020-09-08 | 郑州大学 | Single crystal of 14-dehydroxy-13-dehydroandrographolide-12-calcium sulfonate acetone solvate and preparation method thereof |
| CN111635383B (en) * | 2020-07-07 | 2023-01-24 | 郑州大学 | Single crystal of 14-dehydroxy-13-dehydroandrographolide-12-calcium sulfonate acetone solvate and preparation method thereof |
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| Publication number | Publication date |
|---|---|
| CN100577655C (en) | 2010-01-06 |
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