CN1194956C - Extraction and purification process of general rhubarb anthraquinone and its application in preparing kidney hypofuction-treating medicine - Google Patents
Extraction and purification process of general rhubarb anthraquinone and its application in preparing kidney hypofuction-treating medicine Download PDFInfo
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- CN1194956C CN1194956C CN 01134161 CN01134161A CN1194956C CN 1194956 C CN1194956 C CN 1194956C CN 01134161 CN01134161 CN 01134161 CN 01134161 A CN01134161 A CN 01134161A CN 1194956 C CN1194956 C CN 1194956C
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Abstract
The present invention relates to an extraction method of rhubarb total anthraquinone, and an application in preparing medicines for treating renal failure. The extraction method comprises the following steps: 1) mixing rhubarb decoction pieces and concentrated ethanol according to weight ratio of 1: 4 to 8, and extracting the mixture for 3 times by using a refluxing method; 2) filtering extraction liquor, recovering ethanol, and making the filter liquor into extractum; 3) adding macroporous adsorptive resin columns into the extractum, using dilute ethanol which is 8 to 16 times as heavy as rhubarb decoction pieces to flush the extractum, and then, removing flushing liquor, and continuously using the concentrated ethanol to flush the extractum; 4) taking out eluant, recovering the ethanol till no ethanol smell exists, and regulating the pH value of eluant to acidity; 5) filtering the eluant, and drying solid matter obtained from precipitation to obtain the products. The medicines for curing renal failure use the rhubarb total anthraquinone as effective ingredients, and the content of the rhubarb total anthraquinone is more than 50%. The extraction of the rhubarb total anthraquinone of the present invention has the advantages of simple process, low cost, and non environment pollution; the extracted rhubarb total anthraquinone has obvious curative effect on renal failure.
Description
Technical field
The present invention relates to a kind of medicine for the treatment of renal failure.
Background technology
Chronic kidney hypofunction is a global problem, and only just there are millions of patients in China, has a strong impact on the raising of the people's Health and Living quality.Keep on a diet clinically at present, patient can't adhere to for a long time that oral angiotensin converting enzyme inhibitor uncertain therapeutic efficacy is cut, therefore a lot of patients are ready to accept hemodialysis and renal transplantation, but,, have only minority can take this treatment for kidney derived deficiency and expense height also because of the need specific installation.
Rheum officinale is a kind of conventional Chinese medicine, and it develops into uremia to the control chronic nephropathy more significantly effect.Through the applicant after deliberation, active substance wherein mainly is a general anthraquinone, but the applicant does not see the report that direct employing general anthraquinone is treated chronic kidney hypofunction as yet at present.
At present, what prior art separated from rheum officinale that general rhubarb anthraquinone generally adopts is with method of extraction such as organic reagent chloroform, ether, and environment is had bigger threat, and productive rate is low, danger is big and cost an arm and a leg.
Summary of the invention
The technical problem to be solved in the present invention is exactly existing conventional treatment means and the unfavorable problem of pharmacological agent renal failure, is the medicine and preparation method thereof of the treatment renal failure of main component with the general rhubarb anthraquinone for people provide a kind of
The present invention is effective ingredient with the general rhubarb anthraquinone, and its content should be greater than 50%, and all the other compositions are that W-Gum, dextrin, carboxy cellulose such as receive at auxiliary material.
Of the present invention is that the preparation method of the medicine of effective ingredient comprises the steps: with the general rhubarb anthraquinone
(1) rhubarb decoction pieces and dense ethanol are pressed 1: the weight ratio of 4-8 is mixed, and extracts three times by circumfluence method;
(2) filter extracting solution, reclaim ethanol, filtrate is made medicinal extract;
(3) medicinal extract being added macroporous adsorptive resins, is rhubarb decoction pieces 8-16 Diluted Alcohol flushing doubly with weight, discards washing fluid, continues to use dense alcohol flushing;
(4) get elutriant, reclaim ethanol and after having the alcohol flavor, elutriant is not transferred to acidity;
(5) filter elutriant, the solid matter drying that precipitation is obtained.
(6) with the solid matter that obtains and technology film-making routinely after auxiliary materials such as W-Gum, dextrin, shuttle Ji Xianweisuna mix.
In the above-mentioned processing step, be 1 hour during refluxing extraction at every turn; When medicinal extract is added macroporous adsorptive resins, preferably macropore absorption resin and medicinal extract are mixed and stirred the back adding, be about to medicinal extract and macropore absorption resin and add macroporous adsorptive resins simultaneously.
Dense concentration of ethanol described in the above-mentioned processing step (1) is 70%-90%, the Diluted Alcohol described in the step 3 be that concentration is 20%-40%, dense concentration of ethanol is 75%-95%.
The pH value of elutriant should transfer to 1-5 described in the above-mentioned processing step (4).
Simple, the with low cost and non-environmental-pollution problem of preparation technology of the present invention, its effective ingredient general rhubarb anthraquinone has tangible curative effect to renal failure.
Below be the effective ingredient general rhubarb anthraquinone main pharmacodynamics experimental data of the present invention that adopts above-mentioned processing step from rheum officinale, to extract:
One, experiment material:
1, medicine and reagent
General rhubarb anthraquinone is pale brown toner end, extracts by above-mentioned technology.Use the distilled water wiring solution-forming before the experiment.
TP, Randox, lot number 0092F.
ALB, Beijing Zhongsheng Biological Engineering High Technology Company, lot number 000502.
URea, Randox, lot number 0104F.
Cr, Pointe, lot number 9360.
2, laboratory animal
Experiment is supplied with conformity certification with SD ♂ rat by Nanjing University of Traditional Chinese Medicine's Experimental Animal Center: Soviet Union's kinoplaszm 97003.
3, laboratory apparatus
Olympus AUT-560 automatic clinical chemistry analyzer, Japan.
DF110 type electronic balance, Changshu City, Jiangsu Province weighing apparatus industry society.
Two, experiment condition
Before and after the administration, the experimental rat sub-cage rearing is fed and is raised complete granular (Jiangpu, Nanjing county institute for drug control laboratory animal feed-processing plant provides), freely drinks water 22 ± 2 ℃ of room temperatures.
Three, experimental result
Table 1 general rhubarb anthraquinone causes influence (the g) (X ± S) of rat CRF body weight to VITAMIN B4
Medication (W)
Before the preceding medication of group modeling
1 2 3 4
Normal control group 236.50 304.00 343.00 353.00 374.00 377.00
±15.88 ±25.18 ±31.00 ±31.71 ±32.38 ±32.72
Model group 241.78 241.92 235.76 227.91 225.91 226.50
±19.51 ±26.20 ±26.15 ±23.31 ±25.65 ±31.46
Dexamethasone group 238.21 244.28 233.92 222.50 222.50 222.00
±19.89 ±17.20 ±16.38 ±17.73 ±36.55 ±52.87
The multiple health group 230.0 250.38 262.31 of kidney
*257.70
*260.42
*264.50
*
±10.74 ±13.65 ±18.14 ±21.36 ±20.35 ±14.04
The total anthracene 237.14 247.08 255.91 237.72 245.45 245.46 of rheum officinale
Quinone I group ± 17.99 ± 22.86 ± 19.52 ± 22.60 ± 23.68 ± 24.72
The total anthracene 236.07 242.14 256.43 232.27 234.09 236.36 of rheum officinale
Quinone II group ± 18.63 ± 26.57 ± 35.52 ± 35.50 ± 36.48 ± 38.02
The total anthracene 247.14 258.93 259.58 237.91 249.54 258.18 of rheum officinale
*
Quinone III group ± 20.32 ± 26.40 ± 26.33 ± 36.54 ± 29.19 ± 30.98
Compare * P＜0.05, * * P＜0.01 with model group.
Compare △ P＜0.05, △ △ P＜0.01 with normal control.
Test-results shows: 70mg.kg
-1The dosage group is behind administration 4w, and body weight obviously increases, and compares significant difference (* * P＜0.01) with model group
Table 2 general rhubarb anthraquinone causes the influence (X ± S) of rat CRF food ration (g/100g) to VITAMIN B4
Medication (w) before the medication before the group modeling
1 2 3 4
Normal control group 12.10 9.70 9.35 8.95 7.60 7.15
±1.50 ±1.50 ±0.65 ±0.10 ±0.30 ±0.25
Model group 11.20 7.20
△6.27
△ △6.45
△ △6.67
△ △6.79
△ △
±1.23 ±1.15 ±0.30 ±0.57 ±0.62 ±0.42
Dexamethasone group 11.96 7.06 5.60
△5.36
*6.93 6.53
±0.94 ±0.60 ±0.51 ±0.65 ±0.71 ±0.70
The multiple health group 11.73 7.00 6.06 6.22 6.53 6.93 of kidney
±0.33 ±0.50 ±0.33 ±0.56 ±0.6?0 ±0.54
The total anthracene 12.66 6.83 6.06 6.50 6.08 7.53 of rheum officinale
Quinone I group ± 0.80 ± 0.45 ± 1.54 ± 1.40 ± 0.45 ± 1.46
The total anthracene 11.83 7.80 6.53 6.46 6.66 6.99 of rheum officinale
Quinone II group ± 0.34 ± 0.86 ± 0.71 ± 0.60 ± 1.10 ± 0.78
The total anthracene 11.36 7.03 6.07 6.13 6.68 7.13 of rheum officinale
Quinone III group ± 0.31 ± 0.47 ± 0.30 ± 0.33 ± 0.81 ± 1.20
Compare * P＜0.05, * * P＜0.01 with model.
Compare △ P＜0.05, △ △ P＜0.01 with normal control.
The rat food ration is compared with the normal control group after the modeling, and obvious reduction is promptly arranged, and a group rat appetite does not have obvious increase after the medication, and difference does not have significance between the model group.
Table 3 general rhubarb anthraquinone causes the influence (X ± S) of CRF rat kidney coefficient to VITAMIN B4
Heavy (g) kidney coefficient (g/100g) of group body weight (g) kidney
Normal control group 377.00 ± 32.72 2.48 ± 0.32 0.66 ± 0.06
Model group 226.50 ± 31.46 6.43 ± 1.89 2.82 ± 0.61
△ △
Dexamethasone group 222.0 ± 52.87 5.02 ± 0.73 2.34 ± 0.43
The multiple health group 264.50 of kidney ± 14.04 5.05 ± 0.67 2.00 ± 0.27
*
General rhubarb anthraquinone I group 245.46 ± 24.72 5.46 ± 1.07 2.22 ± 0.48
*
General rhubarb anthraquinone II group 236.36 ± 38.02 5.22 ± 0.71 2.17 ± 0.33
*
General rhubarb anthraquinone III group 258.18 ± 30.98 5.80 ± 1.01 2.26 ± 0.43
*
Compare * P＜0.05, * * P＜0.01 with model.
Compare △ △ P＜0.01 with normal control.
Test-results shows that 3 dosage group kidney coefficients all obviously lower, and compares significant difference (P＜0.05, P＜0.01) with model group.
Table 4 general rhubarb anthraquinone causes the influence (X=S) of rat CRF serum creatinine, blood urea nitrogen to VITAMIN B4
Group Scr (μ mol/L) Bun (mmol/L)
Medication 15d medication 15d medication 15d medication 15d
Normal control group 39.60 ± 8.74 45.87 ± 12.26 10.28 ± 1.89 10.00 ± 1.03
Model group 205.37 ± 39.76
△ △143.13 ± 30.77
△ △52.60 ± 8.63
△ △29.91 ± 7.78
Dexamethasone group 155.69 ± 27.53
*105.71 ± 15.77
*47.67 ± 12.23 21.81 ± 2.36
*
The multiple health group 145.51 ± 36.14 of kidney
*88.82 ± 21.59
*31.49 ± 10.97
*16.88 ± 3.40
*
General rhubarb anthraquinone I group 200.67 ± 55.75 130.07 ± 26.51 43.03 ± 11.25
*25.00 ± 3.62
General rhubarb anthraquinone II group 165.86 ± 22.51
*113.41 ± 30.26
*39.52 ± 9.77
*21.86 ± 5.22
*
General rhubarb anthraquinone III group 159.93 ± 31.32
*104.40 ± 33.21
*35.04 ± 7.17
*23.48 ± 4.97
*
Compare * P＜0.05, * * P＜0.01 with model.
Compare △ P＜0.05, △ △ P＜0.01 with normal control.
Table 5 general rhubarb anthraquinone causes rat CRF total serum protein, albuminous influence (X ± S) to VITAMIN B4
Group TP (g/L) ALB (g/L)
Medication 15d medication 15d medication 15d medication 15d
Normal control group 87.39 ± 1.83 88.56 ± 4.14 36.92 ± 0.83 37.66 ± 2.38
Model group 74.51 ± 8.83
△ △72.22 ± 5.37
△ △31.80 ± 1.27
△ △32.90 ± 2.88
△ △
Dexamethasone group 77.97 ± 10.53 81.26 ± 3.09
*33.43 ± 1.93
*32.59 ± 2.58
The multiple health group 68.98 of kidney ± 4.61 75.02 ± 2.52 34.09 ± 1.56
*33.23 ± 1.58
General rhubarb anthraquinone I group 79.72 ± 6.80 75.95 ± 4.51 34.58 ± 2.73
*37.68 ± 1.56
*
General rhubarb anthraquinone II group 82.22 ± 6.79
*77.74 ± 5.12
*34.30 ± 2.98
*38.31 ± 2.03
*
General rhubarb anthraquinone III group 81.67 ± 5.80
*78.53 ± 7.49
*32.80 ± 1.27 35.01 ± 2.74
Compare * P＜0.05, * * P＜0.01 with model.
Compare △ P＜0.05, △ △ P＜0.01 with normal control.
After the animal modeling, model group is compared with the normal control group, serum creatinine (Scr), blood urea nitrogen (Bun) has obvious rising, with control group comparing difference remarkable (P＜0.01), total protein (TP) and albumin (HLB) then show as tangible reduction, compare significant difference (P＜0.01) with control group.35.0mg.kg
-1And 70mg.kg
-1After the dosage group connected administration 15d, 30d, serum creatinine and blood urea nitrogen obviously reduced, and compared significant difference (P＜0.05, P＜0.01) with model group; Total serum protein and albumin obviously raise, and compare significant difference (P＜0.05, P＜0.01) with model group.
Table 6 general rhubarb anthraquinone causes rat CRF rat urine amount, uric creatinine and proteic influence (X ± S) to VITAMIN B4
Group urine amount (ml) uric creatinine (mol/L) urine protein (mg/L)
Medication 15d medication 15d medication 15d medication 15d medication 15d medication 15d
Normal control group 8.70 9.40 3979.70 3060.0 768.0
886.40
±2.36 ±2.41 ±1762.8 ±1016.94 ±367.39 ±400.07
Model group 25.10
△ △24.60
△ △1156.90
△ △1129.30
△ △2129.90
△ △2028.80
△ △
±4.96 ±6.02 ±145.81 ±538.37 ±729.02 ±444.60
Dexamethasone group 23.25 21.37
*1672.10 1639.10
*901.0
*1235.20
*
±6.21 ±4.27 ±781.65 ±283.85 ±307.09 ±453.39
The multiple health group 18.30 of kidney
*19.00
*1836.40
*1709.10
*1267.78
*1220.0
*
±5.23 ±3.92 ±378.34 ±361.30 ±331.42 ±610.81
The total anthracene 25.20 28.80 1615.80 of rheum officinale
*1210.10 1460.6
*1222.40
*
Quinone I group ± 7.70 ± 10.93 ± 180.36 ± 266.17 ± 449.04 ± 309.11
The total anthracene 27.40 29.70 1778.50 of rheum officinale
*1360.60 1490.90
*1272.0
*
Quinone II group ± 3.16 ± 10.22 ± 88.70 ± 780.01 ± 305.94 ± 376.06
The total anthracene 30.80 27.10 1858.10 of rheum officinale
*1689.40
*1290.0
*1068.80
*
Quinone III group ± 9.04 ± 6.50 ± 369.68 ± 371.15 ± 417.11 ± 284.94
Compare * P＜0.05, * * P＜0.01 with model.
Compare △ P＜0.05, △ △ P＜0.01 with normal control.
Urine amount showed increased after the animal modeling, the normal control group compares, significant difference (P＜0.01).A dosage group urine amount is compared no considerable change after the medication with model group.After the fast cry of certain animals modeling of gland, the uric creatinine excretion is obvious
Embodiment
Embodiment 1
Get rhubarb decoction pieces 100Kg, adding weight is 70% ethanol of 4 times of rhubarb decoction pieces, refluxing extraction 3 times, and each 1 hour, three times extracting solutions are merged the back filter, decompression filtrate recycling ethanol is got medicinal extract.Macroporous adsorbent resin is about 16 times of rhubarb decoction pieces with weight 20% alcohol flushing pillar will be gone up behind medicinal extract and the macroporous adsorbent resin mix, discard that to continue behind the washing fluid with pH value be 9 75% ethanol elution, elutriant reclaims ethanol to there not being the alcohol flavor, transfer pH value to 1, again elutriant is filtered, precipitates, drying promptly gets pale brown toner powder general rhubarb anthraquinone.
Embodiment 2
Rhubarb decoction pieces consumption and processing step are with embodiment 1, and different is: refluxing extraction adopts is 6 times 80% ethanol; Macroporous adsorbent resin is about 12 times of rhubarb decoction pieces with weight 30% alcohol flushing pillar will be gone up behind medicinal extract and the macroporous adsorbent resin mix; After abandoning washing fluid, with pH value 8 85% ethanol elution.Elutriant reclaims ethanol to nothing alcohol flavor, and its pH value is transferred to 3.
Embodiment 3
Rhubarb decoction pieces consumption and processing step are with embodiment 1, different is: refluxing extraction adopts is 8 times 90% ethanol, macroporous adsorbent resin is about 8 times of rhubarb decoction pieces with weight 40% alcohol flushing pillar will be gone up behind medicinal extract and the macroporous adsorbent resin mix, after abandoning washing fluid, with pH value 7 75% ethanol elution.Elutriant reclaims ethanol to nothing alcohol flavor, and its pH value is transferred to 5.
Below be the relevant concrete data of above-mentioned three embodiment:
Batch dried cream amount of medicinal material amount (kg) (kg) purity (%) assay (Schuttgelb+chrysophanol)
(mg/g)
001 100 3.04 54.5 321.6
002 100 2.92 56.0 341.6
003 100 3.01 54.3 350.0
The general rhubarb anthraquinone that the foregoing description is made and W-Gum, dextrin, carboxy cellulose receive etc. auxiliary material mix after routinely technology can make patent medicine, generally be to make tablet.The content of its general rhubarb anthraquinone should be greater than 50% (weight ratio), and W-Gum, dextrin, carboxy cellulose the concrete content of auxiliary material such as are received and can be depended on actual need and decide in the patent medicine.
Claims (4)
1, a kind of medicine for the treatment of renal failure is characterized in that it is effective ingredient with the general rhubarb anthraquinone, and its content should be greater than 50%, and all the other compositions are conventional auxiliary material, and its preparation method comprises the steps:
(1) with rhubarb decoction pieces and concentration be the dense ethanol of 70%-90% by 1: the weight ratio of 4-8 is mixed, and extracts three times each 1 hour by circumfluence method;
(2) filter extracting solution, reclaim ethanol, filtrate is made medicinal extract;
(3) medicinal extract being added macroporous adsorptive resins, is that rhubarb decoction pieces 8-16 concentration doubly is the Diluted Alcohol flushing of 20%-40% with weight, discards washing fluid, and continuing with concentration is the dense alcohol flushing of 75%-95%;
(4) get elutriant, the pH value with elutriant after recovery ethanol to nothing alcohol is distinguished the flavor of transfers to acidity;
(5) filter elutriant, the solid matter drying with precipitation obtains promptly gets general rhubarb anthraquinone;
(6) with dried general rhubarb anthraquinone and technology film-making routinely after auxiliary material mixes, promptly get tablet patent medicine.
2, the virtuous medicine that declines of treatment as claimed in claim 1 is characterized in that described conventional auxiliary material is that W-Gum, dextrin, carboxy cellulose are received.
3, the medicine of treatment renal failure as claimed in claim 1 or 2 when it is characterized in that in the step (3) in manufacturing processed that medicinal extract added macroporous adsorptive resins, adds macropore absorption resin simultaneously.
4, the medicine of treatment renal failure as claimed in claim 1 or 2 is characterized in that the pH value of elutriant described in step poly-(4) of manufacturing processed should transfer to 1-5.
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| CN 01134161 CN1194956C (en) | 2001-11-09 | 2001-11-09 | Extraction and purification process of general rhubarb anthraquinone and its application in preparing kidney hypofuction-treating medicine |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR100915961B1 (en) * | 2009-02-23 | 2009-09-10 | 김태진 | Patch for treating constipation using crude drugs and method for treating constipation using its patch |
| CN103288889B (en) * | 2013-02-22 | 2016-04-06 | 中国科学院昆明植物研究所 | Anthraquinone derivative and pharmaceutical composition thereof and its application in pharmacy |
| CN104224951A (en) * | 2014-09-28 | 2014-12-24 | 江西百神药业股份有限公司 | Total anthraquinones with stable and uniform proportions of various components and composition of total anthraquinones for treating cholecystitis |
| CN104224952A (en) * | 2014-09-28 | 2014-12-24 | 江西百神昌诺药业有限公司 | Preparation method for total anthraquinones of rheum officinale with stable and uniform proportions of all components |
| CN104224953A (en) * | 2014-09-28 | 2014-12-24 | 江西百神昌诺药业有限公司 | Total anthraquinones with stable and uniform proportions of various components and composition of total anthraquinones for treating chronic renal failure |
| CN104909999B (en) * | 2015-04-16 | 2016-07-20 | 聊城大学 | A kind of isolated and purified anthraquinone analog compound and method of styrene acid from Radix Et Rhizoma Rhei |
| CN107216228B (en) * | 2017-04-14 | 2021-06-01 | 四川农业大学 | Eutectic solvent and method for extracting anthraquinone in rheum officinale |
| CN107412356A (en) * | 2017-05-10 | 2017-12-01 | 湘潭大学 | A kind of method of the extraction purification general anthraquinone from rheum officinale |
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