CN102274299B - Method for preparing raw medicinal material for improving combined anthraquinone in rhubarb decoction pieces - Google Patents
Method for preparing raw medicinal material for improving combined anthraquinone in rhubarb decoction pieces Download PDFInfo
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- CN102274299B CN102274299B CN 201110267135 CN201110267135A CN102274299B CN 102274299 B CN102274299 B CN 102274299B CN 201110267135 CN201110267135 CN 201110267135 CN 201110267135 A CN201110267135 A CN 201110267135A CN 102274299 B CN102274299 B CN 102274299B
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- rhizoma rhei
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Abstract
The invention discloses a method for preparing a raw medicinal material for improving combined anthraquinone in rhubarb decoction pieces, and belongs to the processing of the conventional Chinese medicinal materials. The method comprises the following steps of: removing impurities from a rhubarb raw medicinal material, sorting, putting into a container, steaming for 2 to 6 hours, taking the raw medicinal material out, slicing, and drying to prepare the rhubarb decoction pieces. By the prepared rhubarb decoction pieces, the influence on the active ingredients and a purgative effect of rhubarb is small, the content of the combined anthraquinone also can be improved, so that the combined anthraquinone is improved to over 90 percent of the raw medicinal material and is improved by more than 3 times compared with the decoction pieces prepared by the conventional process. Therefore, the extraction rate of the active ingredients in rhubarb extract is improved, a medicinal effect is played to a maximum degree, a clinical curative effect is improved, and Chinese medicinal resources are saved. The processing time before cutting is shortened, and the rhubarb decoction pieces are convenient to cut and store, so the cost is reduced; and the prepared rhubarb decoction pieces do not contain sulphur, the addition of poisonous ingredients is avoided, so the method is suitable for large-scale production and has great economic and social benefits.
Description
Technical field
The present invention relates to the Preparation process of Chinese medicine material, specifically a kind of crude drug preparation method that improves combined anthraquinone in the Radix Et Rhizoma Rhei decoction piece.
Background technology
" Pharmacopoeia of People's Republic of China (one one) " version in 2010. Chinese Pharmacopoeia Commission, Chinese Medicine publishing house, 2010:22～23.Radix Et Rhizoma Rhei is the dry root and rhizome of polygonum rheum palmatum Rheum palmatum L., Rheum tanguticum Rheum tanguticum Maxim. ex Balf. or Rheum officinale Rheum officinale Baill..Effect is rushed down lower attack, clearing away heat-fire, removing pathogenic heat from blood and toxic substance from the body, eliminating blood stasis and inducing menstruation, dampness removing jaundice eliminating.Be used for the stagnant constipation of excess-heat, heat in blood is told nosebleed, the conjunctival congestion pharyngeal swelling, and the carbuncle furuncle, abdominalgia with intestinal abscess, blood stasis amenorrhea etc. are traditional Chinese medical science parts of generic medicinal plants.Modern study proves, it mainly contains the compositions such as anthraquinone derivatives (comprising chrysophanol, chrysophanic acid, emodin, aloe-emodin, physcione and glycosides thereof), tannin, wherein combined anthraquinone is for mainly rushing down lower effective ingredient, and combined anthraquinone accounts for 96.3% of general anthraquinone in the Radix Et Rhizoma Rhei crude drug in whole.
The process of preparing Chinese medicine kind of using Radix Et Rhizoma Rhei till today mainly contains Radix Et Rhizoma Rhei, Radix et Rhizoma Rhei (stir-fried with wine), Radix Et Rhizoma Rhei, charred Radix Et Rhizoma Rhei.Wherein Radix et Rhizoma Rhei (stir-fried with wine) is to get clean rhubarb tablets, adds yellow wine and mixes thoroughly, and is vexed, puts in the parch container, fries to the degree of regulation with slow fire.Radix Et Rhizoma Rhei is to get clean Radix Et Rhizoma Rhei piece, adds yellow wine and mixes thoroughly, and is vexed, puts suitable steaming in the container, water proof or steam or stew to adjuvant with Steam Heating and exhausted section, drying.Because it is deep that Radix Et Rhizoma Rhei is given birth to abnormal smells from the patient, walk and do not keep, the through part of the body cavity below the umbilicus, housing the bladder, kidneys and bowels, discharge function is high strong, the gas that easily injures one's stomach, parch (Radix et Rhizoma Rhei (stir-fried with wine), charred Radix Et Rhizoma Rhei), steam (Radix Et Rhizoma Rhei) after discharge function relax, increased the effect of invigorating blood circulation.Just put down in writing in the Lei Gong's Treatise on Preparation and Broiling of Materia Medica and steamed medicine kind more than 70, wherein steaming Radix Et Rhizoma Rhei namely is that above-mentioned wine steams Radix Et Rhizoma Rhei, and namely Radix Et Rhizoma Rhei has changed the property of medicine, has expanded scope of medication.
At present, be used for processing Chinese patent medicine and clinical use take the Radix Et Rhizoma Rhei decoction pieces as main, always the concocting method of Radix Et Rhizoma Rhei is take moistening method as main.
" national Chinese medicine processing standard " 1988 editions. People's Health Publisher, the 6th page.The Radix Et Rhizoma Rhei crude drug, removal impurity, size is respectively separated, and slightly profit is pulled out, drenches when moistening extremely thoroughly, cuts sheet or fritter, dries or cold drying.
At present, the universal method that the Radix Et Rhizoma Rhei decoction piece that circulates on the market is concocted is: Radix Et Rhizoma Rhei crude drug size is respectively separated, add and soaked in the tank approximately 6 ~ 10 hours, time in winter can prolong, and then covers the Polypropylence Sheet moistening 12 ~ 24 hours, adds sulfur fumigation at least 24 hours again, section is dried or is dried.
Be the method for generally using at present with sulfur fumigation, relate to a lot of medical material kinds commonly used.Because the medical material color that sulfur was smoked is good-looking, medical material is not clamminess, and is beneficial to section; Insect protected is convenient to preserve, and present medicinal herb grower adds sulfur more or less, and addition causes residual sulphur compound in the Radix Et Rhizoma Rhei decoction piece only by rule of thumb.
Although the steaming method is widely used in a lot of Chinese medicines as a kind of traditional concocting method,, people generally believe that Radix Et Rhizoma Rhei steams can affect its effective ingredient and discharge function thereof after being heated, and is continuing the concocting method of traditional " profit " always.
According to the method described above, with with a collection of medical material, the laboratory test of carrying out, and carry out pilot scale processing in the former building site that adds, wherein combined anthraquinone all only accounts for about 30% of crude drug in the Radix Et Rhizoma Rhei decoction piece after the processing, shows that combined anthraquinone runs off or has been converted into the sequestered anthraquinone in concocting process.
Summary of the invention
The present invention is exactly in order to have solved the Radix Et Rhizoma Rhei crude drug in concocting into the decoction pieces process, the problem of effective ingredient hydrolysis, and the crude drug preparation method of combined anthraquinone in the raising Radix Et Rhizoma Rhei decoction piece that a kind of better preservation rushes down lower composition is provided.
The present invention realizes by following technical scheme.
A kind of crude drug preparation method that improves combined anthraquinone in the Radix Et Rhizoma Rhei decoction piece, it is that the Radix Et Rhizoma Rhei crude drug is removed impurity, the size sorting is put in the container, and steamed 2-6 hour, take out, section, drying makes Radix Et Rhizoma Rhei decoction piece.
The crude drug preparation method of combined anthraquinone in the described raising Radix Et Rhizoma Rhei decoction piece, the drying of section was to ventilate to drying after it was steamed, or the 50-70 ℃ of interior cold drying of baking oven.
Steamed in the crude drug preparation method of combined anthraquinone in the described raising Radix Et Rhizoma Rhei decoction piece, its container is Steam by water bath in airtight steamer, or leads to vapours in vapor tight tank.
The crude drug preparation method of combined anthraquinone in the described raising Radix Et Rhizoma Rhei decoction piece, combined anthraquinone content is not less than 90% of crude drug in its Radix Et Rhizoma Rhei decoction piece that makes.
The Radix Et Rhizoma Rhei decoction piece for preparing like this, not only very little on effective ingredient and the discharge function impact thereof of Radix Et Rhizoma Rhei, can also improve the content of combined anthraquinone in the Radix Et Rhizoma Rhei decoction piece, wherein combined anthraquinone is brought up to more than 90% of crude drug in the Radix Et Rhizoma Rhei decoction piece, and the decoction pieces for preparing than traditional handicraft has improved more than 3 times.Thereby the extraction ratio of effective ingredient in the raising Radix Et Rhizoma Rhei extract is brought into play drug effect to greatest extent, improves clinical efficacy, the saving Chinese medicaments resource.And greatly shorten the process time before the cutting, shorten drying time, accelerate turnover, save cost; The Radix Et Rhizoma Rhei that the present invention steams need not to add sulfur, has avoided the adding of toxic component, is convenient to cutting, is convenient to preserve; Suitable large production has huge economic benefit and social benefit.
Description of drawings
Fig. 1 is aloe-emodin, chrysophanic acid, chrysophanol, emodin, physcione standard substance collection of illustrative plates;
Fig. 2 is Radix Et Rhizoma Rhei crude drug (individual sub-goods) general anthraquinone collection of illustrative plates;
Fig. 3 is Radix Et Rhizoma Rhei crude drug (individual sub-goods) sequestered anthraquinone collection of illustrative plates;
Fig. 4 is the general anthraquinone collection of illustrative plates of decoction pieces of the present invention;
Fig. 5 is the sequestered anthraquinone collection of illustrative plates of decoction pieces of the present invention;
Fig. 6 is the general anthraquinone collection of illustrative plates that tradition is concocted decoction pieces;
Fig. 7 is the sequestered anthraquinone collection of illustrative plates that tradition is concocted decoction pieces;
Fig. 8 is decoction pieces aqueous extract general anthraquinone collection of illustrative plates of the present invention;
Fig. 9 is decoction pieces aqueous extract combined anthraquinone collection of illustrative plates of the present invention;
Figure 10 is that tradition is concocted decoction pieces aqueous extract general anthraquinone collection of illustrative plates;
Figure 11 is that tradition is concocted decoction pieces aqueous extract combined anthraquinone collection of illustrative plates.
The specific embodiment
The present invention is described in detail below in conjunction with drawings and Examples.
One. preparation method
Embodiment 1:
Take by weighing Radix Et Rhizoma Rhei crude drug 1kg, remove impurity, select evenly stature of size, put in the airtight steamer, add water 3000ml, Steam by water bath 2 hours takes out, and cuts into slices or fritter, and ventilation is dried, and makes Radix Et Rhizoma Rhei decoction piece.
Embodiment 2:
Take by weighing Radix Et Rhizoma Rhei crude drug 2kg, remove impurity, select evenly stature of size, put in the airtight steamer, add water 4000ml, Steam by water bath 6 hours takes out, and cuts sheet or fritter, and ventilation is dried, and makes Radix Et Rhizoma Rhei decoction piece.
Embodiment 3:
Take by weighing Radix Et Rhizoma Rhei crude drug 1kg, remove impurity, select evenly stature of size, place in the band blow vent vapor tight tank, passed into vapours 2 hours from blow vent, take out, cut sheet or fritter, put cold drying in the 50-70 ℃ of baking oven, make Radix Et Rhizoma Rhei decoction piece.
Two. detection method
1. chromatographic condition: be filler with octadecylsilane chemically bonded silica, methanol-1% perchloric acid (85:15) is mobile phase; Detect wavelength 254nm.Number of theoretical plate is pressed aloe-emodin, chrysophanic acid, emodin, chrysophanol, the calculating of physcione peak, should all be not less than 2000.
2. the preparation of reference substance solution: get aloe-emodin, chrysophanic acid, emodin, chrysophanol, physcione reference substance an amount of, accurately weighed, add respectively the acetonitrile dissolving, shake up, make the solution that every 1ml contains aloe-emodin, chrysophanic acid, emodin, chrysophanol, physcione 0.25mg.Precision measures above-mentioned aloe-emodin solution 2.0ml, chrysophanic acid solution 2.0ml, emodin solution 2.0ml, chrysophanol solution 5.0ml, physcione solution 1.5ml, puts in the 25ml volumetric flask, adds methanol and is diluted to scale, shakes up, and gets the mixing reference substance solution.
3. the sequestered anthraquinone content is measured: get Radix Et Rhizoma Rhei crude drug fine powder 0.1g, and accurately weighed, place the 100ml round-bottomed flask, add chloroform 40ml, water-bath (80 ℃) refluxed 30 minutes, put to room temperature, careful sucking-off chloroform solution, second and third time adds chloroform 20ml, refluxes 20 minutes at every turn, the careful supernatant of drawing, colourless to supernatant, combined chloroform liquid, filter, reclaim solvent to doing, with the dissolve with methanol residue in the 5ml volumetric flask and be diluted to scale, shake up, cross 0.45 μ m microporous filter membrane, and get final product.
4. Assay of Total Anthraquinone method: get Radix Et Rhizoma Rhei crude drug fine powder 0.06g, accurately weighed; Or the accurate Radix Et Rhizoma Rhei extract that is equivalent to the 0.06g crude drug of drawing, decompression volatilizes solvent, places the 100ml round-bottomed flask, add 20% sulphuric acid 5.0ml, room temperature jolting 5 minutes adds chloroform 40ml again, water-bath (80 ℃) back hydrolysis 120 minutes, put to room temperature, the sucking-off chloroform layer adds later on chloroform 20ml repeatedly, jolting, slightly leave standstill, colourless to the sucking-off chloroform layer, combined chloroform liquid, add an amount of anhydrous sodium sulfate, filter, with a small amount of chloroform washing residue, reclaim solvent to doing, with the dissolve with methanol residue in the 25ml volumetric flask and be diluted to scale, shake up, cross 0.45 μ m microporous filter membrane, and get final product.
5. combined anthraquinone content assaying method: get Radix Et Rhizoma Rhei crude drug fine powder 0.06g, accurately weighed; Or draw the Radix Et Rhizoma Rhei extract that is equivalent to the 0.06g crude drug, decompression volatilizes solvent, places the 100ml round-bottomed flask, the 20ml that adds diethyl ether, water-bath (40 ℃) reflux, extract, 30 minutes is drawn ether solution and is discarded, the 20ml that adds diethyl ether again, water-bath (40 ℃) reflux, extract, 30 minutes is drawn ether solution and is discarded, residue volatilizes ether, adds 20% sulphuric acid 5.0ml, room temperature jolting 5 minutes, add chloroform 40ml, water-bath (80 ℃) back hydrolysis 120 minutes is put to room temperature again, the sucking-off chloroform layer, repeatedly add later on chloroform 20ml, jolting is slightly left standstill, colourless to the sucking-off chloroform layer, combined chloroform liquid adds an amount of anhydrous sodium sulfate, filters, with a small amount of chloroform washing residue, reclaim solvent to doing,, shake up in the 25ml volumetric flask and be diluted to scale with the dissolve with methanol residue, cross 0.45 μ m microporous filter membrane, and get final product.
6. algoscopy difference precision is drawn reference substance solution and each 20 μ l of need testing solution, and the injection liquid chromatography is measured, and be get final product.
Combined anthraquinone content (crude drug and decoction pieces)=total anthraquinones content-sequestered anthraquinone content
Sequestered anthraquinone content (aqueous extract)=total anthraquinones content-combined anthraquinone content
Adopt said method that Radix Et Rhizoma Rhei crude drug, decoction pieces and the decoction pieces aqueous extract concocted are measured among the present invention, and compare with traditional concocting method, see Table 1, Fig. 1 ~ 11.The result shows, combined anthraquinone content is significantly higher than tradition and concocts decoction pieces in the decoction pieces that Radix Et Rhizoma Rhei of the present invention is concocted, and sequestered anthraquinone content result antithesis, and total anthraquinones content is basically identical.
Through verifying with two kinds of decoction pieces of water extraction Radix Et Rhizoma Rhei, the sequestered anthraquinone content is all less in the aqueous extract of two kinds of methods of result, and general anthraquinone and combined anthraquinone content are all concocted decoction pieces apparently higher than tradition in the decoction pieces aqueous extract of the present invention simultaneously.Therefore, in clinical decoction is used, guarantee the discharge function of Radix Et Rhizoma Rhei, saved the consumption of decoction pieces, when producing economic benefit, produced again social benefit.
Table 1 Radix Et Rhizoma Rhei is concocted relatively (unit: the mg/g crude drug) of each step content of section
(in aloe-emodin, chrysophanic acid, chrysophanol, emodin, physcione content sum)
| Title | Total anthraquinones content | The sequestered anthraquinone content | Combined anthraquinone content |
| Crude drug | 18.649 | 0.698 | 17.951 |
| The decoction pieces that tradition is concocted | 18.048 | 13.134 | 4.914 |
| The decoction pieces that the present invention concocts | 18.592 | 0.567 | 18.025 |
| Tradition is concocted the aqueous extract of decoction pieces | 5.350 | 0.468 | 4.882 |
| The present invention concocts the aqueous extract of decoction pieces | 13.424 | 0.832 | 12.592 |
Claims (4)
1. crude drug preparation method that improves combined anthraquinone in the Radix Et Rhizoma Rhei decoction piece is characterized in that: the Radix Et Rhizoma Rhei crude drug, remove impurity, and the size sorting is put in the container, and steamed 2-6 hour, take out, section, drying makes Radix Et Rhizoma Rhei decoction piece.
2. the crude drug preparation method of combined anthraquinone in the described raising Radix Et Rhizoma Rhei decoction piece according to claim 1, it is characterized in that: the drying of section is to ventilate to drying after steamed, or cold drying in 50-70 ℃ of baking oven.
3. the crude drug preparation method of combined anthraquinone in the described raising Radix Et Rhizoma Rhei decoction piece according to claim 1, it is characterized in that: steamed in the container is Steam by water bath in airtight steamer, or in vapor tight tank logical vapours.
4. the crude drug preparation method of combined anthraquinone in the described raising Radix Et Rhizoma Rhei decoction piece of any one according to claim 1-3, it is characterized in that: combined anthraquinone content is not less than 90% of crude drug in the Radix Et Rhizoma Rhei decoction piece.
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| 叶定江主编.大黄.《中药炮制学》.上海科学技术出版社,1996, * |
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