CN103405497A - Preparation method of isodon excisoides total diterpenoid extractive - Google Patents
Preparation method of isodon excisoides total diterpenoid extractive Download PDFInfo
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Abstract
The invention relates to a preparation method of an isodon excisoides total diterpenoid extractive, which is capable of effectively solving the problem of extracting total diterpenoid from isodon excisoides with high quality and high extraction rate. The preparation method disclosed by the invention comprises the following steps of crushing isodon excisoides, decocting by adding water, filtering water decoction, and cooling to form sampling solution; after immersing macroreticular resin by using ethanol, dynamically cleaning resin by using ethanol, washing till alcohol smell does not exist, immersing by using hydrochloric acid, washing again till the macroreticular resin is neutral, then, immersing by using NaOH solution, dynamically cleaning resin, washing till the macroreticular resin is neutral, after dynamically eluting ethanol, packing the macroreticular resin in a column through a wet method, and dynamically absorbing the sampling solution through a resin column; and eluting the sample column by using water after absorbing, eluting through ethanol again, collecting ethanol eluent, decompressing and recycling the solvent, and evaporating, thereby obtaining the isodon excisoides total diterpenoid extractive. The preparation method disclosed by the invention is simple, easy to operate and use, steady, reliable, high in product yield, good in quality, simple, practical and free from pollution; research basis is provided for researching isodon amethystoides diterpenoid anti-tumour candidate drugs.
Description
Technical field
The present invention relates to Isodon excisoides total diterpene extract, and the preparation method of macroporous adsorbent resin Isodon excisoides total diterpene extract, field of medicaments belonged to.
Background technology
The Rabdosia plant demonstrates obvious antitumor action, since 1976 in this platymiscium diterpene-kind compound become the focus that Chinese scholars is sought the new antitumoral lead compound.In recent years along with the discovery successively of new Herba Rabdosiae glaucocalycis diterpene-kind compound, reported and had in a large number Cytotoxic Herba Rabdosiae glaucocalycis Diterpenoids from bulbus, at present as the antitumor candidate compound rubescensine A, Eriocalyxin A., rabdophyllin G etc., Related product Folium solani verbascifolii sheet (ternateleaf rabdosia leaf), Rabdosia rubescens syrup, sheet (Rabdosia rubescens), XIAOYAN LIDAN PIAN (containing Herba Rabdosiae Lophanthoidis) etc. are arranged.In addition, there is report to show that the Herba Rabdosiae glaucocalycis Diterpenoids from bulbus still has the effects such as obvious antibacterial action, anti-liver injury.
Isodon excisoides
Isodon excisoides(Sun ex C. H. Hu) C. Y. Wu et H. W. Li is Labiatae Rabdosia herbaceos perennial, begins to be stated from herbal for Relief of Famines, enters decoct more, the determined curative effects such as treatment chronic pharyngitis, esophageal carcinoma.Our research shows in Isodon excisoides total diterpene body has stronger inhibitory action to mice lotus s180 ascitic type tumor; Separately studies have reported that the anti tumor activity in vitro of the multiple diterpene-kind compound of Isodon excisoides.Therefore Diterpenoids from bulbus is anti-tumor active ingredient in this platymiscium, and the treatment of malignant tumor is had to larger using value.
Because Isodon excisoides mainly contains diterpene-kind compound, it after such composition purification, is the bitter neutral compound of colourless crystallization, character and the compatible principle of structural similarity according to diterpene-kind compound, the extracting method of report has the ether warm macerating at present, solvent apportion design methanol or ethanol extraction, the most acetone room temperatures that adopt of solvent apportion design are extracted the solvent apportion design.Also useful warm water soaking in early days, active carbon adsorption, but efficiency is low, and impurity disturbs large, and not environmental protection, be not suitable for industrialized great production, current no longer application.
In Isodon excisoides total diterpene body, has stronger antitumor action, but have no at present the preparation method of Isodon excisoides total diterpene, how to set up and both met the clinical application characteristics, efficient Extraction and enrichment method easily again, be the key of Chinese medicine Natural Medicine Chemistry research, the present invention adopts modern macroporous adsorbing resin for purification technology to prepare the Isodon excisoides total diterpene.The present invention can remove a large amount of impurity, and more than the total diterpene weight percentage of preparation reached 60 % at least, preparation efficiency was high, reproducible, and preparation process is without poisonous organic solvent pollution, and cost is low, is applicable to suitability for industrialized production.
Summary of the invention
The present invention's purpose just is to provide a kind of preparation method of Isodon excisoides total diterpene extract, can effectively solve the problem from extraction total diterpene Isodon excisoides of high-quality, high extraction.
Technical scheme of the present invention is:
(1), the preparation of sample solution: method is, pulverizing medicinal materials by the Isodon excisoides drying, decoct with water twice, decocted 1 hour at every turn, add for the first time the water of 12 times of Isodon excisoides weight, the water that adds for the second time 8 times of Isodon excisoides weight in medicinal residues, merge decocting liquid twice, filter the standing room temperature that is cooled to, get supernatant, be sample solution;
(2), to the resin pretreatment: method is, macroporous adsorbent resin is that 95% soak with ethanol is after 24 hours by volumetric concentration, by volumetric concentration, be 95% ethanol dynamic cleaning resin again, amount of alcohol added is the volume of 5 times of resins, be washed to again without after the alcohol flavor, by volumetric concentration, be 5% soak with hydrochloric acid 6 hours successively, the dynamic cleaning macroporous adsorbent resin, the hydrochloric acid addition is 3 times of volumes of macroporous adsorbent resin, again be washed to neutrality, by volumetric concentration, be 5% NaOH solution soaking 6 hours afterwards, the dynamic cleaning resin, NaOH solution addition is 3 times of volumes of macroporous adsorbent resin, and wash with water to neutrality, it by volumetric concentration, is 95% ethanol dynamic desorption, be eluted to the water that adds 5 times of volumes, be not white in color till turbid solution, obtain the good macroporous adsorbent resin of pretreatment,
(3), dress post and absorption: the macroporous adsorbent resin wet method that step (2) pretreatment is good fills post, makes the resin bed blade diameter length ratio reach 1 ︰ 6-12, then the sample solution in step (1) is passed through to resin column, carries out dynamic adsorption with the 1.6BV/h flow velocity;
(4), remove impurity and eluting: after having adsorbed, resin column is first with 2-6 times of volume water elution, by the volumetric concentration of 2 times of volumes, be the ethanol elution of 10-25% again, by the volumetric concentration of 2 times of volumes, be the ethanol elution of 60-90% again, each elution flow rate is 3BV/h, and collected volume concentration is the eluent of 60-90% ethanol, decompression and solvent recovery ethanol, evaporate to dryness, obtain Isodon excisoides total diterpene extract.
The macroporous adsorbent resin of described step (2) is a kind of of D101 type macroporous adsorbent resin, HP20 type macroporous adsorbent resin, AB8 type macroporous adsorbent resin.
The resin bed blade diameter length ratio of described step (3) is 1 ︰ 6, or 1 ︰ 7, or 1 ︰ 8, or 1 ︰ 9, or 1 ︰ 10, or 1:11, or 1:12.
The inventive method is simple, easy to operate, reliable and stable, the product yield is high, quality is good, simple and practical, pollution-free, the Diterpene macroporous resin enrichment technique that meets suitability for industrialized production, character for main effective ingredient and impurity component, take maximal absorptive capacity and absorption-desorption rate as investigating index, preferably the macroporous adsorbent resin of preparation use, the content of total diterpene of take is leading indicator, optimized the production method that Amberlyst process prepares the Isodon excisoides total diterpene, for the research of Herba Rabdosiae glaucocalycis diterpene antitumor drug candidate provides Research foundation, has larger economic and social benefit.
The accompanying drawing explanation
Fig. 1 is reference substance spectrogram of the present invention.
Fig. 2 is Isodon excisoides total diterpene extract spectrogram of the present invention.
Fig. 3 is medical material spectrogram of the present invention.
The specific embodiment
Following examples are intended to the specific embodiment of the present invention is elaborated.Rather than limit in any form the present invention.
The present invention, in concrete enforcement, is realized by following steps:
(1), the preparation of sample solution: the medical material 1kg of Isodon excisoides drying is pulverized, decoct with water twice, decocted 1 hour at every turn, add for the first time water 12L, in medicinal residues, add for the second time water 8L, merge decocting liquid twice, filter, the standing room temperature that is cooled to, obtain supernatant 10L, is sample solution;
(2), to the resin pretreatment: method is, the D101 macroporous adsorbent resin is that 95% soak with ethanol is after 24 hours by volumetric concentration, wet method dress post, and by volumetric concentration, be 95% ethanol dynamic cleaning resin, amount of alcohol added is the volume of 5 times of resins, be washed to again without after the alcohol flavor, by volumetric concentration, be 5% soak with hydrochloric acid 6 hours successively, the dynamic cleaning resin, the hydrochloric acid addition is 3 times of volumes of resin, again be washed to neutrality, by volumetric concentration, be 5% NaOH solution soaking 6 hours afterwards, the dynamic cleaning resin, NaOH solution addition is 3 times of volumes of resin, and wash with water to neutrality, it by volumetric concentration, is 95% ethanol dynamic desorption, be eluted to the water that adds 5 times of volumes, be not white in color till turbid solution, obtain the good resin of pretreatment,
(3), dress post and absorption: the resin wet method that step (2) pretreatment is good fills post, makes the resin bed blade diameter length ratio reach 1 ︰ 8, then the sample solution in step (1) is passed through to resin column, carries out dynamic adsorption with the 1.6BV/h flow velocity;
(4) remove impurity and eluting: after having adsorbed, resin column is first used 4 times of volume water elutions, by the volumetric concentration of 2 times of volumes, be 25% ethanol elution again, by the volumetric concentration of 2 times of volumes, be 70% ethanol elution again, each elution flow rate is 3BV/h, and collected volume concentration is the eluent of 70% ethanol, decompression and solvent recovery ethanol, evaporate to dryness, obtain Isodon excisoides diterpene 23.89g, and Isodon excisoides diterpene weight percentage is 69.2%.
Embodiment 2
The present invention is realized by following steps:
(1), the preparation of sample solution: the medical material 1kg of Isodon excisoides drying is pulverized, decoct with water twice, decocted 1 hour at every turn, add for the first time water 12L, in medicinal residues, add for the second time water 8L, merge decocting liquid twice, filter, the standing room temperature that is cooled to, obtain supernatant 10L, is sample solution;
(2), to the resin pretreatment: method is, the HP20 macroporous adsorbent resin is that 95% soak with ethanol is after 24 hours by volumetric concentration, wet method dress post, and by volumetric concentration, be 95% ethanol dynamic cleaning resin, amount of alcohol added is the volume of 5 times of resins, be washed to again without after the alcohol flavor, by volumetric concentration, be 5% soak with hydrochloric acid 6 hours successively, the dynamic cleaning resin, the hydrochloric acid addition is 3 times of volumes of resin, again be washed to neutrality, by volumetric concentration, be 5% NaOH solution soaking 6 hours afterwards, the dynamic cleaning resin, NaOH solution addition is 3 times of volumes of resin, and wash with water to neutrality, it by volumetric concentration, is 95% ethanol dynamic desorption, be eluted to the water that adds 5 times of volumes, be not white in color till turbid solution, obtain the good resin of pretreatment,
(3), dress post and absorption: the resin wet method that step (2) pretreatment is good fills post, makes the resin bed blade diameter length ratio reach 1 ︰ 10, then the sample solution in step (1) is passed through to resin column, carries out dynamic adsorption with the 1.6BV/h flow velocity;
(4) remove impurity and eluting: after having adsorbed, resin column is first used 4 times of volume water elutions, by the volumetric concentration of 2 times of volumes, be 25% ethanol elution again, by the volumetric concentration of 2 times of volumes, be 80% ethanol elution again, each elution flow rate is 3BV/h, and collected volume concentration is the eluent of 80% ethanol, decompression and solvent recovery ethanol, evaporate to dryness, obtain Isodon excisoides diterpene 21.89g, Isodon excisoides diterpene weight percentage 65.2%.
Embodiment 3
The present invention is realized by following steps:
(1), the preparation of sample solution: the medical material 1kg of Isodon excisoides drying is pulverized, decoct with water twice, decocted 1 hour at every turn, add for the first time water 12L, in medicinal residues, add for the second time water 8L, merge decocting liquid twice, filter, the standing room temperature that is cooled to, obtain supernatant 10L, is sample solution;
(2), to the resin pretreatment: method is, the AB8 macroporous adsorbent resin is that 95% soak with ethanol is after 24 hours by volumetric concentration, wet method dress post, and by volumetric concentration, be 95% ethanol dynamic cleaning resin, amount of alcohol added is the volume of 5 times of resins, be washed to again without after the alcohol flavor, by volumetric concentration, be 5% soak with hydrochloric acid 6 hours successively, the dynamic cleaning resin, the hydrochloric acid addition is 3 times of volumes of resin, again be washed to neutrality, by volumetric concentration, be 5% NaOH solution soaking 6 hours afterwards, the dynamic cleaning resin, NaOH solution addition is 3 times of volumes of resin, and wash with water to neutrality, it by volumetric concentration, is 95% ethanol dynamic desorption, be eluted to the water that adds 5 times of volumes, be not white in color till turbid solution, obtain the good resin of pretreatment,
(3), dress post and absorption: the resin wet method that step (2) pretreatment is good fills post, makes the resin bed blade diameter length ratio reach 1 ︰ 6, then the sample solution in step (1) is passed through to resin column, carries out dynamic adsorption with the 1.6BV/h flow velocity;
(4) remove impurity and eluting: after having adsorbed, resin column is first used 6 times of volume water elutions, by the volumetric concentration of 2 times of volumes, be 25% ethanol elution again, by the volumetric concentration of 2 times of volumes, be 90% ethanol elution again, each elution flow rate is 3BV/h, and collected volume concentration is the eluent of 90% ethanol, decompression and solvent recovery ethanol, evaporate to dryness, obtain Isodon excisoides diterpene 20.42g, Isodon excisoides diterpene weight content 67.3%.
Adopt said method to prepare three batches of Isodon excisoides total diterpenes, all obtained identical or akin result, show that this method process stabilizing is reliable, good product quality, purity is high, and its product is effective to malignant tumor and has obtained sufficient proof through experiment, and relevant experimental data is as follows:
Total diterpene assay in Isodon excisoides total diterpene position
The content assaying method of total diterpene in Isodon excisoides total diterpene position: " 2010 editions appendix VA of Chinese pharmacopoeia measure, and the Kamebanin of take is reference substance, detect wavelength 235nm according to ultraviolet spectrophotometry.
1, the preparation of reference substance solution: precision takes Kamebanin reference substance 3.12mg, to the 10ml volumetric flask, by methanol constant volume to scale product stock solution in contrast, precision sucts in the volumetric flask of stating reference substance stock solution 1ml to 10ml again, by methanol constant volume, to scale, make concentration: the reference substance solution of 0.031mg/ml.
2, the preparation of Isodon excisoides total diterpene need testing solution: precision takes Isodon excisoides extract 6.50mg, to the 10ml volumetric flask, with dissolve with methanol and be settled to scale.The accurate absorption in above-mentioned solution 1ml to 10ml volumetric flask, add methanol constant volume to scale again, makes the need testing solution of 0.065mg/ml.
3, the preparation of Isodon excisoides medical material need testing solution: get dry Isodon excisoides medical material fine powder (crossing the pharmacopeia sieve No. 3) 1g, accurately weighed is 0.101g, puts in tool match conical flask, and precision adds methanol 100ml, accurately weighed weight, reflux, extract, 1h, let cool, accurately weighed, with methanol, supply the weight of less loss, shake up, filter, get the need testing solution that subsequent filtrate namely obtains 1.01mg/ml.
4, according to the content assaying method of setting up, measure the content of total diterpene in medical material, Isodon excisoides diterpene position, calculate and extract the final rate of transform in purge process.The results are shown in Table 1.Spectrogram is shown in Fig. 1, Fig. 2, Fig. 3.
Content, the rate of transform of total diterpene in 3 batches of Isodon excisoides total diterpene extracts of table 1
Pharmaceutical test
The activity experiment of Isodon excisoides total diterpene of the present invention, the experiment proved that, Isodon excisoides total diterpene prepared by the present invention has: s180 ascitic type tumor is had to stronger impact in body, the treatment of malignant tumor is had to larger using value.
The clean level of 1 experiment material kunming mice, the Isodon excisoides total diterpene.
The foundation of 2 murine sarcoma S180 models
Choose 50 of mices, adaptability is raised l after week, is divided at random 5 groups, carries out the inoculation of sarcoma S180.Get inoculation 7 days, and tumor growth is good, without the ascitic type S180 tumor-bearing mice of diabrosis, by the cervical vertebra execution that dislocate, be defined on stencil plate, by skin of abdomen with after 2% iodine tincture disinfection, 75% alcohol disinfecting, extraction ascites.With normal saline dilution, become every milliliter of suspension that contains 1 * 107 oncocyte, be seeded in the front axillary fossa of experiment mice subcutaneous, every 0.2 mL, after inoculation 124h, random packet.
1.3 grouping, administration and detection
Each tumor-bearing mice body weight of weighing, be divided into respectively 5 groups at random by tumor volume size, 10 every group.Gavage respectively the high, normal, basic dosage of Isodon excisoides total diterpene (200mg/kg, 100mg/kg, 50mg/kg, the gavage volume is 0.2mL/10g), positive controls (Bleomycin A5), negative control group (normal saline).After gastric infusion 12d, the stripping tumor is weighed continuously.With the maximum major diameter (x) of vernier caliper measurement tumor body, transverse diameter (y), to calculate each and respectively organize result, result shows that in Isodon excisoides total diterpene body, the tumour inhibiting rate to lotus S180 mice is 46.8%.Show in Isodon excisoides total diterpene body and have stronger antitumor action.
Claims (5)
1. an Isodon excisoides total diterpene extract, is characterized in that the weight percentage of total diterpene in Isodon excisoides total diterpene extract is no less than 60%.
2. according to described this Isodon excisoides total diterpene extract of claims 1, it is characterized in that, in Isodon excisoides total diterpene extract, the weight percentage of total diterpene is 60%-72%.
3. the preparation method of the described Isodon excisoides total diterpene of claims 1 or 2 extract, is characterized in that, comprises the following steps:
(1), the preparation of sample solution: method is, pulverizing medicinal materials by the Isodon excisoides drying, decoct with water twice, decocted 1 hour at every turn, add for the first time the water of 12 times of Isodon excisoides weight, the water that adds for the second time 8 times of Isodon excisoides weight in medicinal residues, merge decocting liquid twice, filter the standing room temperature that is cooled to, get supernatant, be sample solution;
(2), to the resin pretreatment: method is, macroporous adsorbent resin is that 95% soak with ethanol is after 24 hours by volumetric concentration, by volumetric concentration, be 95% ethanol dynamic cleaning resin again, amount of alcohol added is the volume of 5 times of resins, be washed to again without after the alcohol flavor, by volumetric concentration, be 5% soak with hydrochloric acid 6 hours successively, the dynamic cleaning macroporous adsorbent resin, the hydrochloric acid addition is 3 times of volumes of macroporous adsorbent resin, again be washed to neutrality, by volumetric concentration, be 5% NaOH solution soaking 6 hours afterwards, the dynamic cleaning resin, NaOH solution addition is 3 times of volumes of macroporous adsorbent resin, and wash with water to neutrality, it by volumetric concentration, is 95% ethanol dynamic desorption, be eluted to the water that adds 5 times of volumes, be not white in color till turbid solution, obtain the good macroporous adsorbent resin of pretreatment,
(3), dress post and absorption: the macroporous adsorbent resin wet method that step (2) pretreatment is good fills post, makes the resin bed blade diameter length ratio reach 1 ︰ 6-12, then the sample solution in step (1) is passed through to resin column, carries out dynamic adsorption with the 1.6BV/h flow velocity;
(4), remove impurity and eluting: after having adsorbed, resin column is first with 2-6 times of volume water elution, by the volumetric concentration of 2 times of volumes, be the ethanol elution of 10-25% again, by the volumetric concentration of 2 times of volumes, be the ethanol elution of 60-90% again, each elution flow rate is 3BV/h, and collected volume concentration is the eluent of 50-80% ethanol, decompression and solvent recovery ethanol, evaporate to dryness, obtain Isodon excisoides total diterpene extract.
4. the preparation method of Isodon excisoides total diterpene extract according to claim 3, it is characterized in that, the macroporous adsorbent resin of described step (2) is a kind of of D101 type macroporous adsorbent resin, HP20 type macroporous adsorbent resin, AB8 type macroporous adsorbent resin.
5. the preparation method of Isodon excisoides total diterpene extract according to claim 3, is characterized in that, the resin bed blade diameter length ratio of described step (3) is 1:6, or 1 ︰ 7, or 1 ︰ 8, or 1 ︰ 9, or 1 ︰ 10, or 1:11, or 1:12.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104306435A (en) * | 2014-10-14 | 2015-01-28 | 河南省医药科学研究院 | Extraction method of isodon excisoides extracts |
| CN106928064A (en) * | 2017-02-20 | 2017-07-07 | 河南中医药大学 | A kind of compound extracted from Isodon excisoides and its preparation method and application |
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| CN102389456A (en) * | 2011-11-29 | 2012-03-28 | 苏州大学 | Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A |
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| CN101940615A (en) * | 2010-08-25 | 2011-01-12 | 吉林天药药物研发有限公司 | New preparation method of Isodon excisa total diterpene |
| CN102389456A (en) * | 2011-11-29 | 2012-03-28 | 苏州大学 | Method for extracting isodon japonica var.galaucocalyx total diterpenoids or Glaucocalyxin A |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104306435A (en) * | 2014-10-14 | 2015-01-28 | 河南省医药科学研究院 | Extraction method of isodon excisoides extracts |
| CN104306435B (en) * | 2014-10-14 | 2018-11-13 | 河南省医药科学研究院 | A kind of extracting method of Isodon excisoides extract |
| CN106928064A (en) * | 2017-02-20 | 2017-07-07 | 河南中医药大学 | A kind of compound extracted from Isodon excisoides and its preparation method and application |
| CN106928064B (en) * | 2017-02-20 | 2019-08-16 | 河南中医药大学 | A kind of compound and its preparation method and application extracted from Isodon excisoides |
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