CN103405497B - A kind of preparation method of Isodon excisoides total diterpene extract - Google Patents
A kind of preparation method of Isodon excisoides total diterpene extract Download PDFInfo
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Abstract
The present invention relates to the preparation method of Isodon excisoides total diterpene extract, effectively can solve the problem extracting total diterpene from Isodon excisoides of high-quality, high extraction, method is pulverized by Isodon excisoides, decoct with water, decocting liquid filters, cooling, becomes sample solution; Macroporous adsorbent resin is with after body soak with ethanol, then use ethanol dynamic cleaning resin, then be washed to without after alcohol taste, with soak with hydrochloric acid, again be washed to neutrality, soak by NaOH solution afterwards, dynamic cleaning resin, and wash with water to neutrality, after ethanol dynamic desorption, by macroporous adsorbent resin wet method dress post, by sample solution by resin column, carry out dynamic adsorption; After having adsorbed, resin column first washes with water, then uses ethanol elution, collect ethanol elution, decompression and solvent recovery, evaporate to dryness, obtain, the inventive method is simple, and easy to operate is reliable and stable, product yield is high, quality is good, simple and practical, pollution-free, for the research of Herba Rabdosiae glaucocalycis diterpene antitumor drug candidate provides Research foundation.
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, belong to field of medicaments.
Background technology
Rabdosia plant demonstrates obvious antitumor action, and since 1976, in this platymiscium, diterpene-kind compound becomes the focus that Chinese scholars seeks new antitumoral lead compound.In recent years along with the discovery successively of new Herba Rabdosiae glaucocalycis diterpene-kind compound, report and there is Cytotoxic Herba Rabdosiae glaucocalycis Diterpenoids from bulbus in a large number, rubescensine A, Eriocalyxin A., rabdophyllin G etc. are had, Related product Folium solani verbascifolii sheet (ternateleaf rabdosia leaf), Rabdosia rubescens syrup, sheet (Rabdosia rubescens), XIAOYAN LIDAN PIAN (containing Herba Rabdosiae Lophanthoidis) etc. at present as antitumor candidate compound.In addition, report display Herba Rabdosiae glaucocalycis Diterpenoids from bulbus is had still to have 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 loaded in herbal for Relief of Famines, enters decoct more, determined curative effect such as treatment chronic pharyngitis, esophageal carcinoma etc.Our research shows there is stronger inhibitory action to mice lotus s180 ascitic type tumor in Isodon excisoides total diterpene body; 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, has larger using value to the treatment of malignant tumor.
Because Isodon excisoides is mainly containing diterpene-kind compound, it is the bitter neutral compound of colourless crystallization after such component purification, according to the character of diterpene-kind compound and the principle of structure similar compatibility, the extracting method of current report has ether warm macerating, solvent apportion design methanol or ethanol extraction, solvent apportion design majority adopts acetone room temperature Extraction solvent apportion design.Early stage also useful warm water soaking, active carbon adsorption, but efficiency is low, impurity interference is large, not environmentally, is not suitable for industrialized great production, currently no longer applies.
In Isodon excisoides total diterpene body, there is stronger antitumor action, but have no the preparation method of Isodon excisoides total diterpene at present, how to set up and both met clinical application feature, 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 Isodon excisoides total diterpene.The present invention can remove a large amount of impurity, and the total diterpene weight percentage of preparation at least reaches 60 more than %, and preparation efficiency is high, reproducible, and preparation process is polluted without toxic organic solvents, and cost is low, is applicable to suitability for industrialized production.
Summary of the invention
The object of the present invention is just to provide a kind of preparation method of Isodon excisoides total diterpene extract, effectively can solve the problem extracting total diterpene from Isodon excisoides of high-quality, high extraction.
Technical scheme of the present invention is:
(1), the preparation of sample solution: method is, by the pulverizing medicinal materials of Isodon excisoides drying, decoct with water twice, each decoction 1 hour, adds the water of Isodon excisoides weight 12 times for the first time, the water of Isodon excisoides weight 8 times is added in second time medicinal residues, merge twice decocting liquid, filter, leave standstill and be cooled to room temperature, get supernatant, be sample solution;
(2), to resin pretreatment: method is, macroporous adsorbent resin volumetric concentration is that the soak with ethanol of 95% is after 24 hours, be the ethanol dynamic cleaning resin of 95% again by volumetric concentration, amount of alcohol added is the volume of resin 5 times, be washed to without after alcohol taste again, be the soak with hydrochloric acid 6 hours of 5% successively by volumetric concentration, dynamic cleaning macroporous adsorbent resin, hydrochloric acid addition is macroporous adsorbent resin 3 times of volumes, again be washed to neutrality, 6 hours are soaked afterwards by the NaOH solution that volumetric concentration is 5%, dynamic cleaning resin, NaOH solution addition is macroporous adsorbent resin 3 times of volumes, and wash with water to neutrality, with the ethanol dynamic desorption that volumetric concentration is 95%, be eluted to the water adding 5 times of volumes, till not in white turbid solution, obtain the macroporous adsorbent resin that pretreatment is good,
(3), dress post and absorption: macroporous adsorbent resin wet method good for step (2) pretreatment is filled post, makes resin bed blade diameter length ratio reach 1 ︰ 6-12, then by the sample solution in step (1) by resin column, carry out dynamic adsorption with 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, be the ethanol elution of 10-25% by the volumetric concentration of 2 times of volumes again, be the ethanol elution of 60-90% by the volumetric concentration of 2 times of volumes 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, obtains Isodon excisoides total diterpene extract.
The macroporous adsorbent resin of described step (2) is the one 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, product yield is high, quality is good, simple and practical, pollution-free, meet the Diterpene macroporous resin enrichment technique of suitability for industrialized production, for the character of principle active component and impurity component, with maximal absorptive capacity and absorption-desorption rate for inspection target, the preferably macroporous adsorbent resin of preparation, with the content of total diterpene for leading indicator, optimize the production method that Amberlyst process prepares Isodon excisoides total diterpene, for the research of Herba Rabdosiae glaucocalycis diterpene antitumor drug candidate provides Research foundation, there is larger economic and social benefit.
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.
Detailed description of the invention
Following examples are intended to elaborate to the specific embodiment of the present invention.Instead of limit the present invention in any form.
Embodiment 1
The present invention, in concrete enforcement, is realized by following steps:
(1), the preparation of sample solution: pulverized by the medical material 1kg of Isodon excisoides drying, decoct with water twice, each decoction 1 hour, add water 12L for the first time, add water in second time medicinal residues 8L, merges twice decocting liquid, filter, leave standstill and be cooled to room temperature, obtain supernatant 10L, be sample solution;
(2), to resin pretreatment: method is, D101 macroporous adsorbent resin volumetric concentration is that the soak with ethanol of 95% is after 24 hours, wet method dress post, and be the ethanol dynamic cleaning resin of 95% by volumetric concentration, amount of alcohol added is the volume of resin 5 times, be washed to without after alcohol taste again, be the soak with hydrochloric acid 6 hours of 5% successively by volumetric concentration, dynamic cleaning resin, hydrochloric acid addition is resin 3 times of volumes, again be washed to neutrality, 6 hours are soaked afterwards by the NaOH solution that volumetric concentration is 5%, dynamic cleaning resin, NaOH solution addition is resin 3 times of volumes, and wash with water to neutrality, with the ethanol dynamic desorption that volumetric concentration is 95%, be eluted to the water adding 5 times of volumes, till not in white turbid solution, obtain the resin that pretreatment is good,
(3), dress post and absorption: resin wet method good for step (2) pretreatment is filled post, makes resin bed blade diameter length ratio reach 1 ︰ 8, then by the sample solution in step (1) by resin column, carry out dynamic adsorption with 1.6BV/h flow velocity;
(4) remove impurity and eluting: after having adsorbed, resin column first uses 4 times of volume water elutions, be the ethanol elution of 25% by the volumetric concentration of 2 times of volumes again, be the ethanol elution of 70% by the volumetric concentration of 2 times of volumes 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, obtains 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: pulverized by the medical material 1kg of Isodon excisoides drying, decoct with water twice, each decoction 1 hour, add water 12L for the first time, add water in second time medicinal residues 8L, merges twice decocting liquid, filter, leave standstill and be cooled to room temperature, obtain supernatant 10L, be sample solution;
(2), to resin pretreatment: method is, HP20 macroporous adsorbent resin volumetric concentration is that the soak with ethanol of 95% is after 24 hours, wet method dress post, and be the ethanol dynamic cleaning resin of 95% by volumetric concentration, amount of alcohol added is the volume of resin 5 times, be washed to without after alcohol taste again, be the soak with hydrochloric acid 6 hours of 5% successively by volumetric concentration, dynamic cleaning resin, hydrochloric acid addition is resin 3 times of volumes, again be washed to neutrality, 6 hours are soaked afterwards by the NaOH solution that volumetric concentration is 5%, dynamic cleaning resin, NaOH solution addition is resin 3 times of volumes, and wash with water to neutrality, with the ethanol dynamic desorption that volumetric concentration is 95%, be eluted to the water adding 5 times of volumes, till not in white turbid solution, obtain the resin that pretreatment is good,
(3), dress post and absorption: resin wet method good for step (2) pretreatment is filled post, makes resin bed blade diameter length ratio reach 1 ︰ 10, then by the sample solution in step (1) by resin column, carry out dynamic adsorption with 1.6BV/h flow velocity;
(4) remove impurity and eluting: after having adsorbed, resin column first uses 4 times of volume water elutions, be the ethanol elution of 25% by the volumetric concentration of 2 times of volumes again, be the ethanol elution of 80% by the volumetric concentration of 2 times of volumes 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, obtains 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: pulverized by the medical material 1kg of Isodon excisoides drying, decoct with water twice, each decoction 1 hour, add water 12L for the first time, add water in second time medicinal residues 8L, merges twice decocting liquid, filter, leave standstill and be cooled to room temperature, obtain supernatant 10L, be sample solution;
(2), to resin pretreatment: method is, AB8 macroporous adsorbent resin volumetric concentration is that the soak with ethanol of 95% is after 24 hours, wet method dress post, and be the ethanol dynamic cleaning resin of 95% by volumetric concentration, amount of alcohol added is the volume of resin 5 times, be washed to without after alcohol taste again, be the soak with hydrochloric acid 6 hours of 5% successively by volumetric concentration, dynamic cleaning resin, hydrochloric acid addition is resin 3 times of volumes, again be washed to neutrality, 6 hours are soaked afterwards by the NaOH solution that volumetric concentration is 5%, dynamic cleaning resin, NaOH solution addition is resin 3 times of volumes, and wash with water to neutrality, with the ethanol dynamic desorption that volumetric concentration is 95%, be eluted to the water adding 5 times of volumes, till not in white turbid solution, obtain the resin that pretreatment is good,
(3), dress post and absorption: resin wet method good for step (2) pretreatment is filled post, makes resin bed blade diameter length ratio reach 1 ︰ 6, then by the sample solution in step (1) by resin column, carry out dynamic adsorption with 1.6BV/h flow velocity;
(4) remove impurity and eluting: after having adsorbed, resin column first uses 6 times of volume water elutions, be the ethanol elution of 25% by the volumetric concentration of 2 times of volumes again, be the ethanol elution of 90% by the volumetric concentration of 2 times of volumes 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, obtains 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 achieve 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 obtains sufficient proof through experiment, and regarding assay 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: measuring according to ultraviolet spectrophotometry " Chinese Pharmacopoeia " 2010 editions annex VA, take Kamebanin as reference substance, determined wavelength 235nm.
1, the preparation of reference substance solution: precision takes Kamebanin reference substance 3.12mg, to in 10ml volumetric flask, by methanol constant volume to scale product stock solution in contrast, precision sucts in the volumetric flask stating reference substance stock solution 1ml to 10ml again, by methanol constant volume to scale, the reference substance solution of obtained concentration: 0.031mg/ml.
2, the preparation of Isodon excisoides total diterpene need testing solution: precision takes Isodon excisoides extract 6.50mg, in 10ml volumetric flask, is settled to scale with dissolve with methanol.Again in above-mentioned solution 1ml to the 10ml volumetric flask of accurate absorption, add methanol constant volume to scale, the need testing solution of obtained 0.065mg/ml.
3, the preparation of Isodon excisoides medical material need testing solution: get dry Isodon excisoides fine medicinal material powder (crossing No. 3 pharmacopeia sieves) 1g, accurately weighed is 0.101g, and put in tool match conical flask, precision adds methanol 100ml, accurately weighed weight, reflux, extract, 1h, lets cool, accurately weighed, the weight of less loss is supplied with methanol, shake up, filter, get the need testing solution that namely subsequent filtrate obtains 1.01mg/ml.
4, measure the content of total diterpene in medical material, Isodon excisoides diterpene position according to the content assaying method set up, calculate the final rate of transform in extraction purification 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 table 13 batches of Isodon excisoides total diterpene extracts
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: have stronger impact to s180 ascitic type tumor in body, have larger using value to the treatment of malignant tumor.
1 experiment material cleaning grade kunming mice, Isodon excisoides total diterpene.
The foundation of 2 S180 sarcoma models
Choose mice 50, adaptability is divided into 5 groups at random, carries out the inoculation of euphorbia egg decoctum after raising l week.Get inoculation 7 days, and tumor growth is good, without the ascitic type S180 tumor-bearing mice of diabrosis, is put to death, be defined on stencil plate by cervical dislocation, after skin of abdomen 2% iodine tincture disinfection, 75% alcohol disinfecting, extracts ascites.Become every milliliter containing the suspension of 1 × 107 oncocyte with normal saline dilution, before being seeded in experiment mice, axillary fossa is subcutaneous, every only 0.2 mL, after inoculation 124h, and random packet.
1.3 groupings, administration and detection
Weigh each tumor-bearing mice body weight, be divided into 5 groups at random respectively by tumor volume size, often organize 10.Gavage the high, normal, basic dosage of Isodon excisoides total diterpene (200mg/kg, 100mg/kg, 50mg/kg, gavage volume is 0.2mL/10g) respectively, positive controls (Bleomycin A5), negative control group (normal saline).After continuous gastric infusion 12d, stripping tumor is weighed.With the maximum major diameter (x) of vernier caliper measurement tumor body, transverse diameter (y), calculate and respectively organize result, it is 46.8% that result to show in Isodon excisoides total diterpene body the tumour inhibiting rate of mice bearing S180.Show, in Isodon excisoides total diterpene body, there is stronger antitumor action.
Claims (3)
1. a preparation method for Isodon excisoides total diterpene extract, is characterized in that, in this Isodon excisoides total diterpene extract, the weight percentage of total diterpene is 60%-72%, and its preparation method comprises the following steps:
(1), the preparation of sample solution: method is, by the pulverizing medicinal materials of Isodon excisoides drying, decoct with water twice, each decoction 1 hour, adds the water of Isodon excisoides weight 12 times for the first time, the water of Isodon excisoides weight 8 times is added in second time medicinal residues, merge twice decocting liquid, filter, leave standstill and be cooled to room temperature, get supernatant, be sample solution;
(2), to resin pretreatment: method is, D101 macroporous adsorbent resin volumetric concentration is that the soak with ethanol of 95% is after 24 hours, be the ethanol dynamic cleaning resin of 95% again by volumetric concentration, amount of alcohol added is the volume of resin 5 times, be washed to without after alcohol taste again, be the soak with hydrochloric acid 6 hours of 5% successively by volumetric concentration, dynamic cleaning macroporous adsorbent resin, hydrochloric acid addition is macroporous adsorbent resin 3 times of volumes, again be washed to neutrality, 6 hours are soaked afterwards by the NaOH solution that volumetric concentration is 5%, dynamic cleaning resin, NaOH solution addition is macroporous adsorbent resin 3 times of volumes, and wash with water to neutrality, with the ethanol dynamic desorption that volumetric concentration is 95%, be eluted to the water adding 5 times of volumes, till not in white turbid solution, obtain the macroporous adsorbent resin that pretreatment is good,
(3), dress post and absorption: macroporous adsorbent resin wet method good for step (2) pretreatment is filled post, makes resin bed blade diameter length ratio reach 1 ︰ 6-12, then by the sample solution in step (1) by resin column, carry out dynamic adsorption with 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, be the ethanol elution of 10-25% by the volumetric concentration of 2 times of volumes again, be the ethanol elution of 60-90% by the volumetric concentration of 2 times of volumes 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, obtains Isodon excisoides total diterpene extract.
2. the preparation method of Isodon excisoides total diterpene extract according to claim 1, 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.
3. the Isodon excisoides total diterpene extract that prepared by method described in claim 1 or 2 is preparing the application in antitumor drug.
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| 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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| 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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