CN101602740B - Method for extracting epigoitrin from isatis root - Google Patents
Method for extracting epigoitrin from isatis root Download PDFInfo
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Abstract
The invention relates to a method for extracting epigoitrin from isatis root with high extraction ratio, comprising the following steps: 1. isatis root medicinal material is crushed into coarse powder, 10-25 times of water or low-concentration ethanol is added in the coarse powder for being extracted at the temperature of 20-70 DEG C; 2. filtrate is decompressed and concentrated at the temperature of 40-70 DEG C for obtaining epigoitrin constituent; 3. concentrated solution passes through processed macroporous resin, and is washed by 5-12 times of column volume of water, and is washed by 2-5 times of column volume of water, and is washed by 30 percent to 50 percent of ethanol by mass concentration and then is collected; 4. ethanol eluent is decompressed and concentrated at the temperatureof 40-70 DEG C, thereby obtaining epigoitrin macroporous resin separated constituent; 5. the epigoitrin macroporous resin separated constituent is separated by column chromatography or high-efficiency industrial chromatographic column, thereby preparing into epigoitrin monomer. Compared with the prior art, the extraction efficiency of the epigoitrin is 2.4 times higher than that of the prior art;in addition, the period is short, the impurities are less, the post-processing is convenient, the raw material can be fully utilized, the cost can be shortened and economic benefit is improved.
Description
Technical field
The present invention relates to a kind of in the extraction process of pharmaceutically active ingredient, be specifically related to a kind of from Root of Indigowoad the method for high extraction ground extraction epi-Goitrin.
Background technology
Root of Indigowoad is Chinese traditional anti virus herb, dry root that records to cruciferae isatis Isatisindigotica Fort. of the Pharmacopoeia of the People's Republic of China (version in 2005), beginning is stated from Shennong's Herbal, effect with clearing heat and detoxicating, cool blood relieve sore throat is usually used in viral and bacterial infection disease clinically.Epi-Goitrin, English Epigoitrin by name is the alkaloid compound of a class sulfur-bearing, its structural formula is as follows:
The bibliographical information epi-Goitrin is that the main component of Root of Indigowoad is (referring to 1. bang profit, Wu Lijun, Li Hua, Deng. the chemical constitution study of Root of Indigowoad [J]. Shenyang Pharmaceutical University's journal, 2002,19 (2), 93-96. is Huang Q S 2., Yoshihiro K, Natori S.Isolation of 2-hydroxy-3-butenylthiocyanate, epigoitrin and adenosine from " Banlangen ", Isatis indigotica root[J] .Planta Medica, 1981,42 (3): 308-310. is Xu Li China 3., Huang Fang, Chen Ting, etc. the antiviral activity composition [J] in the Root of Indigowoad. Chinese natural drug, 2005,3 (6): 359-360.), and significant antiviral activity is arranged (referring to Xu Lihua, Huang Fang, Chen Ting, Deng. the antiviral activity composition [J] in the Root of Indigowoad. Chinese natural drug, 2005,3 (6): 359-360.).At present, the method that document and relevant patent are extracted epi-Goitrin has 30～95% alcohol reflux of 6～12 times of amounts, 8～12 times of water gagings decoct the method for extracting, (referring to: 1. yellow virtue, Xiong Yating, Xu Lihua, Deng. the antiviral ingredients epi-Goitrin is at pharmacokinetics in rats [J] in the different extracts of Root of Indigowoad. China Medicine University's journal, 2006,37 (6): 519-522. is Xu Li China 2.. method of extraction epi-Goitrin and uses thereof [P] from Root of Indigowoad. and Chinese patent: CN1666984,2005-09-14. 3. beam is prosperous vast, Feng Jiatao, Xu Qing, etc. a kind of method for separating and preparing of epi-Goitrin [P]. Chinese patent: CN101289429A, 2008-10-22.), these methods exist extraction yield low, length consuming time, the impurity that extracts is many, shortcomings such as aftertreatment is loaded down with trivial details.
Summary of the invention
The purpose of this invention is to provide a kind of from Root of Indigowoad high extraction ground extract the method for epi-Goitrin, this method can effectively be extracted epi-Goitrin, and the cycle is short, few, the convenient post-treatment of extraction impurity, makes full use of raw material to satisfy, the reduction input cost, the needs of increasing economic efficiency.
For achieving the above object, the technical solution used in the present invention is:
A kind of from Root of Indigowoad high extraction ground extract the method for epi-Goitrin, it is characterized in that step is as follows:
Step 1, exsiccant Root of Indigowoad pulverizing medicinal materials is become meal, the solvent that adds 10～25 times of weight extracts certain hour under 20～70 ℃ of temperature; Described solvent is the ethanol (1～50% ethanol) of water or lower concentration;
Step 2, under 40～70 ℃ of temperature, be evaporated to certain volume, obtain epi-Goitrin and extract component obtaining filtrate in the step 1;
Step 3, the macroporous resin of concentrated solution by having handled well that step 2 is obtained are earlier with the water flushing of 5～12 times of column volumes, then with the also collection of alcohol flushing of 2～5 times of column volumes, 30～50% mass concentrations;
Step 4, with alcohol eluen concentrating under reduced pressure under 40～70 ℃ of temperature that step 3 obtains, be epi-Goitrin macroporous resin separated portion;
Step 5, with the epi-Goitrin macroporous resin separated portion that obtains in the step 4, separate through column chromatography or efficient industrial chromatography post, prepare the epi-Goitrin monomer.
Among the above-mentioned preparation method, the Root of Indigowoad medicinal material was the meal of 10～40 mesh sieves in the step 1, and more excellent was 10～20 mesh sieves, and optimum was 20 mesh sieves;
Among the above-mentioned preparation method, extracting solvent in the step 1 is the ethanol of water or 1～50%, and optimum is a water;
Among the above-mentioned preparation method, it is 10～25 times of amounts that the solvent that adds in the step 1 is doubly measured, and more excellent is 15～20 times, and optimum is 20 times of amounts;
Among the above-mentioned preparation method, extracting temperature in the step 1 is 20～70 ℃, and more excellent is 40～70 ℃, and optimum is 60 ℃;
Among the above-mentioned preparation method, extraction time is 5～60min in the step 1, and more excellent is 5～20min, and optimum is 10min;
Among the above-mentioned preparation method, used extracting method can be that microwave-assisted extraction, supersound extraction or cold soaking stir extraction in the step 1;
Among the above-mentioned preparation method, extraction time is 1～4 time in the step 1, and more excellent is 1～2 time, and is optimum for extracting 1 time;
Among the above-mentioned preparation method, the concentrating under reduced pressure temperature is 40～70 ℃ in the step 2, and more excellent is 50～70 ℃, and optimum is 60 ℃;
Among the above-mentioned preparation method, be evaporated to certain volume in the step 2, its relative density is 1.05～1.20, and more excellent is 1.05～1.10, and optimum is 1.10;
Among the above-mentioned preparation method, the big pore resin is D101, AB-8, resins such as LSA-10, HPD100 commonly used in the step 3, and more excellent is D101, LSA-10, and optimum is D101;
Among the above-mentioned preparation method, earlier with the water flushing of 5～12 times of column volumes, more excellent is 8～10 times of column volumes in the step 3, and optimum is 8 times of column volumes;
Among the above-mentioned preparation method, with 30～50% alcohol flushings of 2～5 times of column volumes, more excellent is 30～40% alcohol flushings of 2～3 times of column volumes in the step 3, and optimum is 1 times of column volume 30% alcohol flushing;
Among the above-mentioned preparation method, the concentrating under reduced pressure temperature is 40～70 ℃ in the step 4, and more excellent is 50～70 ℃, and optimum is 60 ℃.
The present inventor finds that under study for action it is remarkable to the extraction efficiency influence of epi-Goitrin to extract temperature, and in the disclosed prior art of former document and patent, to the extraction temperature of epi-Goitrin all higher (for example, adopting 100 ℃ decoction).Temperature that the present invention is clear and definite is the key factor to the influence of epi-Goitrin extraction yield, and has selected best extraction temperature and technology.
Adopt the present invention to extract epi-Goitrin and have following characteristics:
1, extraction efficiency height.
1. the assay of epi-Goitrin in the Root of Indigowoad medicinal material
Chromatographic condition: ZORBAX SB-C18 chromatographic column (4.6mm * 150mm, 5 μ m), moving phase are acetonitrile-(4.0mL phosphoric acid+0.3mL triethylamine+500mL water)=8.5: 91.5; Flow velocity is 0.7mL/min, and the detection wavelength is 245nm, and sample size is 20 μ L, and column temperature is 30 ℃.
Sample treatment: get the about 0.2g of Root of Indigowoad medicinal powder (crossing 40 mesh sieves), the accurate title, decide, and be triplicate, put respectively in the 50mL tool plug Erlenmeyer flask, add water 20mL, weigh, supersound extraction under the room temperature condition (power 250W, frequency 20KHz) 60min takes out, put cold, weigh, water is supplied bodies lost weight again, 0.45 μ m filtering with microporous membrane, discard filtrate just, get subsequent filtrate as supplying test agent.
Measurement result: HPLC detects, and epi-Goitrin content is 2566.40 μ g/g in the calculating medicinal material.
2. the comparison of extracting method extraction efficiency in the present invention and document and the patent
Extracting method extracts sample in document and the patent:
Extracting method 1: Root of Indigowoad medicinal material coarse powder 10g, the accurate title, decide, use 30% ethanol, 70% ethanol, 95% alcohol reflux 2 times of 6 times of amounts respectively, united extraction liquid, 60 ℃ are evaporated to dried, wash out with coordinative solvent respectively, be settled in the volumetric flask of 50mL, 0.45 μ m filtering with microporous membrane discards filtrate just, get subsequent filtrate as for test agent, standby.
Extracting method 2: Root of Indigowoad medicinal material coarse powder 10g, the accurate title, decide, use 30% ethanol, 70% ethanol, 95% alcohol reflux 2 times of 12 times of amounts respectively, united extraction liquid, 60 ℃ are evaporated to dried, wash out with coordinative solvent respectively, be settled in the volumetric flask of 50mL, 0.45 μ m filtering with microporous membrane discards filtrate just, get subsequent filtrate as for test agent, standby.
Extracting method 3: Root of Indigowoad medicinal material coarse powder 10g, accurate claim surely, add the water boiling and extraction 2 times of 8 times of its weight, each 1h, united extraction liquid, 60 ℃ are evaporated to proper volume, move in the volumetric flask of 50mL, and wash container with water, be settled to scale at last, 0.45 μ m filtering with microporous membrane discards filtrate just, get subsequent filtrate as for test agent, standby.
Extracting method 4: Root of Indigowoad medicinal material coarse powder 10g, accurate claim surely, add the water boiling and extraction 3 times of 8 times of its weight, each 3h, united extraction liquid, 60 ℃ are evaporated to proper volume, move in the volumetric flask of 50mL, and wash container with water, be settled to scale at last, 0.45 μ m filtering with microporous membrane discards filtrate just, get subsequent filtrate as for test agent, standby.
Extracting method 5: Root of Indigowoad medicinal material coarse powder 10g, accurate claim surely, add the water boiling and extraction 2 times of 12 times of its weight, each 1h, united extraction liquid, 60 ℃ are evaporated to proper volume, move in the volumetric flask of 50mL, and wash container with water, be settled to scale at last, 0.45 μ m filtering with microporous membrane discards filtrate just, get subsequent filtrate as for test agent, standby.
Extracting method 6: Root of Indigowoad medicinal material coarse powder 10g, accurate claim surely, add the water boiling and extraction 3 times of 12 times of its weight, each 3h, united extraction liquid, 60 ℃ are evaporated to proper volume, move in the volumetric flask of 50mL, and wash container with water, be settled to scale at last, 0.45 μ m filtering with microporous membrane discards filtrate just, get subsequent filtrate as for test agent, standby.
Extracting method of the present invention:
Root of Indigowoad medicinal material coarse powder 10g, the accurate title, decide, adopt the used method of the present invention to extract, extracting solution is evaporated to proper volume for 60 ℃, moves in the volumetric flask of 50mL, and use the coordinative solvent washing container, be settled to scale at last, 0.45 μ m filtering with microporous membrane discards filtrate just, get subsequent filtrate as for test agent, standby.
HPLC detects, and calculates and extracts the amount of epi-Goitrin, and the total extraction yield of epi-Goitrin in the 10g medicinal material is arranged.The results are shown in Table 1.
Extracting method compares (n=3) among the extraction yield of the method extraction epi-Goitrin of table 1 prior art and the present invention
Content extraction yield in the medicinal material
The amount that the extracting method extraction solvent extracts (mg)
(mg) (％)
Extracting method 1 30% ethanol 2.15 25.72 8.36
Extracting method 1 70% ethanol 1.19 25.97 4.58
Extracting method 1 95% ethanol 0.77 26.12 2.95
Extracting method 2 30% ethanol 2.20 25.94 8.48
Extracting method 2 70% ethanol 1.32 26.26 5.03
Extracting method 2 95% ethanol 0.83 25.68 3.23
Extracting method 3 water 8.78 25.87 33.94
Extracting method 4 water 9.21 26.05 35.36
Extracting method 5 water 9.57 25.92 36.92
Extracting method 6 water 10.25 26.33 38.93
Extracting method water of the present invention or low-concentration ethanol 24.28 25.84 93.96
By the result as can be known, adopt the used method of the present invention to extract epi-Goitrin, its extraction efficiency is higher more than 2.4 times than extraction yield (38.93%) the highest in existing document and the patent.
2, the impurity that extracts is few.The used extracting method of the present invention extraction time weak point, it is low to extract temperature, so the impurity that extracts is few, need not carries out alcohol precipitation and handle, and subsequent purification is convenient.
3, the cycle is shorter.The used extracting method technology of the present invention is simple, and extraction time is short, and it is shorter to be crushed to extraction, purifying cycle from crude drug.
4, suitability for industrialized production preferably.The present invention can extract the epi-Goitrin in the Root of Indigowoad more complete, has made full use of raw material, has reduced input cost; Technology of the present invention is very easy to realize stdn in addition, and automatization is suitable for carrying out industrialization scale operation.
Embodiment
Further describe the present invention by following example, but should notice that scope of the present invention is not subjected to any restriction of these examples.
Embodiment 1: take by weighing Root of Indigowoad medicinal material coarse powder (crossing 20 mesh sieves) 50g, the 60 ℃ of microwave-assisted of water that add 20 times of amounts extract 10min, filter, get subsequent filtrate dilution back as supplying test agent, HPLC detects the concentration of epi-Goitrin, the amount that calculating extracts epi-Goitrin is 118.49mg, and calculating extraction yield by following formula is 92.34%.
Formula (1)
Embodiment 2: take by weighing Root of Indigowoad medicinal material coarse powder 200g (crossing 20 mesh sieves), the 60 ℃ of microwave-assisted of water that add 20 times of amounts extract 10min, filter, get subsequent filtrate dilution back as supplying test agent, HPLC detects the concentration of epi-Goitrin, the amount that calculating extracts epi-Goitrin is 478.12mg, and calculating extraction yield by following formula is 93.13%.
Embodiment 3: take by weighing Root of Indigowoad medicinal material coarse powder 500g (crossing 20 mesh sieves), the 60 ℃ of microwave-assisted of water that add 20 times of amounts extract 10min, filter, get subsequent filtrate dilution back as supplying test agent, HPLC detects the concentration of epi-Goitrin, the amount that calculating extracts epi-Goitrin is 1196.22mg, and calculating extraction yield by following formula is 93.20%.
Embodiment 4: take by weighing Root of Indigowoad medicinal material coarse powder 5kg (crossing 20 mesh sieves), the 60 ℃ of microwave-assisted of water that add 20 times of amounts extract 10min, filter, get subsequent filtrate dilution back as supplying test agent, HPLC detects the concentration of epi-Goitrin, the amount that calculating extracts epi-Goitrin is 11888.85mg, and calculating extraction yield by following formula is 92.64%.
Embodiment 5: it is 1.10g/mL that microwave extraction liquid is concentrated into relative density, by the D101 macroporous adsorbent resin of having handled well, and sample on 1/3 column volume, with the water flushing of 8 times of column volumes, flow velocity is 3mL/min earlier; Use 30% ethanol elution of 2 times of column volumes again, collect alcohol eluen, 60 ℃ of concentrating under reduced pressure, vacuum-drying promptly get epi-Goitrin purifying position, and the content of HPLC detection epi-Goitrin is 34.18%.
Embodiment 6: it is 1.10g/mL that microwave extraction liquid is concentrated into relative density, by the D101 macroporous adsorbent resin of having handled well, and sample on 1/3 column volume, with the water flushing of 8 times of column volumes, flow velocity is 3mL/min earlier; Use 30% ethanol elution of 2 times of column volumes again, collect alcohol eluen, 60 ℃ of concentrating under reduced pressure, vacuum-drying promptly get epi-Goitrin purifying position, and the content of HPLC detection epi-Goitrin is 35.47%.
Embodiment 7: it is 1.10g/mL that microwave extraction liquid is concentrated into relative density, by the D101 macroporous adsorbent resin of having handled well, and sample on 1/3 column volume, with the water flushing of 8 times of column volumes, flow velocity is 3mL/min earlier; Use 30% ethanol elution of 2 times of column volumes again, collect alcohol eluen, 60 ℃ of concentrating under reduced pressure, vacuum-drying promptly get epi-Goitrin purifying position, and the content of HPLC detection epi-Goitrin is 34.60%.
Embodiment 8, and is substantially the same manner as Example 1, but following change is arranged:
In the step 1, used extracting method is a supersound extraction;
Described Root of Indigowoad medicinal material was the meal of 10 mesh sieves; Described extraction solvent is the ethanol of 50% mass concentration; It is 15 times that the solvent of described adding is doubly measured; Described extraction temperature is 40 ℃; Described extraction time is 60min;
In the step 2, described concentrating under reduced pressure temperature is 50 ℃; The described certain volume that is evaporated to is meant: being concentrated into its relative density is 1.05;
In the step 3, the water yield of flushing macroporous resin is 10 times of column volumes; The amount of alcohol of flushing macroporous resin is 3 times of column volumes, and mass concentration is 40%;
The concentrating under reduced pressure temperature is 50 ℃ in the step 4.
Embodiment 9, and is substantially the same manner as Example 1, but following change is arranged:
In the step 1, used extracting method is that cold soaking stirs extraction;
Described extraction solvent is the ethanol of 30% mass concentration; It is 25 times of amounts that the solvent of described adding is doubly measured; Described extraction temperature is 70 ℃; Described extraction time is 20min; Described extraction time is 4 times;
In the step 2, described concentrating under reduced pressure temperature is 70 ℃; The described certain volume that is evaporated to is meant: being concentrated into its relative density is 1.05;
In the step 3, the water yield of flushing macroporous resin is 12 times of column volumes; The amount of alcohol of flushing macroporous resin is 3 times of column volumes, and mass concentration is 40%;
The concentrating under reduced pressure temperature is for being 40 ℃ in the step 4.
Embodiment 10, and is substantially the same manner as Example 1, but following change is arranged:
In the step 1, the solvent of described adding is a water; It is 10 times of amounts that the solvent of described adding is doubly measured; Described extraction temperature is 20 ℃; Described extraction time is 10min; Described extraction time is 2 times;
In the step 2, described concentrating under reduced pressure temperature is 40 ℃; The described certain volume that is evaporated to is meant: being concentrated into its relative density is 1.05;
In the step 3, the amount of alcohol of flushing macroporous resin is 3 times of column volumes, and mass concentration is 50%;
The concentrating under reduced pressure temperature is for being 70 ℃ in the step 4.
Embodiment 11, and is substantially the same manner as Example 1, but following change is arranged:
In the step 1, the solvent of described adding is a water; It is 10 times of amounts that the solvent of described adding is doubly measured; Described extraction time is 5min; Described extraction time is 1 time;
In the step 2, the described certain volume that is evaporated to is meant: being concentrated into its relative density is 1.20;
In the step 3, the amount of alcohol of flushing macroporous resin is 5 times of column volumes, and mass concentration is 30%.
More than each embodiment big pore resin can be among D101, AB-8, LSA-10 or the HPD100 any one.
Embodiment 12, and is substantially the same manner as Example 1, but following change is arranged:
In the step 1, described extraction solvent is the ethanol of 1% mass concentration.
Claims (4)
- One kind from Root of Indigowoad high extraction ground extract the method for epi-Goitrin, it is characterized in that step is as follows:Step 1, exsiccant Root of Indigowoad pulverizing medicinal materials is become meal, the solvent that adds 10～25 times of weight extracts certain hour under 20～70 ℃ of temperature; Described solvent is the ethanol of water or 1%～50% mass concentration, and used extracting method is that microwave-assisted extracts;Step 2, with the extracting solution that obtains in the step 1, filter, filtrate is evaporated to certain volume under 40～70 ℃ of temperature, obtain epi-Goitrin and extract component;Step 3, the macroporous resin of concentrated solution by having handled well that step 2 is obtained are earlier with the water flushing of 5～12 times of column volumes, then with the also collection of alcohol flushing of 2～5 times of column volumes, 30%～50% mass concentration;Step 4, with alcohol eluen concentrating under reduced pressure under 40～70 ℃ of temperature that step 3 obtains, be epi-Goitrin macroporous resin separated portion;Step 5, with the epi-Goitrin macroporous resin separated portion that obtains in the step 4, separate through column chromatography or efficient industrial chromatography post, prepare the epi-Goitrin monomer.
- 2. according to claim 1 from Root of Indigowoad high extraction ground extract the method method of epi-Goitrin, it is characterized in that, in the step 1,Described extraction solvent is a water;It is 15～20 times that the solvent of described adding is doubly measured;Described extraction temperature is 40～70 ℃;Described extraction time is 5～60min;In the step 2,Described concentrating under reduced pressure temperature is 50～70 ℃;The described certain volume that is evaporated to is meant: being concentrated into its relative density is 1.05～1.20;In the step 3,The big pore resin is selected from: D101, AB-8, LSA-10, HPD100;The water yield of flushing macroporous resin is 8～10 times of column volumes;The amount of alcohol of flushing macroporous resin is 2～3 times of column volumes, and mass concentration is 30～40%;The concentrating under reduced pressure temperature is 50～70 ℃ in the step 4.
- 3. according to claim 1 from Root of Indigowoad high extraction ground extract the method for epi-Goitrin, it is characterized in that, in the step 1,It is 20 times of amounts that the solvent of described adding is doubly measured;Described extraction temperature is 60 ℃;Described extraction time is 5～20min;Extraction time is 1～4 time;In the step 2,Described concentrating under reduced pressure temperature is 60 ℃;The described certain volume that is evaporated to is meant: being concentrated into its relative density is 1.05～1.10;In the step 3,The big pore resin is selected from D101, LSA-10;The water yield of flushing macroporous resin is 8 times of column volumes;The concentrating under reduced pressure temperature is 60 ℃ in the step 4.
- 4. according to claim 3 from Root of Indigowoad high extraction ground extract the method method of epi-Goitrin, it is characterized in that, in the step 1,Described extraction time is 10min;Described extraction time is 1～2 time;In the step 2,The described certain volume that is evaporated to is meant: being concentrated into its relative density is 1.10;In the step 3,The big pore resin is D101.
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| CN108409679A (en) * | 2018-04-19 | 2018-08-17 | 深圳极致本草生物医药有限公司 | A method of extracting epigoitrin from Radix Isatidis |
| CN109010407A (en) * | 2018-09-11 | 2018-12-18 | 华润三九（雅安）药业有限公司 | A kind of Radix Isatidis syrup and preparation method thereof |
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