CN103319481B - Extracting process of swainsonine in astragalus strictus - Google Patents
Extracting process of swainsonine in astragalus strictus Download PDFInfo
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- CN103319481B CN103319481B CN201310281344.XA CN201310281344A CN103319481B CN 103319481 B CN103319481 B CN 103319481B CN 201310281344 A CN201310281344 A CN 201310281344A CN 103319481 B CN103319481 B CN 103319481B
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Abstract
The invention provides an extracting process of swainsonine in astragalus strictus. The extracting process comprises the following steps of: directly crushing by using roots and/or stems of astragalus strictus as materials, adding petroleum ether to form a solution; ultrasonically degreasing the solution after 3-5 hours, and recycling petroleum ether; controlling the moisture content of the ultrasonically degreased materials to 30%-70%; using methanol with concentration of 85%-90% as a solvent, soaking for 0.5 hour-1 hour to carry out microwave extraction for 35 seconds-40 seconds at the microwave output power of 650 W-700W to obtain an extricated solution, wherein the weight volume ratio of the materials to the methanol is 1:45g/ml-50g/ml; evaporating the extracted solution for 25 minutes-30 minutes under the normal pressure at 130 DEG C-140 DEG C, and evaporating for 15 minutes-25 minutes by reducing the pressure to 0.3 MP-0.5MP to obtain a swainsonine pure product. The extracting process of the swainsonine in the astragalus strictus can be used for realizing further improving the extracting efficiency of the swainsonine on the basis of shortening the extracting time.
Description
Technical field
The present invention relates to a kind of from medicinal plant the technique of extracting effective components, more particularly, the present invention relates to the extraction process of trihydroxyoctahydroindolizidine in a kind of Astragalus strictus, belong to natural product chemistry field.
Background technology
Astragalus strictus (Astragalus strictus Grah) is pulse family Astragalus perennial plant.In various places, Tibet, all have distribution, vertical distribution is in 2900～4600 meters of height above sea level.Root is sturdy, wooden.Stem is upright, high 15-30 centimetre.Astragalus strictus happiness is wet cold-resistant, drought-enduring, salt affected soil is had to stronger adaptive faculty, in addition well developed root system, seed quantity is large, reproductivity and aggressiveness are strong, annual have large quantities of Livestock poisoneds dead in the pastoral area of its intensive growth, caused serious loss to local herdsman, is one of the most serious poisonous weeds of China pasturing area in Tibet harm.
Trihydroxyoctahydroindolizidine (swainsonine) is the main toxic ingredient in Astragalus strictus.Trihydroxyoctahydroindolizidine is that in a kind of indoles of large polarity, Alkaloid is stung in west, because of can be consumingly and suppress specifically lysosome
αthe sweet enzyme I of-seminose and Golgi apparatus
αthe activity of the sweet enzyme II of-seminose, thus the expression of cell surface glycoprotein suppressed, thus suppressed growth and the transfer of tumour.Therefore trihydroxyoctahydroindolizidine has obtained domestic and international researchist's concern as a kind of brand-new cancer therapy drug in recent years, and the standby medicine screening as antitumour drug.
In prior art, the extraction process of trihydroxyoctahydroindolizidine mainly contains following several:
1, State Intellectual Property Office in 2007.10.10, to disclose an application number be 200710017844.7, name is called the patent of invention of " a kind of novel method of extracting trihydroxyoctahydroindolizidine from loco weed ", so described in patent, effective ingredients in plant extracts conventional traditional method decocting method, THROUGH METHOD, reflux extraction, continuous circumfluence extraction method etc., but these methods all exist the shortcomings such as effective component extraction rate is low, energy consumption is high, extraction time is long.
2, State Intellectual Property Office in 2003.02.12, to disclose an application number be 02114590.3, name is called the patent of invention of " purifying technique of trihydroxyoctahydroindolizidine in loco weed ", the subject matter that this patent exists is:
2.1, adopted equally traditional THROUGH METHOD, reflux extraction, continuous circumfluence extraction method etc., there is equally the shortcomings such as effective component extraction rate is low, energy consumption is high, extraction time is long.
2.2, this technology the first step is extracted organic total composition in loco weed grass meal, adopts repeatedly cold soaking to extract 4-6 times, and the time of each cold soaking is 7 days, is only this step, just needs about one month consuming time, and extraction time is oversize.
2.3, adopt the extraction yield of trihydroxyoctahydroindolizidine sterling after this technology to only have about 0.0009%-0.0015%.Therefore, this technology extraction time is oversize, and extraction yield is low, is unsuitable for industrial application.
3, State Intellectual Property Office in 2012.05.02, to disclose an application number be 201110420357.1, name is called the patent of invention of " the microwave-assisted extraction process of trihydroxyoctahydroindolizidine in a kind of Astragalus strictus ", although adopted microwave-assisted extraction in this technology, larger raising the extraction yield of trihydroxyoctahydroindolizidine, but the subject matter that this patent also exists is:
3.1, ultrasonic degreasing proportion is 30～45KHz, and this also belongs to conventional range of frequency, but when this frequency is when having added the Astragalus strictus of sherwood oil, because Astragalus strictus root is sturdy, wooden, easily affect cavatition, thereby reduce the extraction yield of trihydroxyoctahydroindolizidine.
3.2, carry out immediately ultrasonic degreasing after adding sherwood oil in the Astragalus strictus raw material after pulverizing, sherwood oil can not infiltrate Astragalus strictus organization internal completely, affects the extraction of effective constituent, thereby also can reduce the extraction yield of trihydroxyoctahydroindolizidine.
3.3, ultrasonic degreasing temperature is 30～45 ℃, during for Astragalus strictus, and excess Temperature, unfavorable to the generation of cavitation, and bubble has strengthened shock absorption when closed and cavitation is weakened, and also can reduce the extraction yield of trihydroxyoctahydroindolizidine.
3.4, employing be complete stool Astragalus strictus, the ability that causes absorbing microwave due to structural difference is different, causes microwave extracting efficiency notable difference, thereby affects the extraction yield of trihydroxyoctahydroindolizidine.
3.5, it dries Astragalus strictus open air under natural condition, not only needs time of growing, and has reduced the water ratio of Astragalus strictus, thereby causes microwave extraction poor effect, has reduced the extraction yield of trihydroxyoctahydroindolizidine.
3.6, the weightmeasurement ratio of Astragalus strictus raw material and methyl alcohol is 1:10～20g/ml, and the mutually intersubjective mass transfer force of solid, liquid is less, thereby affects microwave extraction effect.
4, the outstanding rich Master's thesis full-text database of the China of the 05th phase in 2007 (master) agricultural science and technology is collected and is disclosed a kind of " trihydroxyoctahydroindolizidine extracting method in loco weed ", first utilize the ultrasonic cleaner of 40KHz to process loco weed powder, the technical process of setting up batch extracting trihydroxyoctahydroindolizidine; Apply subsequently the ultrasonic circulating extracting machine of 20KHz and process loco weed powder, but equally also there are the following problems:
4.1, this technology has adopted traditional have decocting method, THROUGH METHOD, reflux extraction, continuous circumfluence extraction method etc. equally, has equally the shortcomings such as effective component extraction rate is low, energy consumption is high, extraction time is long.
4.2, ultrasonic wave proportion is 20～40KHz, equally also belongs to conventional range of frequency, but when if this frequency is when having added the Astragalus strictus of sherwood oil, because Astragalus strictus root is sturdy, wooden, easily affect cavatition, thereby reduce the extraction yield of trihydroxyoctahydroindolizidine.
Summary of the invention
The object of the invention is to overcome the problems referred to above that the extraction process of existing trihydroxyoctahydroindolizidine exists, the extraction process of trihydroxyoctahydroindolizidine in a kind of Astragalus strictus is provided, the present invention, shortening on the basis of extraction time, realizes the extraction yield that further improves trihydroxyoctahydroindolizidine.
In order to realize foregoing invention object, its concrete technical scheme is as follows:
In Astragalus strictus, an extraction process for trihydroxyoctahydroindolizidine, is characterized in that, comprises following processing step:
A, root and/or the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 70～80 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:30～1:40g/ml;
B, after 3-5 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 55～60KHz, and temperature is 20～25 ℃, and the time is 15～25min;
C, by the raw material moisture control after ultrasonic degreasing 30-70%;
D, use the methyl alcohol of 85-90% concentration as solvent again, soaking after 0.5-1 hour is 650～700W at microwave output power, carries out microwave extraction 35～40s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:45～50g/ml;
E, by extracting solution under 130-140 degree, first atmospheric evaporation 25-30min, then be decompressed to 0.3-0.5MP evaporation, 15-25min, obtains trihydroxyoctahydroindolizidine sterling.
The present invention also comprises the step of sterilizing, and raw material is adopted to ultraviolet disinfection 10-20 minutes, more directly pulverizes.
Preferred technique is:
A, root and the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 73～76 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:32～1:36g/ml;
B, after 3.5-4.5 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 58KHz, and temperature is 23-25 ℃, and the time is 20-23min;
C, by the raw material moisture control after ultrasonic degreasing 30-40%;
D, use the methyl alcohol of 88% concentration as solvent again, soaking after 0.5 hour is 650 at microwave output power, carries out microwave extraction 37～39s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:47～49g/ml;
E, by extracting solution under 135 degree, first atmospheric evaporation 27-29min, then be decompressed to 0.3-0.4MP evaporation, 15-20min, obtains trihydroxyoctahydroindolizidine sterling.
Optimised process is:
A, root and the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 74 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:32g/ml;
B, after 3.5 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 58KHz, and temperature is 23 ℃, and the time is 20min;
C, by the raw material moisture control after ultrasonic degreasing 35%;
D, use the methyl alcohol of 88% concentration as solvent again, soaking after 0.5 hour is 650 at microwave output power, carries out microwave extraction 37s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:49g/ml;
E, by extracting solution under 135 degree, first atmospheric evaporation 29min, then be decompressed to 0.3MP evaporation 18min, obtains trihydroxyoctahydroindolizidine sterling.
In raw material after described a step is pulverized, after the raw material pulverizing of 70% mass ratio, cross 75-80 mesh sieves, after the raw material pulverizing of 30% mass ratio, cross 70-74 mesh sieves.
In described a step, the root of Astragalus strictus of take is raw material, after directly pulverizing, crosses 75～80 mesh sieves, in the raw material after pulverizing, adds sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:35～1:40g/ml.
In described a step, the stem of Astragalus strictus of take is raw material, after directly pulverizing, crosses 70～73 mesh sieves, in the raw material after pulverizing, adds sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:32～1:36g/ml.
In described b step, constant-temperature ultrasonic degreasing 5-10 min at 20-22 ℃, then at 23-25 ℃ constant-temperature ultrasonic degreasing 10-15 min.
In described c step, by 70% raw material moisture control after ultrasonic degreasing 30-35%, by 30% raw material moisture control after ultrasonic degreasing 60-70%.
The useful technique effect that the present invention brings:
One, in the present invention, root and the stem of Astragalus strictus of take is raw material, and because the textural difference of root and stem is less, the ability that makes to absorb microwave is basic identical, makes microwave extracting efficiency there is no notable difference, thereby has guaranteed the extraction yield of trihydroxyoctahydroindolizidine in Astragalus strictus; After directly pulverizing, cross 70～80 mesh sieves, all not identical with prior art, existing or pulverized 30-50 mesh sieves, or do not pulverize, the present invention is directed to after the root of Astragalus strictus and stem are directly pulverized and cross 70～80 mesh sieves, this order number has not only guaranteed microwave extraction efficiency, and make extracting solution limpid, if be greater than this order number, affect microwave extraction efficiency, be less than this order number, cause filtration difficulty and extracting solution muddy; In the raw material after pulverizing, add sherwood oil to form solution, the weightmeasurement ratio of raw material and sherwood oil is 1:30～1:40g/ml, root and stem for Astragalus strictus adopt this ratio to make degreasing rate up to 67% left and right, if be less than this ratio, degreasing rate obviously reduces, if higher than this ratio, degreasing rate does not have considerable change, increased cost.
Two, in the present invention, after 3-5 hours, solution is carried out to ultrasonic degreasing, now sherwood oil has been dipped to the heart by raw material, and be conducive to sherwood oil and infiltrate raw tissue inside, thereby by extracts active ingredients out, if the time is too short, the impact of extraction efficiency is larger, and overlong time can increase cost; Reclaim sherwood oil, can reuse, reduced cost; Ultrasonic degreasing frequency is 55～60KHz, this for the specific root for Astragalus strictus and stem be raw material, different from existing ultrasonic degreasing frequency, if frequency is too high or too low, all can cavitation, thus affect degreasing effect; Temperature is 20～25 ℃, time is 15～25min, within the scope of this temperature and time, for Astragalus strictus root and this specific solution of stem, generation to cavitation is the most favourable, and during excess Temperature, in bubble, vapour pressure increases, bubble has strengthened shock absorption when closed and cavitation is weakened, and can farthest reduce oil-soluble impurities.
Three, in the present invention, by the raw material moisture control after ultrasonic degreasing 60-70%, for this specific raw material of Astragalus strictus, this water ratio can accelerate the infiltration of methyl alcohol to raw material when microwave extraction, improve extraction yield, if water ratio is too low or too high, affect extraction effect; If carry out moisture control before ultrasonic degreasing, can change water ratio during ultrasonic degreasing, therefore must after ultrasonic degreasing, control water ratio.
Four, in the present invention, use again the methyl alcohol of 85-90% concentration as solvent, guarantee microwave extraction rate, root and stem for Astragalus strictus, higher or lower than this concentration, extraction yield all can decline, if adopt 70-80% concentration of the prior art, test shows, in this concentration range, microwave extraction rate obviously declines, therefore adopting the methyl alcohol of 85-90% concentration is the specific root for Astragalus strictus and stem, if be applied to the extraction of trihydroxyoctahydroindolizidine in other loco weed, adopts the extraction yield of microwave extraction lower, soaking after 0.5-1 hour is 650～700W at microwave output power, owing to having carried out moisture control, make methyl alcohol can be in the short period of time by raw material soaking to the heart thoroughly, and for Astragalus strictus root and this specific solution of stem, and carried out moisture control, therefore adopt this specific microwave output power, extraction efficiency is the highest, the general the highest 600W of microwave output power that adopts in prior art, if higher than this power, effective component extraction rate can decline, but be Astragalus strictus root and this specific solution of stem of having controlled water ratio due to what the present invention is directed to, adopt the output rating of this scope that extraction yield is significantly improved, carry out microwave extraction 35～40s, obtain extracting solution, the weightmeasurement ratio of raw material and methyl alcohol is 1:45～50g/ml, because the methyl alcohol in the application can be recycled, adopts this specific solid-to-liquid ratio, all different from existing microwave extraction, the general solid-to-liquid ratio of existing microwave extraction technology is during higher than 1:40, and extracted amount does not have amplification, and the present invention is directed to Astragalus strictus root and this specific solution of stem, not only there is not the problem of subsequent disposal, and make extracted amount be line style growth.
Five, the present invention by extracting solution 130-140 degree under, first atmospheric evaporation 25-30min, because the present invention is the purification of carrying out after microwave extraction, therefore adopt this temperature and time not only can removal of impurities, and make the loss reduction of trihydroxyoctahydroindolizidine, lower than this temperature and time, impurity-eliminating effect is not good, trihydroxyoctahydroindolizidine sterling can not reach more than 99%, be decompressed to again 0.3-0.5MP evaporation, 15-25min, obtain trihydroxyoctahydroindolizidine sterling, this step is in conjunction with whole technical process, the trihydroxyoctahydroindolizidine obtaining does not need to purify again, purity can reach more than 99%, and because trihydroxyoctahydroindolizidine easily evaporates, adopt the first normal pressure method of reduction vaporization again, can reduce the loss of trihydroxyoctahydroindolizidine.
Six, the present invention carries out moisture control after ultrasonic degreasing, carry out again microwave extraction, must be in strict accordance with this technical process, the change of any step all can cause the purity drop of extraction yield and trihydroxyoctahydroindolizidine sterling, all different from prior art, the specific root for Astragalus strictus of technical process of the present invention and processing parameter and stem, and be not suitable for Astragalus strictus complete stool or other similar loco weed trihydroxyoctahydroindolizidine extracting method, especially processing parameter is all different from prior art, the parameter of for example ultrasonic degreasing parameter and microwave extraction, parameter in whole technique, an if parameter change, capital causes the change of processing step and other processing parameter, and can affect extraction effect and the purity of trihydroxyoctahydroindolizidine, thereby these parameters are that those skilled in the art can not be tested and be drawn by limited number of time, if be applied to complete stool or similarly loco weed trihydroxyoctahydroindolizidine extraction, extraction effect and the purity of trihydroxyoctahydroindolizidine all can not reach requirement.
Seven, the present invention also comprises the step of sterilizing, raw material is adopted to ultraviolet disinfection 10-20 minutes, directly pulverize again, adopt this step, the purity of trihydroxyoctahydroindolizidine can be brought up to 99.7 left and right from 99.1% left and right, obtain the trihydroxyoctahydroindolizidine that purity is higher, experimental results show that, when this method is applied to other loco weed trihydroxyoctahydroindolizidine extraction, purity is not had a significant effect.
Eight, in the raw material after a step pulverizing of the present invention, after the raw material pulverizing of 70% mass ratio, cross 75-80 mesh sieves, after the raw material pulverizing of 30% mass ratio, cross 70-74 mesh sieves, adopt this step at the solution that adds sherwood oil to form and add in the solution of the formation of methanol, can increase the frictional force between feed particles, being also conducive to solvent by the extremely saturating heart of raw material soaking, and adopt the raw material grain of different-grain diameter, can make extracting solution limpider, thereby improve degreasing and extraction efficiency, reduce foreign matter content.
Nine, in a step of the present invention, the root of Astragalus strictus of take is raw material, after directly pulverizing, crosses 75～80 mesh sieves, and while being raw material for the root of Astragalus strictus, this order number is convenient to filter and is guaranteed that extracting solution is limpid; In the raw material after pulverizing, add sherwood oil to form solution, the weightmeasurement ratio of raw material and sherwood oil is 1:35～1:40g/ml, and this solid-to-liquid ratio makes degreasing rate up to more than 70% for the root of Astragalus strictus, thus raising extraction yield.
Ten, in a step of the present invention, the stem of Astragalus strictus of take is raw material, after directly pulverizing, crosses 70～73 mesh sieves, and while being raw material for the stem of Astragalus strictus, this order number is convenient to filter and is guaranteed that extracting solution is limpid; In the raw material after pulverizing, add sherwood oil to form solution, the weightmeasurement ratio of raw material and sherwood oil is 1:32～1:36g/ml.
11, in b step of the present invention, constant-temperature ultrasonic degreasing 5-10 min at 20-22 ℃, constant-temperature ultrasonic degreasing 10-15 min at 23-25 ℃ again, adopt two different temperature to carry out constant-temperature ultrasonic degreasing, can obviously improve degreasing rate, further reduce oil-soluble impurities, with first normal pressure again reduction vaporization be combined, the purity of trihydroxyoctahydroindolizidine is reached more than 99%.
12, in c step of the present invention, 70% raw material moisture control after ultrasonic degreasing, 60-65%, 66-70%, is adopted to the raw material of different water cut by 30% raw material moisture control after ultrasonic degreasing, once can extract completely, improve the efficiency that absorbs micro-wave energy.
Embodiment
Embodiment 1
An extraction process for trihydroxyoctahydroindolizidine in Astragalus strictus, comprises following processing step:
A, root and the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 70 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:30g/ml;
B, after 3 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 55KHz, and temperature is 20 ℃, and the time is 15min;
C, by the raw material moisture control after ultrasonic degreasing 30%;
D, use the methyl alcohol of 85% concentration as solvent again, soaking after 0.5 hour is 650W at microwave output power, carries out microwave extraction 35s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:45g/ml;
E, by extracting solution under 130 degree, first atmospheric evaporation 25min, then be decompressed to 0.3MP evaporation 15min, obtains trihydroxyoctahydroindolizidine sterling.
The trihydroxyoctahydroindolizidine that adopts above-mentioned technique to extract can reach following index:
As seen from the above table, the These parameters of the trihydroxyoctahydroindolizidine sterling that the present invention extracts is all better than prior art, especially moisture content index and extraction yield.
Embodiment 2
An extraction process for trihydroxyoctahydroindolizidine in Astragalus strictus, comprises following processing step:
A, root and the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 80 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:40g/ml;
B, after 5 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 60KHz, and temperature is 25 ℃, and the time is 25min;
C, by the raw material moisture control after ultrasonic degreasing 70%;
D, use the methyl alcohol of 90% concentration as solvent again, soaking after 1 hour is 700W at microwave output power, carries out microwave extraction 40s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 50g/ml;
E, by extracting solution under 140 degree, first atmospheric evaporation 30min, then be decompressed to 0.5MP evaporation 25min, obtains trihydroxyoctahydroindolizidine sterling.
The trihydroxyoctahydroindolizidine that adopts above-mentioned technique to extract can reach following index:
As seen from the above table, the These parameters of the trihydroxyoctahydroindolizidine sterling that the present invention extracts is all better than prior art, especially purity index and extraction yield.
Embodiment 3
An extraction process for trihydroxyoctahydroindolizidine in Astragalus strictus, comprises following processing step:
A, root or the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 75 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:35g/ml;
B, after 4 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 57KHz, and temperature is 23 ℃, and the time is 20min;
C, by the raw material moisture control after ultrasonic degreasing 65%;
D, use the methyl alcohol of 87% concentration as solvent again, soaking after 0.8 hour is 680W at microwave output power, carries out microwave extraction 37s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:48g/ml;
E, by extracting solution under 135 degree, first atmospheric evaporation 28min, then be decompressed to 0.4MP evaporation 20min, obtains trihydroxyoctahydroindolizidine sterling.
The trihydroxyoctahydroindolizidine that adopts above-mentioned technique to extract can reach following index:
The These parameters of the trihydroxyoctahydroindolizidine sterling that as seen from the above table, the present invention extracts is all better than prior art.
Embodiment 4
Preferred technique is:
A, root and the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 73～76 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:32～1:36g/ml;
B, after 3.5-4.5 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 58KHz, and temperature is 23-25 ℃, and the time is 20-23min;
C, by the raw material moisture control after ultrasonic degreasing 30-40%;
D, use the methyl alcohol of 88% concentration as solvent again, soaking after 0.5 hour is 650 at microwave output power, carries out microwave extraction 37～39s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:47～49g/ml;
E, by extracting solution under 135 degree, first atmospheric evaporation 27-29min, then be decompressed to 0.3-0.4MP evaporation, 15-20min, obtains trihydroxyoctahydroindolizidine sterling.
The trihydroxyoctahydroindolizidine that adopts above-mentioned technique to extract can reach following index:
The These parameters of the trihydroxyoctahydroindolizidine sterling that as seen from the above table, the present invention extracts is all better than prior art.
Embodiment 5
Optimised process is:
A, root or the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 74 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:32g/ml;
B, after 3.5 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 58KHz, and temperature is 23 ℃, and the time is 20min;
C, by the raw material moisture control after ultrasonic degreasing 35%;
D, use the methyl alcohol of 88% concentration as solvent again, soaking after 0.5 hour is 650 at microwave output power, carries out microwave extraction 37s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:49g/ml;
E, by extracting solution under 135 degree, first atmospheric evaporation 29min, then be decompressed to 0.3MP evaporation 18min, obtains trihydroxyoctahydroindolizidine sterling.
Embodiment 6
The present embodiment and above-described embodiment are basic identical, and the key distinction is:
In raw material after described a step is pulverized, after the raw material pulverizing of 70% mass ratio, cross 75-80 mesh sieves, after the raw material pulverizing of 30% mass ratio, cross 70-74 mesh sieves.
The trihydroxyoctahydroindolizidine that adopts above-mentioned technique to extract can reach following index:
As seen from the above table, the present invention adopts the raw material of different-grain diameter, trihydroxyoctahydroindolizidine very high purity, and These parameters is all better than prior art, and especially extraction yield is high.
Embodiment 7
The present embodiment and above-described embodiment are basic identical, and the key distinction is:
In described a step, the root of Astragalus strictus of take is raw material, after directly pulverizing, crosses 75～80 mesh sieves, in the raw material after pulverizing, adds sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:35～1:40g/ml.
Embodiment 8
The present embodiment and above-described embodiment are basic identical, and the key distinction is:
In described a step, the stem of Astragalus strictus of take is raw material, after directly pulverizing, crosses 70～73 mesh sieves, in the raw material after pulverizing, adds sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:32～1:36g/ml.
Embodiment 9
The present embodiment and above-described embodiment are basic identical, and the key distinction is:
In described b step, constant-temperature ultrasonic degreasing 5-10 min at 20-22 ℃, then at 23-25 ℃ constant-temperature ultrasonic degreasing 10-15 min.
As from the foregoing, in above-mentioned two different temperature, carry out constant temperature degreasing, can obviously improve purity and extraction yield.
Embodiment 10
The present embodiment and above-described embodiment are basic identical, and the key distinction is:
In described c step, by 70% raw material moisture control after ultrasonic degreasing 30-35%, by 30% raw material moisture control after ultrasonic degreasing 60-70%.
As from the foregoing, raw material is carried out to above-mentioned different moisture control, can obviously improve microwave extraction rate.
Embodiment 11
In the Astragalus strictus extracting with aforesaid method, the content of trihydroxyoctahydroindolizidine is analyzed by gas-chromatography marker method.
Process of the test is as follows:
1, material and method
1.1 instruments and reagent material
Microwave reactor WBFY-201; Gas chromatograph (VARIAN CP-3380); Varian capillary chromatograph CP-SIL5 CB (15 mm * 0.33, m * 0.25
μm); Astragalus strictus raw material is provided by Tibet agriculture and animal husbandry academy of sciences; The buying of trihydroxyoctahydroindolizidine standard substance is from Xi'an Yangling Tianli Biotechnology Co., Ltd., purity is 98.42%, PEARLITOL 25C (analytical pure), two (TMS) trifluoroacetamide BSTFA, (trimethylchlorosilane) TMCS purchase from lark prestige company, and the chemical reagent such as pyridine are analytical pure.
1.2 extracting method
1.2.1 Astragalus strictus raw material is processed
Open air under Astragalus strictus natural condition is dried, after pulverizing, cross 75 mesh sieves, standby.
1.2.2 trihydroxyoctahydroindolizidine extracts
Precision takes 5.0g Astragalus strictus hay powder in flask, adds 150ml sherwood oil, and ultrasonic degreasing 25min under 22 ℃, 60 KHz reclaims sherwood oil.
By the raw material moisture control after ultrasonic degreasing, 65%, the methyl alcohol that is 85% by concentration by residue soaks 0.5h, then carries out microwave extraction, filtrate is condensed into medicinal extract, with 1 mol/ L HCl, dissolve, filter, remove solid impurity, with chloroform extraction, remove partial impurities, water transfer layer pH is 10, uses the n-butanol extraction aqueous solution, reclaim propyl carbinol, and with 2ml pyridine dissolution residual substance as test sample.
1.2.3 standard substance, extraction analyte derivativeization are processed
Because trihydroxyoctahydroindolizidine contains 3 hydroxyls, for large polarity alkaloid, can not directly carry out gas phase analysis.So by carrying out derivatize with two (three silyls) trifluoroacetamides (BSTFA) of N-O-, the product Heat stability is good of acquisition, high volatility, easily gasification.Accurately measure standardized solution and extract sample solution each 100
μl, adds respectively 10
μl inner mark solution and 100
μl BSTFA+TMCS(volume ratio is 99:1).
1.2.4 trihydroxyoctahydroindolizidine detects the preparation of sample solution
Accurately take PEARLITOL 25C 2mg, be dissolved in 1ml pyridine, be made into the solution that mass concentration is 2g/l.Accurately take 1mg trihydroxyoctahydroindolizidine standard substance, with pyridine, be made into the standardized solution that mass concentration is 1g/l, and it is diluted respectively to the standardized solution for 0.5g/l, 0.25 g/l, 0.625 g/l, 0.3125 g/l and 0.0156 g/l.
2, test-results
The optimum result of 2.1 extraction yield influence conditions
Selected and had 3 factors of shadow (solid-liquid ratio, power, time) to consider three levels to extraction yield, with L
9(3
3) orthogonal table tests influence factor optimization.Optimum result in Table 1, table 2.
Table 1 orthogonal test influence factor water-glass
Table 2 L9(3
3) orthogonal experiments
As can be seen from Table 2, when in Astragalus strictus, trihydroxyoctahydroindolizidine adopts microwave method to extract, the size that each factor is extracted impact to trihydroxyoctahydroindolizidine is B>C>A, wherein between each level of factor B, has significant difference.Under this experiment condition, the best of breed of microwave extraction technique is A
1b
2c
2, the test level that all the other each factors adopt also can finely be extracted trihydroxyoctahydroindolizidine, is better than traditional extraction technology.
Test-results shows, microwave power and radiated time are the major influence factors of microwave extraction technique, and to the extraction of trihydroxyoctahydroindolizidine, there were significant differences.In scope of experiment, consider reagent production cost, optimum extraction condition is A
1b
2c
2.
2.2 trihydroxyoctahydroindolizidine assays
2.2.1 optimize chromatography condition result
Column temperature is initially 150 ℃, and per minute raises 5 ℃, reaches 190 ℃, and rear per minute raises 30 ℃ until 250 ℃, and injector temperature is 260 ℃, and flame ionization detector (FID) temperature is 260 ℃, and gas is high pure nitrogen, and flow velocity is 1ml/min, sample introduction 0.4
μl, quantivative approach is internal mark working curve method.
2.2.2 the making of typical curve
Take the peak area of trihydroxyoctahydroindolizidine and the ratio of interior mark peak area in standard model is ordinate zou, take the mass concentration of trihydroxyoctahydroindolizidine as X-coordinate drawing standard curve, calculates regression equation y=5.7403x+0.1175, R
2=0.9993.Result shows that trihydroxyoctahydroindolizidine concentration becomes good linear relationship within the scope of 0.0156-0.5000 g/L.Result (in Table 3).
The ratio of table 3 SW and PEARLITOL 25C average area
| Trihydroxyoctahydroindolizidine reference substance concentration | SW peak area | PEARLITOL 25C area | The ratio of SW and PEARLITOL 25C average area |
| 0.5 | 115169 | 38792 | 2.968885 |
| 0.25 | 63059 | 39495 | 1.596632 |
| 0.0625 | 18986 | 41310 | 0.459598 |
| 0.0312 | 10869 | 40801 | 0.266391 |
| 0.0156 | 9283 | 40578 | 0.228769 |
Embodiment 12
Process application of the present invention is in root and the stem of Astragalus strictus, and extract trihydroxyoctahydroindolizidine and compare with being applied to complete stool Astragalus strictus, as following table:
| Project | Root and stem | Complete stool Astragalus strictus | Root | Stem |
| Trihydroxyoctahydroindolizidine, % >= | 99.2 | 96.0 | 99.1 | 99.3 |
| Molten, ℃ | 141—143℃ | 143—146℃ | 141—143℃ | 141—143℃ |
| Moisture content, %≤ | 0.2 | 0.4 | 0.2 | 0.2 |
| Extraction yield, % | 0.0027 | 0.0010 | 0.0029 | 0.0027 |
As seen from the above table, the present invention is applied to the root of Astragalus strictus and the trihydroxyoctahydroindolizidine that stem extracts, and purity, fusing point and moisture content are obviously better than complete stool and extract.
The trihydroxyoctahydroindolizidine that application the present invention extracts, and adopts process application of the present invention to extract trihydroxyoctahydroindolizidine other loco weed to compare, as following table:
| Project | The present invention | Yellowflower crazyweed herb | Glacier whin | Variation Radix Astragali loco weed |
| Trihydroxyoctahydroindolizidine, % >= | 99.2 | 85.0 | 87.1 | 82.3 |
| Molten, ℃ | 141—143℃ | 143—146℃ | 143—144℃ | 145—146℃ |
| Moisture content, %≤ | 0.2 | 0.4 | 0.4 | 0.5 |
| Extraction yield, % | 0.0025 | 0.0007 | 0.0009 | 0.0007 |
As seen from the above table, the technique in the present invention, is applied to other loco weed and extracts trihydroxyoctahydroindolizidine, and the purity of trihydroxyoctahydroindolizidine, fusing point and moisture content are unsatisfactory, and especially extraction yield is extremely low.
Embodiment 13
The present invention and above-described embodiment are basic identical, and the key distinction is:
The present invention also comprises the step of sterilizing, and raw material is adopted to ultraviolet disinfection 10-20 minutes, more directly pulverizes.For example adopt ultraviolet disinfection light irradiation.
Adopt after sterilizing, the trihydroxyoctahydroindolizidine index of extraction is as follows
| Project | Root and stem | Stem | Root |
| Trihydroxyoctahydroindolizidine, % >= | 99.77 | 99.79 | 99.70 |
| Molten, ℃ | 141—142℃ | 141—142℃ | 141—142℃ |
| Moisture content, %≤ | 0.13 | 0.12 | 0.14 |
| Extraction yield, % | 0.0026 | 0.0029 | 0.0027 |
Claims (1)
1. an extracting method for trihydroxyoctahydroindolizidine in Astragalus strictus, is characterized in that, comprises following processing step:
A, root and the stem of Astragalus strictus of take are raw material, after directly pulverizing, cross 74 mesh sieves, in the raw material after pulverizing, add sherwood oil to form solution, and the weightmeasurement ratio of raw material and sherwood oil is 1:32g/ml;
B, after 3.5 hours, solution is carried out to ultrasonic degreasing, reclaim sherwood oil, ultrasonic degreasing frequency is 58KHz, and temperature is 23 ℃, and the time is 20min;
C, by 70% raw material moisture control after ultrasonic degreasing 30-35%, by 30% raw material moisture control after ultrasonic degreasing 60-70%;
D, use the methyl alcohol of 88% concentration as solvent again, soaking after 0.5 hour is 650W at microwave output power, carries out microwave extraction 37s, obtains extracting solution, and the weightmeasurement ratio of raw material and methyl alcohol is 1:49g/ml;
E, by extracting solution under 135 degree, first atmospheric evaporation 29min, then be decompressed to 0.3MPa evaporation 18min, obtains trihydroxyoctahydroindolizidine sterling;
And the step that also comprises sterilizing, adopts ultraviolet disinfection 10-20 minutes by raw material, more directly pulverize.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000037465A2 (en) * | 1998-12-18 | 2000-06-29 | Glycodesign Inc. | Novel derivatives of swainsonine, processes for their preparation, and their use as therapeutic agents |
| CN1396161A (en) * | 2002-05-24 | 2003-02-12 | 杨凌大农生物技术有限公司 | Process for purifying swainsonine in Feng grass |
| CN102432609A (en) * | 2011-12-15 | 2012-05-02 | 西藏自治区农牧科学院 | Microwave-assisted extraction process for swainsonine in astragalus strictus |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000037465A2 (en) * | 1998-12-18 | 2000-06-29 | Glycodesign Inc. | Novel derivatives of swainsonine, processes for their preparation, and their use as therapeutic agents |
| CN1396161A (en) * | 2002-05-24 | 2003-02-12 | 杨凌大农生物技术有限公司 | Process for purifying swainsonine in Feng grass |
| CN102432609A (en) * | 2011-12-15 | 2012-05-02 | 西藏自治区农牧科学院 | Microwave-assisted extraction process for swainsonine in astragalus strictus |
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