CN104524812B - Use immobilized liquid-liquid extraction post from Chinese medicine Aqueous extracts, extract the method for active ingredient - Google Patents
Use immobilized liquid-liquid extraction post from Chinese medicine Aqueous extracts, extract the method for active ingredient Download PDFInfo
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Abstract
The invention discloses a kind of method using immobilized liquid-liquid extraction post to extract active ingredient from Chinese medicine Aqueous extracts, comprise the steps: Chinese medicine Aqueous extracts to be placed in immobilized liquid-liquid extraction post that specification is 10-5000g, leave standstill 15-20min, wash-out is carried out with the solvent immiscible with aqueous phase, the flow velocity of eluent is 10-400mL/min, collect eluent, reduced pressure concentration is pressed powder.Feature of the present invention is: 1, extracting operation is simple, and extraction times reduces to 1 time for 3-4 time by liquid-liquid extraction; 2, solvent use amount reduces 10-40%; 3, the processing time reduces to 0.5-1h by original 1-2h; 4, the active ingredient rate of recovery remains unchanged or slightly increases.5, immobilized liquid-liquid extraction column packing adopts diatomite, substitutes the purification that extract is carried out in traditional liquid-liquid extraction, effectively avoid emulsion by immobilized liquid-liquid extraction method.
Description
Technical field
The present invention relates to the method extracting active ingredient from Chinese medicine Aqueous extracts.
Background technology
The extraction of effective components from natural materials normally carries out liquid-liquid extraction with the extract organic solvent of water backflow, to remove the chaff interference such as polysaccharide, tannin, although the method for liquid-liquid extraction can reach the object of purification, but complicated operation, easy emulsification, reappearance is not high, and the rate of recovery is low, and solvent use amount is large.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, provide a kind of general simple to operate, favorable reproducibility, the immobilized liquid-liquid extraction post of the use that solvent use amount is few extracts the method for active ingredient from Chinese medicine Aqueous extracts.
Technical scheme of the present invention is summarized as follows:
Use immobilized liquid-liquid extraction post from Chinese medicine Aqueous extracts, extract the method for active ingredient, comprise the steps: Chinese medicine Aqueous extracts to be placed in immobilized liquid-liquid extraction post that specification is 10-5000g, leave standstill 15-20min, wash-out is carried out with the solvent immiscible with aqueous phase, the flow velocity of eluent is 10-400mL/min, collect eluent, reduced pressure concentration is pressed powder.
Chinese medicine Aqueous extracts is agastache rugosa water extract, sword-like leave barrenwort Aqueous extracts or fruit of Chinese magnoliavine Aqueous extracts.
The specification of immobilized liquid-liquid extraction post is 10-5000kg.
The solvent immiscible with aqueous phase is preferred: chloroform, carrene, benzinum at least one.
The flow velocity of eluent is preferred: 10-400mL/min.
Feature of the present invention is: 1, extracting operation is simple, and extraction times reduces to 1 time for 3-4 time by liquid-liquid extraction; 2, solvent use amount reduces 10-40%; 3, the processing time reduces to 0.5-1h by original 1-2h; 4, the active ingredient rate of recovery remains unchanged or slightly increases.5, immobilized liquid-liquid extraction column packing adopts diatomite, substitutes the purification that extract is carried out in traditional liquid-liquid extraction, effectively avoid emulsion by immobilized liquid-liquid extraction method.
Accompanying drawing explanation
Fig. 1 extracts the chromatogram of magnolol and honokiol from agastache rugosa water extract by method of the present invention;
Fig. 2 extracts the chromatogram of icariin from sword-like leave barrenwort Aqueous extracts by method of the present invention;
Fig. 3 extracts the chromatogram of Ge meter Xin Q and gomisin H from fruit of Chinese magnoliavine Aqueous extracts by method of the present invention.
Detailed description of the invention
Filler in immobilized liquid-liquid extraction post is diatomite, diatomite has water imbibition and porous, sample aqueous solution disperses at its porous surface Quick uniform, then in balance, drip washing (wash-out) is carried out with the another kind of solvent immiscible with aqueous phase, active ingredient is extracted from the aqueous solution, reaches enrichment, go disturb object.By diatomaceous peptizaiton, make aqueous extract form the film of one deck aqueous phase on diatomite surface, substantially increase contact and the exchange area of organic extraction solvent and aqueous phase.This extraction mode can also be avoided because machinery shakes the emulsion layer causing being formed between organic extraction solvent and aqueous extract simultaneously.Method of the present invention can also pass through selective absorption, further removes some impurity, and filters out particle that is that bring in some aqueous extracts or that formed at two-phase contact surface or jelly simultaneously.
The immobilized liquid-liquid extraction post brand that the present invention adopts is Cleanert
rsLE, is purchased from Beaune Ai Jieer Science and Technology Ltd..
Below by specific embodiment, the present invention is further illustrated.
Embodiment 1
Use immobilized liquid-liquid extraction post from Chinese medicine Aqueous extracts, extract the method for active ingredient, comprise the steps:
Get agastache rugosa water extract 500mL, add concentrated hydrochloric acid and make volumetric concentration be 0.04%, be placed in immobilized liquid-liquid extraction post that specification is 800g/1500mL, leave standstill 15min, with 1.2L chloroform with the flow velocity wash-out of 100mL/min, collect eluent, at 35 DEG C, reduced pressure concentration is pressed powder.
Get pressed powder 3mg, dissolve with methyl alcohol, filter, get subsequent filtrate and enter HPLC detection by official method;
After testing, in 27g wrinkled giant hyssop medicinal material, magnolol in agastache rugosa water extract and honokiol content are respectively 0.453g and 0.585g, are respectively 80.6% and 83.3% with the content of magnolol and honokiol in agastache rugosa water extract for 0.730mg/mL and 0.975mg/mL calculates its rate of recovery; Use eluent 1.2L.The chromatogram extracting magnolol and honokiol from agastache rugosa water extract is shown in Fig. 1.The peak of retention time 14.655min is honokiol; Retention time 24.574min is the peak of magnolol.
Comparative example:
Use liquid-liquid extraction method from Chinese medicine Aqueous extracts, extract the method for active ingredient, comprise the steps:
Get agastache rugosa water extract 500mL, add concentrated hydrochloric acid and make volumetric concentration be 0.04%, then add 500mL chloroform, jolting 5min, leave standstill 15min, take out upper strata, again add 500mL chloroform, re-extract 3 times, combining extraction liquid, adds 5g anhydrous calcium chloride, leaves standstill 10min, filter, filtrate reduced pressure concentration at 35 DEG C is pressed powder.
Get pressed powder 3mg, dissolve with methyl alcohol, filter, get subsequent filtrate and enter HPLC detection by official method;
After testing, calculate by the mode identical with immobilized liquid-liquid extraction, in agastache rugosa water extract, the content of magnolol and honokiol is that 0.727mg/mL and 0.964mg/mL calculates its rate of recovery and be respectively 80.2% and 82.4%; Use eluent 1.5L.
Embodiment 2
Use immobilized liquid-liquid extraction post from Chinese medicine Aqueous extracts, extract the method for active ingredient, comprise the steps:
Get the medicinal extract 2.0g that sword-like leave barrenwort Aqueous extracts is concentrated, add the ultrasonic 20min of 25mL water, be placed in immobilized liquid-liquid extraction post that specification is 10g/100mL, leave standstill 20min, be that the mixed solution that forms of the carrene of 2:8 and benzinum is with the flow velocity wash-out of 10mL/min by 45mL volume ratio, collect eluent, at 35 DEG C, reduced pressure concentration is pressed powder.
After testing, in 9g sword-like leave epimedium herb, with HPLC detection computations, must containing the solid 1.6g of icariin 25%, extraction and cleaning is respond well.The chromatogram extracting icariin from sword-like leave barrenwort Aqueous extracts is shown in Fig. 2; Retention time 11.174min is icariin.
Embodiment 3
Use immobilized liquid-liquid extraction post from Chinese medicine Aqueous extracts, extract the method for active ingredient, comprise the steps:
Get 4.2L fruit of Chinese magnoliavine Aqueous extracts and add 1L acetonitrile and 5mL formic acid, add water to 10L, mixing, is placed in the immobilized liquid-liquid extraction post that specification is 5kg/10L, leave standstill 20min, with the chloroform soln that 4L volumetric concentration is 0.01% triethylamine, with the flow velocity wash-out of 400mL/min, collect eluent, anhydrous calcium chloride 50g is added in eluent, filter after stirring, filter paper 100mL volumetric concentration is that the chloroform soln of 0.01% triethylamine rinses, and merges; 35 DEG C of reduced pressure concentrations are pressed powder.
4.2L fruit of Chinese magnoliavine Aqueous extracts amounts to 2.3kg schisandra chinensis medicinal material, with HPLC detection computations, is respectively the solid 38.4g of 17% and 18.3% in the pressed powder after concentrated containing Ge meter Xin Q and gomisin H.The chromatogram extracting Ge meter Xin Q and gomisin H from fruit of Chinese magnoliavine Aqueous extracts is shown in Fig. 3, and in figure, retention time is 12.269min is Ge meter Xin Q; 14.401min be gomisin H.
The various embodiments described above understand the present invention to enable those skilled in the art to, but the present invention does not impose any restrictions.The solvent immiscible with aqueous phase can also select ether, methyl tertiary butyl ether(MTBE), benzinum, n-hexane, octane, ethyl acetate, butanols, amylalcohol, hexanol and octanol at least one.
Claims (1)
1. use immobilized liquid-liquid extraction post from Chinese medicine Aqueous extracts, extract the method for active ingredient, it is characterized in that comprising the steps: Chinese medicine Aqueous extracts is placed in immobilized liquid-liquid extraction post that specification is 10-5000g, leave standstill 15-20min, wash-out is carried out with the solvent immiscible with aqueous phase, the flow velocity of eluent is 10-400mL/min, collect eluent, reduced pressure concentration is pressed powder; Filler in immobilized liquid-liquid extraction post is diatomite; Described Chinese medicine Aqueous extracts is agastache rugosa water extract, sword-like leave barrenwort Aqueous extracts or fruit of Chinese magnoliavine Aqueous extracts; The described solvent immiscible with aqueous phase is at least one in chloroform, carrene and benzinum.
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| CN104820037B (en) * | 2015-05-12 | 2016-08-24 | 广西壮族自治区梧州食品药品检验所 | Ractopamine in high-acruracy survey feedstuff, clenbuterol, the method for albuterol content |
| CN104820054B (en) * | 2015-05-12 | 2016-07-06 | 广西壮族自治区梧州食品药品检验所 | High-acruracy survey pig urine in Ractopamine, clenbuterol, albuterol content method |
| CN104807918B (en) * | 2015-05-12 | 2016-08-31 | 广西壮族自治区梧州食品药品检验所 | The method of the Ractopamine content in high-acruracy survey pig urine |
| CN104807919B (en) * | 2015-05-12 | 2017-01-04 | 广西壮族自治区梧州食品药品检验所 | Use the method that SLE method separates the clenbuterol in pig urine |
| CN104820038A (en) * | 2015-05-12 | 2015-08-05 | 广西壮族自治区梧州食品药品检验所 | Method for detecting content of ractopamine in feed at high precision |
| CN112979043B (en) * | 2021-03-05 | 2022-08-26 | 生态环境部南京环境科学研究所 | Purification and recovery device of synergistic eluent for restoring organochlorine pesticide contaminated soil |
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| CN101637667B (en) * | 2009-08-19 | 2011-09-14 | 大连理工大学 | Method for extracting effective components from natural products by adopting triple liquid phases |
| CN102179066B (en) * | 2011-05-12 | 2013-10-16 | 中国科学院过程工程研究所 | Method for extracting and separating ions in two valence states of the same element in three phases |
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