CN103059082A

CN103059082A - Method for extracting taxus chinensis from taxus mairei leaves

Info

Publication number: CN103059082A
Application number: CN2012105885854A
Authority: CN
Inventors: 王强; 谢雪娣
Original assignee: TAIKANG TAXUS CHINENSIS BIOLOGICAL ENGINEERING Co Ltd NINGBO CITY
Current assignee: TAIKANG TAXUS CHINENSIS BIOLOGICAL ENGINEERING Co Ltd NINGBO CITY
Priority date: 2012-12-31
Filing date: 2012-12-31
Publication date: 2013-04-24
Anticipated expiration: 2032-12-31
Also published as: CN103059082B

Abstract

The invention discloses a method for extracting taxus chinensis from taxus mairei leaves. The method comprises the following steps: extracting with a supercritical extraction kettle; absorbing with methanol; carrying out chromatography with AB-8 resin and 100 meshes of polyamide in sequence; collecting eluant for 12-15 min; and concentrating and drying to obtain the taxus chinensis with the formula of C27H30O15. The method is simple; and the white crystallization purity of the extracted taxus chinensis is higher up to 99.28%, so that conditions are created for pharmacological research and application of the taxus chinensis.

Description

A kind of method of from leaves of Taxus mairei, extracting the Ramulus et folium taxi cuspidatae element

Technical field

The present invention relates to the extractive technique of flavones, be specifically related to a kind of method of from leaves of Taxus mairei, extracting the Ramulus et folium taxi cuspidatae element.

Background technology

Contain the efficacy components such as taxol, Japanese yew flavones and yew amylose in the leaves of Taxus mairei, the Japanese yew flavones contains common parent nucleus C ₆-C ₃-C ₆Structure, have regulate cardiovascular system effect, anti-inflammatory and anti-immunization, anti-microbial effect, to the effect of peptide ulceration and antitumor action etc.Grant number is extract and the extracting method that the Chinese invention patent of ZL200910157034.0 discloses a kind of southerm yew blade, and the extract major ingredient comprises rutin-3-O-Quercetin, rutin-3-O-kaempferol, rutin-3-O-myricetin, kaempferol-7-O-glucose and glucose-7-O-Quercetin; Extracting method comprises that blade oven dry, crushing screening, immersion alcohol solvent, the lower supersound extraction of stirring, extracting solution concentrating under reduced pressure go alcohol, chloroform extraction degreasing, water concentrate drying step, and what the method obtained is the mixture of various flavones.Grant number is that the Chinese invention patent of ZL201010604150.5 discloses and a kind ofly extracts Sciadopitysin (C from the southerm yew blade ₃₀H ₁₅O ₇) method, extracting method comprises the processes such as blade oven dry, crushing screening, ultrasonic extraction, AB-8 macroporous resin chromatography, silica gel column chromatography separation.Do not find to extract the Ramulus et folium taxi cuspidatae element open report of (belonging to the Japanese yew flavonoid) in the southerm yew.

Summary of the invention

Technical problem to be solved by this invention provides a kind of method of extracting the Ramulus et folium taxi cuspidatae element from leaves of Taxus mairei, the method is extracted first from leaves of Taxus mairei and is obtained the higher Ramulus et folium taxi cuspidatae element monomer of purity, for condition has been created in pharmacological research and the application of this Ramulus et folium taxi cuspidatae element.

The present invention solves the problems of the technologies described above the technical scheme that adopts: a kind of method of from leaves of Taxus mairei, extracting the Ramulus et folium taxi cuspidatae element, and its step is as follows:

1, fresh southerm yew blade is dried 24h under 50 ℃ of temperature, pulverize, cross No. 8 sieves and be powder, in the supercritical extraction reactor of packing into;

2, in the supercritical extraction reactor, be 25 ℃ in extraction temperature, CO ₂Hydrodynamicpressure is 22MPa, under entrainment agent ethanol flow velocity 0.17 ml/min, extracts 1 h, and extraction is extracted thing;

3, in extract, add methyl alcohol and be absorbed as absorption liquid, the addition of described methyl alcohol is to add methyl alcohol 1ml in the extract of above-mentioned powder 5g, absorption liquid AB-8 resin chromatography, then be 80% ethanol elution with mass percentage concentration, obtain the first elutriant, the first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, the first concentrated solution is the ethanol elution of 20 % with mass percentage concentration with 100 order polymeric amide chromatographies again, collects the elutriant of 12～15 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is the Ramulus et folium taxi cuspidatae element, and this Ramulus et folium taxi cuspidatae element molecular formula is C ₂₇H ₃₀O ₁₅Adopt high effective liquid chromatography for measuring, Ramulus et folium taxi cuspidatae element purity reaches 99.28% in the white crystalline compound.

The molecular formula of Ramulus et folium taxi cuspidatae element of the present invention is C ₂₇H ₃₀O ₁₅That the inventor extracts from southerm yew first and separates, inventor's called after Ramulus et folium taxi cuspidatae element, the chemical structure names of this Ramulus et folium taxi cuspidatae element is 4H-1-Benzopyran-4-one, 3-[[4-O-(6-deoxy-α-L-mannopyranosyl)-β-D-glucopyranosyl] oxy]-5,7-dihydroxy-2-(4-hydroxyphenyl.Be a kind of new Japanese yew flavonoid compound, the structural formula of this Ramulus et folium taxi cuspidatae element is:

Figure 2012105885854100002DEST_PATH_IMAGE001

。

Compared with prior art, the invention has the advantages that a kind of method of from leaves of Taxus mairei, extracting the Ramulus et folium taxi cuspidatae element, extract by supercritical extraction reactor, methyl alcohol absorbs, and behind the AB-8 resin chromatography, uses 100 order polymeric amide chromatographies again, collect the elutriant of 12～15 min, it is C that concentrate drying obtains molecular formula ₂₇H ₃₀O ₁₅Ramulus et folium taxi cuspidatae element, this extracting method is simple, the white look crystallization of the Ramulus et folium taxi cuspidatae of extraction purity is higher, reaches 99.28%, for condition has been created in pharmacological research and the application of this Ramulus et folium taxi cuspidatae element.

Embodiment

Below in conjunction with embodiment the present invention is described in further detail.

Embodiment: a kind of method of from leaves of Taxus mairei, extracting the Ramulus et folium taxi cuspidatae element, first fresh southerm yew blade is dried 24h under 50 ℃ of temperature condition, pulverize, cross No. 8 sieves and be powder, the 50g that weighs is in the supercritical extraction reactor of packing into; Be 25 ℃ in extraction temperature in the supercritical extraction reactor, CO ₂Hydrodynamicpressure is 22MPa, under entrainment agent ethanol flow velocity 0.17 ml/min, extracts 1 h, is extracted thing; Add 10ml methyl alcohol in the extract and be absorbed as absorption liquid, absorption liquid AB-8 resin (commercially available) chromatography, the AB-8 resin is low-pole, surface-area 480～520 (m2/g), particle radii 13～14nm, water content 64%; Behind the chromatography be 80% ethanol elution with mass percentage concentration, obtain the first elutriant, the first elutriant is under 500Pa, concentrating under reduced pressure 60min, obtain the first concentrated solution, the first concentrated solution is 20% ethanol elution with mass percentage concentration again with 100 order polymeric amide (commercially available) chromatographies, collect the elutriant of 12～15 min, concentrate drying obtains white crystalline compound, and this white crystalline compound is the Ramulus et folium taxi cuspidatae element, adopt the high performance liquid chromatography conventional determining, its purity reaches 99.28%.Through analysis of the molecular structure, its molecular formula is C ₂₇H ₃₀O ₁₅, be a kind of new Japanese yew flavonoid compound.

Claims

1. method of extracting the Ramulus et folium taxi cuspidatae element from leaves of Taxus mairei is characterized in that step is as follows:

1) fresh southerm yew blade is dried 24h under 50 ℃ of temperature, pulverize, cross No. 8 sieves and be powder, in the supercritical extraction reactor of packing into;

2) in the supercritical extraction reactor, be 25 ℃ in extraction temperature, CO ₂Hydrodynamicpressure is 22MPa, under entrainment agent ethanol flow velocity 0.17 ml/min, extracts 1 h, and extraction is extracted thing;

3) in extract, add methyl alcohol and be absorbed as absorption liquid, the addition of described methyl alcohol is to add methyl alcohol 1ml in the extract of above-mentioned powder 5g, absorption liquid AB-8 resin chromatography, then be 80% ethanol elution with mass percentage concentration, obtain the first elutriant, the first elutriant is concentrating under reduced pressure 60min under 500Pa, obtain the first concentrated solution, the first concentrated solution is the ethanol elution of 20 % with mass percentage concentration with 100 order polymeric amide chromatographies again, collects the elutriant of 12～15 min, concentrate drying, obtain white crystalline compound, this white crystalline compound is the Ramulus et folium taxi cuspidatae element, and this Ramulus et folium taxi cuspidatae element molecular formula is C ₂₇H ₃₀O ₁₅