阅读说明：本技术 一种从番荔枝种子中提取泡番荔枝辛的方法 (A method of it is pungent to extract bubble manaca from sugar apple seed ) 是由 余雁 司文会 于 2019-07-22 设计创作，主要内容包括：本发明涉及从番荔枝种子中提取泡番荔枝辛的方法,其以番荔枝种子为原料,包括(1)、用醇水溶液对番荔枝种子进行提取,得粗提物；(2)、对粗提物进行脱脂处理,得半成品；(3)、将半成品用乙醇-水溶液溶解,制成混浊度低于0.5°的上样溶液,采用大孔树脂D101分离柱,湿法上样以后,静置,至树脂达到吸附平衡,以乙醇-水溶液为洗脱液,进行梯度洗脱或等度分段洗脱,收集泡番荔枝辛质量分数大于30%的洗脱液,合并,浓缩,干燥,得粗品；(4)、对粗品重复步骤(3)的提纯,收集泡番荔枝辛质量分数大于等于95%的洗脱液,合并,浓缩,干燥,即得所述泡番荔枝辛。本发明能从番荔枝种子中高效提取泡番荔枝辛,操作简单,成本低廉,适合大规模生产。(The present invention relates to the pungent method of bubble manaca is extracted from sugar apple seed, using sugar apple seed as raw material, including (1), with alcohol solution sugar apple seed is extracted, obtain crude extract；(2), ungrease treatment is carried out to crude extract, obtains semi-finished product；(3), semi-finished product are dissolved with ethanol-water solution, the load solution that turbidity is lower than 0.5 ° is made, using macroreticular resin D101 splitter, after wet process loading, it stands, until resin reaches adsorption equilibrium, using ethanol-water solution as eluent, carry out gradient elution or isocratic stepwise elution, the eluent that the bubble pungent mass fraction of manaca is greater than 30% is collected, is merged, concentration, it is dry, obtain crude product；(4), the purification of step (3) is repeated to crude product, is collected the eluent that the bubble pungent mass fraction of manaca is more than or equal to 95%, is merged, concentration, drying is pungent to get the bubble manaca.The present invention can from sugar apple seed high efficiency extraction bubble manaca it is pungent, it is easy to operate, it is low in cost, be suitble to large-scale production.)

1. a kind of extract the pungent method of bubble manaca from sugar apple seed, it is characterised in that: using sugar apple seed as raw material, packet Include the following steps successively carried out:

(1), sugar apple seed is extracted with the alcohol solution that alcohol volume content is 80% ~ 95%, concentrated extracting solution, is done It is dry, obtain crude extract；

(2), ungrease treatment is carried out to crude extract obtained by step (1) with petroleum ether, is repeatedly extracted using ether later, merge ether Extract liquor, vacuum decompression recycling design obtain flow-like substance, and 40 DEG C or less are dried in vacuo to obtain semi-finished product；

(3), semi-finished product obtained by step (2) are dissolved with ethanol-water solution, the load solution that turbidity is lower than 0.5 ° is made, adopts With macroreticular resin D101 splitter, after wet process loading, stand, until resin reaches adsorption equilibrium, it is to wash with ethanol-water solution De- liquid, carries out gradient elution or isocratic stepwise elution, collects the eluent that the bubble pungent mass fraction of manaca is greater than 30%, merges, dense Contracting, it is dry, obtain crude product；

(4), the purification of step (3) is repeated to crude product obtained by step (3), is collected the bubble pungent mass fraction of manaca and is more than or equal to 95% Eluent, merge, concentration, drying it is pungent to get the bubble manaca.

2. according to the method described in claim 1, it is characterized by: the sugar apple seed as raw material is dry kind litchi Branch seed powder.

3. according to the method described in claim 1, it is characterized by: the alcohol is ethyl alcohol, described to extract in step (1) It is carried out under room temperature.

4. according to the method described in claim 1, it is characterized by: in step (2), the vacuum drying temperature is 25 DEG C ~ 30℃。

5. according to the method described in claim 1, it is characterized by: carrying out gradient elution in step (3).

6. according to the method described in claim 1, it is characterized by: carry out isocratic stepwise elution in step (3) and (4), with 10% concentration difference is a spacer, and every section of elution volume is 2 ~ 3 column volumes, and eluent flow rate is 1 ~ 2 column Volume/hour.

7. according to the method described in claim 1, standing it is characterized by: the standing carries out at room temperature in step (3) Time be 0.5 ~ 1h.

Technical field

The present invention is a kind of to extract the pungent method of bubble manaca from sugar apple seed.

Background technique

Sugar apple seed is the dry mature seed of Anona Annonaceae plant manaca.The kind of bullock's heart Son Annona lactone rich in, such compound have significant anti-tumor activity.Research shows that bubble manaca is pungent to small The inhibiting rate of mouse lymphotactin Leukemia Cell Lines L1210 is 300 times of taxol.

It is known that sugar apple seed is with the difference in the place of production and the bubble manaca containing different content is pungent.The present invention provide from kind The pungent method of high efficiency extraction bubble manaca will be with important economy and environmental benefit in Litchi chinensis Seeds.

Summary of the invention

High efficiency extraction that technical problem to be solved by the invention is to provide a kind of from sugar apple seed bubble manaca is pungent Method.

In order to solve the above technical problems, the present invention adopts the following technical scheme that:

A method of extraction bubble manaca is pungent from sugar apple seed, using sugar apple seed as raw material, including successively carries out Following steps:

(1), sugar apple seed is extracted with the alcohol solution that alcohol volume content is 80wt% ~ 95wt%, concentrated extracting solution, It is dry, obtain crude extract；

(2), ungrease treatment is carried out to crude extract obtained by step (1) with petroleum ether, is repeatedly extracted using ether later, merge ether Ester extract liquor, vacuum decompression recycling design obtain flow-like substance, and 40 DEG C or less are dried in vacuo to obtain semi-finished product；

(3), semi-finished product obtained by step (2) are dissolved with ethanol-water solution, the load solution that turbidity is lower than 0.5 ° is made, adopts With macroreticular resin D101 splitter, after wet process loading, stand, until resin reaches adsorption equilibrium, it is to wash with ethanol-water solution De- liquid, carries out gradient elution or isocratic stepwise elution, collects the eluent that the bubble pungent mass fraction of manaca is greater than 30%, merges, dense Contracting, it is dry, obtain crude product；

(4), the purification of step (3) is repeated to crude product obtained by step (3), is collected the bubble pungent mass fraction of manaca and is more than or equal to 95% Eluent, merge, concentration, drying it is pungent to get the bubble manaca.

Preferably, the sugar apple seed as raw material is dry sugar apple seed powder.Size of powder particles can be Such as 30 ~ 100 mesh.

Preferably, in step (1), alcohol can be the alcohol that methanol, ethyl alcohol etc. are usually used in plant extract, but preferably ethyl alcohol. The extraction can carry out at normal temperature.

Preferably, in step (2), the vacuum drying temperature is 25 DEG C ~ 30 DEG C.

One according to the present invention specific and preferred aspect in step (3), carries out gradient elution.

Another specific and preferred aspect according to the present invention in step (4), carries out gradient elution, and by the bubble of collection The pungent mass fraction of manaca is that the eluent more than or equal to 95% merges, and is concentrated, dry.

Another specific and preferred aspect according to the present invention in step (3) and (4), carries out isocratic stepwise elution, with 10% Concentration difference be a spacer, every section of elution volume is 2 ~ 3 column volumes, eluent flow rate be 1 ~ 2 column volume/ Hour.

In step (3), the standing carries out at room temperature, and the time of standing is 0.5 ~ 1h.

According to the present invention, in step (1), the dosage of alcohol solution is generally 10 ~ 15 times (V/G) of sugar apple seed.

Due to the implementation of above technical scheme, the invention has the following advantages over the prior art:

(1) preparation process is simple, easily operated；

(2) low in cost, it is suitble to large-scale production, there is application potential.

Specific embodiment

Below in conjunction with specific embodiment, the present invention will be further described in detail, but the present invention is not limited to following realities Apply example.