阅读说明：本技术 一种从海南粗榧中提取三尖杉碱的方法 (Method for extracting cephalotaxine from cephalotaxus hainanensis ) 是由 高非 沈芸 赵德庆 赵曼娜 王小慧 罗海燕 房一明 王荣香 于 2021-02-03 设计创作，主要内容包括：本申请公开了一种从海南粗榧中提取三尖杉碱的方法,加入提取溶剂后以超声提取装置提取海南粗榧粉末得第一提取液,其中硫酸水溶液或甲醇溶液作为提取溶剂,可实现经济节约、环境友好,有利于实现工业化生产；将第一提取液进行离心后倒出上清液,重复执行加入提取溶剂、超声提取、离心、离心结束后倒出上清液操作1～4次,合并上清液得第二提取液,采用制备型高效液相色谱分离纯化三尖杉碱的方法,成功将第二提取液分离纯化出三尖杉碱单体,多次提取可增加三尖杉碱的提取质量、效率高,解决了现有三尖杉属植物中提取三尖杉碱均是采用乙醇等有机溶剂,成本高、不利于实现工业化生产,且分离纯化时多采用柱层析法,该方法溶剂用量大、效率低的技术问题。(The application discloses a method for extracting cephalotaxine from cephalotaxus hainanensis, wherein after an extraction solvent is added, a first extraction solution is obtained by extracting cephalotaxus hainanensis powder by an ultrasonic extraction device, wherein a sulfuric acid aqueous solution or a methanol solution is used as the extraction solvent, so that economic saving and environmental friendliness can be realized, and industrial production can be realized; centrifuging the first extracting solution, pouring out supernatant, repeatedly performing operations of adding an extracting solvent, ultrasonic extraction, centrifugation and pouring out supernatant after centrifugation for 1-4 times, combining the supernatant to obtain a second extracting solution, and successfully separating and purifying the second extracting solution to obtain a cephalotaxine monomer by adopting a method for separating and purifying cephalotaxine by preparative high performance liquid chromatography.)

1. A method for extracting cephalotaxine from cephalotaxus hainanensis is characterized by comprising the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving for later use;

step 2, weighing cephalotaxus hainanensis powder with preset particle size, placing the cephalotaxus hainanensis powder into a centrifugal tube, adding an extraction solvent according to a preset feed-liquid ratio, and placing the cephalotaxus hainanensis powder into an ultrasonic extraction device for ultrasonic extraction to obtain a first extraction solution, wherein the extraction solvent is sulfuric acid aqueous solution or methanol solution;

step 3, placing the first extracting solution into a centrifugal device for centrifugation, pouring out supernatant after centrifugation is finished, repeatedly adding an extracting solvent, carrying out ultrasonic extraction, centrifugation and pouring out supernatant after centrifugation is finished for 1-4 times, and combining the supernatants to obtain a second extracting solution;

step 4, detecting the content of the cephalotaxine in the second extracting solution through UPLC-MS;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

2. The method for extracting cephalotaxus hainanensis li as claimed in claim 1, further comprising, before step 1:

drying the picked cephalotaxus hainanensis leaves to constant weight.

3. The method for extracting cephalotaxine from cephalotaxus hainanensis according to claim 2, wherein the step 1 comprises:

crushing cephalotaxus hainanensis leaves in a crusher to obtain brown yellow uniform powder, sieving the brown yellow uniform powder through a 10-200-target standard inspection sieve to obtain cephalotaxus hainanensis powder with different particle sizes, and storing the cephalotaxus hainanensis powder in a 4 ℃ thermostat for later use.

4. The method for extracting cephalotaxine from cephalotaxus hainanensis according to claim 1, wherein the pH value of the sulfuric acid aqueous solution is 1.0-5.0.

5. The method for extracting cephalotaxus hainanensis li as claimed in claim 4, wherein the pH of the aqueous solution of sulfuric acid is 1.0.

6. The method for extracting cephalotaxine from cephalotaxus hainanensis according to claim 1, wherein in step 2, the ratio of material to liquid is 1: 20-1: 60.

7. The method for extracting cephalotaxus hainanensis li as claimed in claim 1, wherein after step 3 and before step 4, further comprising:

diluting the second extractive solution by 5 times, and filtering with 0.22 μm microporous membrane.

8. The method for extracting cephalotaxine from cephalotaxus hainanensis according to claim 1, wherein in step 2, the ultrasonic power of the ultrasonic extraction device is 240-600W, the extraction temperature is 28-75 ℃, and the extraction time is 10-40 min.

9. The method for extracting cephalotaxine from cephalotaxus hainanensis according to claim 1, wherein in step 3, the centrifugal speed of the centrifugal device is 10000r/min, and the centrifugal time is 5 min.

Technical Field

The application relates to the technical field of cephalotaxine extraction methods, in particular to a method for extracting cephalotaxine from cephalotaxus hainanensis.

Background

Cephalotaxus hainanensis is tree of cephalotaxus genus of cephalotaxaceae family, and its leaves, branches, seeds and roots contain 11 cephalotaxoids such as cephalotaxine and homoharringtonine. The cephalotaxus ester alkaloid has obvious anti-tumor effect and extremely low content in plants, the natural yield of the cephalotaxus ester alkaloid cannot meet the market demand, but most cephalotaxus ester alkaloid contains the same core skeleton, namely cephalotaxus alkali. Therefore, the cephalotaxus alkaloid is extracted from the plants and obtained by a semi-synthesis method, and the resource supply problem of the cephalotaxus alkaloid is hopefully solved. The existing cephalotaxine extraction from cephalotaxus plants adopts organic solvents such as ethanol, chloroform and the like, has high cost and is not beneficial to realizing industrial production, and column chromatography is mostly adopted during separation and purification, and the method has the advantages of large solvent consumption, long consumption time and low efficiency.

Disclosure of Invention

The application provides a method for extracting cephalotaxine from cephalotaxus hainanensis, which is used for solving the technical problems that the existing cephalotaxus plants are extracted by organic solvents such as ethanol, chloroform and the like, the cost is high, the industrial production is not easy to realize, and column chromatography is mostly adopted during separation and purification, the method is large in solvent consumption, long in consumption time and low in efficiency.

In view of the above, the present application provides a method for extracting cephalotaxine from cephalotaxus hainanensis, comprising the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving for later use;

step 2, weighing cephalotaxus hainanensis powder with preset particle size, placing the cephalotaxus hainanensis powder into a centrifugal tube, adding an extraction solvent according to a preset feed-liquid ratio, and placing the cephalotaxus hainanensis powder into an ultrasonic extraction device for ultrasonic extraction to obtain a first extraction solution, wherein the extraction solvent is sulfuric acid aqueous solution or methanol solution;

step 3, placing the first extracting solution into a centrifugal device for centrifugation, pouring out supernatant after centrifugation is finished, repeatedly adding an extracting solvent, carrying out ultrasonic extraction, centrifugation and pouring out supernatant after centrifugation is finished for 1-4 times, and combining the supernatants to obtain a second extracting solution;

step 4, detecting the content of the cephalotaxine in the second extracting solution through UPLC-MS;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Optionally, before step 1, further comprising:

drying the picked cephalotaxus hainanensis leaves to constant weight.

Optionally, step 1 specifically includes:

crushing cephalotaxus hainanensis leaves in a crusher to obtain brown yellow uniform powder, sieving the brown yellow uniform powder through a 10-200-target standard inspection sieve to obtain cephalotaxus hainanensis powder with different particle sizes, and storing the cephalotaxus hainanensis powder in a 4 ℃ thermostat for later use.

Optionally, the pH value of the sulfuric acid aqueous solution is 1.0-5.0.

Alternatively, the aqueous sulfuric acid solution has a pH of 1.0.

Optionally, in the step 2, the ratio of the material to the liquid is 1: 20-1: 60.

Optionally, after step 3 and before step 4, the method further includes:

diluting the second extractive solution by 5 times, and filtering with 0.22 μm microporous membrane.

Optionally, in the step 2, the ultrasonic power of the ultrasonic extraction device is 240-600W, the extraction temperature is 28-75 ℃, and the extraction time is 10-40 min.

Optionally, in step 3, the centrifugal speed of the centrifugal device is 10000r/min, and the centrifugal time is 5 min.

According to the technical scheme, the embodiment of the application has the following advantages:

the application provides a method for extracting cephalotaxine from cephalotaxus hainanensis, which comprises the following steps: step 1, crushing cephalotaxus hainanensis leaves and then sieving for later use; step 2, weighing cephalotaxus hainanensis powder with preset particle size, placing the cephalotaxus hainanensis powder into a centrifugal tube, adding an extraction solvent according to a preset feed-liquid ratio, and placing the cephalotaxus hainanensis powder into an ultrasonic extraction device for ultrasonic extraction to obtain a first extraction solution, wherein the extraction solvent is sulfuric acid aqueous solution or methanol solution; step 3, placing the first extracting solution into a centrifugal device for centrifugation, pouring out supernatant after centrifugation is finished, repeatedly adding an extracting solvent, carrying out ultrasonic extraction, centrifugation and pouring out supernatant after centrifugation is finished for 1-4 times, and combining the supernatants to obtain a second extracting solution; step 4, detecting the content of the cephalotaxine in the second extracting solution through UPLC-MS; and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

According to the method for extracting cephalotaxus from cephalotaxus hainanensis, the extraction solution is added, and then the ultrasonic extraction device is used for extracting cephalotaxus hainanensis powder to obtain the first extraction solution, wherein the sulfuric acid aqueous solution or the methanol solution is used as the extraction solvent, so that the economic saving and the environmental friendliness can be realized, and the industrial production can be realized; centrifuging the first extracting solution, pouring out supernatant, repeatedly performing operations of adding an extraction solvent, ultrasonic extraction, centrifugation and pouring out supernatant after centrifugation is finished for 1-4 times, combining the supernatant to obtain a second extracting solution, and successfully separating and purifying the second extracting solution to obtain a small amount of cephalotaxin monomers by adopting a method for separating and purifying cephalotaxin by preparative high performance liquid chromatography.

Detailed Description

In order to make the technical solutions of the present application better understood, the technical solutions in the following embodiments are clearly and completely described, and it is obvious that the described embodiments are only a part of the embodiments of the present application, not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.

Example 1

One embodiment of the present application provides a method for extracting cephalotaxine from cephalotaxus hainanensis, and a method for extracting cephalotaxine from cephalotaxus hainanensis, comprising the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving for later use;

step 2, weighing cephalotaxus hainanensis powder with preset particle size, placing the cephalotaxus hainanensis powder into a centrifugal tube, adding an extraction solvent according to a preset feed-liquid ratio, and placing the cephalotaxus hainanensis powder into an ultrasonic extraction device for ultrasonic extraction to obtain a first extraction solution, wherein the extraction solvent is a sulfuric acid aqueous solution;

step 3, placing the first extracting solution into a centrifugal device for centrifugation, pouring out supernatant after centrifugation is finished, repeatedly adding an extracting solvent, carrying out ultrasonic extraction, centrifugation and pouring out supernatant after centrifugation is finished for 1-4 times, and combining the supernatants to obtain a second extracting solution;

step 5, detecting the content of the cephalotaxine in the second extracting solution through UPLC-MS;

and 6, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Drying picked cephalotaxus hainanensis leaves to constant weight, putting the cephalotaxus hainanensis leaves into a grinder for grinding to obtain brown yellow uniform powder, sieving the brown yellow uniform powder through a 10-200-target standard inspection sieve to obtain cephalotaxus hainanensis powder with different particle sizes, and putting the cephalotaxus hainanensis powder into a 4 ℃ thermostat for storage for later use. In the extraction experiment, cephalotaxus hainanensis powder which is screened by a 10-target standard test sieve is selected in the examples of the application.

Weighing 0.2g of cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 8mL of sulfuric acid aqueous solution (pH 1) according to the material-to-liquid ratio of 1:40, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 30min, the power is 600W, and a first extracting solution is obtained after the ultrasonic treatment is finished; placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, performing ultrasonic extraction, centrifuging, pouring out supernatant after centrifugation is finished for 2 times, combining supernatant obtained by each centrifugation to obtain a second extract, diluting by 5 times, passing through a 0.22-micrometer microporous filter membrane, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 2.33mg/g, and separating and purifying cephalotaxine monomer from the second extract by preparative high performance liquid chromatography.

Example 2

A method for extracting cephalotaxine from cephalotaxus hainanensis includes the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving the crushed cephalotaxus hainanensis leaves with a 10-mesh sieve;

step 2, weighing 0.2g of cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 8mL of sulfuric acid aqueous solution (pH 1) according to the material-liquid ratio of 1:40, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 30min, the power is 600W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 4 times, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 2.49 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 3

A method for extracting cephalotaxine from cephalotaxus hainanensis includes the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving the crushed cephalotaxus hainanensis leaves with a 10-mesh sieve;

step 2, weighing 0.1g of cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 2mL of sulfuric acid aqueous solution (pH 1) according to the material-liquid ratio of 1:20, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 10min, the power is 600W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 1 time, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 2.06 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 4

A method for extracting cephalotaxine from cephalotaxus hainanensis includes the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving the crushed cephalotaxus hainanensis leaves with a 10-mesh sieve;

step 2, weighing 0.1g of cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 3mL of sulfuric acid aqueous solution (pH 1) according to the material-liquid ratio of 1:30, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 10min, the power is 600W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 1 time, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 1.95 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 5

A method for extracting cephalotaxine from cephalotaxus hainanensis includes the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving the crushed cephalotaxus hainanensis leaves with a 10-mesh sieve;

step 2, weighing 0.1g of cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 2mL of sulfuric acid aqueous solution (pH 1) according to the material-liquid ratio of 1:20, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 10min, the power is 480W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 1 time, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 2.32 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 6

A method for extracting cephalotaxine from cephalotaxus hainanensis includes the following steps:

step 1, crushing cephalotaxus hainanensis leaves and then sieving the crushed cephalotaxus hainanensis leaves with a 10-mesh sieve;

step 2, weighing 0.1g of cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 2mL of sulfuric acid aqueous solution (pH 1) according to the material-liquid ratio of 1:20, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 30 ℃, the time is 10min, the power is 480W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 1 time, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 2.05 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 7

Step 1, crushing cephalotaxus hainanensis leaves, and then sieving the crushed cephalotaxus hainanensis leaves with a sieve of 60 meshes and 100 meshes;

step 2, weighing 0.2g of 60-100 mesh cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 8mL of 20% methanol solution (volume fraction, pH 2) according to the material-to-liquid ratio of 1:40, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 30min, the power is 600W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 2 times, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 4.21 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 8

Step 1, crushing cephalotaxus hainanensis leaves, and then sieving the crushed cephalotaxus hainanensis leaves with a sieve of 60 meshes and 100 meshes;

step 2, weighing 0.2g of 60-100 mesh cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 8mL of 50% methanol solution (volume fraction, pH 2) according to the material-to-liquid ratio of 1:40, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 30min, the power is 600W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 2 times, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 4.41 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 9

Step 1, crushing cephalotaxus hainanensis leaves, and then sieving the crushed cephalotaxus hainanensis leaves with a sieve of 60 meshes and 100 meshes;

step 2, weighing 0.2g of 60-100 mesh cephalotaxus hainanensis powder, placing the cephalotaxus hainanensis powder into a 15mL centrifuge tube, adding 8mL of 80% methanol solution (volume fraction, pH 2) according to the material-to-liquid ratio of 1:40, and carrying out ultrasonic extraction under the ultrasonic conditions: the temperature is 28 ℃, the time is 30min, the power is 600W, and a first extracting solution is obtained after the ultrasonic treatment is finished;

and 3, placing the first extracting solution into a centrifugal device for centrifugation, wherein the centrifugation conditions are as follows: rotating at 10000r/min for 5min, pouring out supernatant after centrifugation, repeatedly adding extraction solvent, ultrasonic extracting, centrifuging, pouring out supernatant after centrifugation for 2 times, mixing supernatants obtained by each centrifugation to obtain second extractive solution, diluting by 5 times, and filtering with 0.22 μm microporous membrane;

step 4, detecting the content of cephalotaxine by UPLC-MS, wherein the content of cephalotaxine in cephalotaxus hainanensis is 4.46 mg/g;

and 5, separating and purifying the cephalotaxine monomer from the second extracting solution by using a preparative high performance liquid chromatography separation method.

Example 10

By using a UPLC-MS detection method, taking the experimental data of the embodiments 1-6, and obtaining experimental data tables with different cephalotaxus hainanensis content in cephalotaxus hainanensis according to the differences of cephalotaxus hainanensis powder gram number, material-liquid ratio, sulfuric acid aqueous solution volume, ultrasonic temperature, ultrasonic time, ultrasonic power and repetition times, as shown in Table 1.

TABLE 1

And (4) conclusion: as can be seen from Table 1, in example 1, the gram number of cephalotaxus hainanensis powder, the ratio of the material to the liquid, the volume of the sulfuric acid aqueous solution, the ultrasonic temperature, the ultrasonic time and the ultrasonic power were the same as those in example 2, and the more the number of repetition, the higher the content of cephalotaxine was measured.

Example 3 compared with example 4, the gram number of cephalotaxus hainanensis powder, the ultrasonic temperature, the ultrasonic time, the ultrasonic power and the repetition times are the same, and the smaller the feed-liquid ratio is, the higher the content of cephalotaxine is measured.

In example 3, compared with example 5, the gram number of cephalotaxus hainanensis powder, the ratio of material to liquid, the volume of the sulfuric acid aqueous solution, the ultrasonic temperature, the ultrasonic time and the repetition times are the same, and the lower the ultrasonic power, the higher the content of the cephalotaxine is measured.

Example 5 compared with example 6, the gram number of cephalotaxus hainanensis powder, the ratio of material to liquid, the volume of the sulfuric acid aqueous solution, the ultrasonic time, the ultrasonic power and the repetition times are all the same, and the higher the ultrasonic temperature is, the lower the content of cephalotaxine is measured.

Example 11

By using the UPLC-MS detection method, the experimental data of examples 7-9, the experimental data tables of different cephalotaxus hainanensis content in cephalotaxus hainanensis are shown in Table 2, wherein the experimental data are obtained under the condition that the number of grams of cephalotaxus hainanensis powder, the material-liquid ratio, the volume of the methanol solution, the ultrasonic temperature, the ultrasonic time, the ultrasonic power and the repetition times are the same, and the volume fraction of methanol is different.

TABLE 2

And (4) conclusion: as can be seen from Table 2, in examples 7 and 8, the grams of cephalotaxus hainanensis powder, the feed-to-liquid ratio, the volume of the methanol solution and the number of repetitions were all the same as in example 9, while the higher the volume fraction of methanol was, the higher the content of cephalotaxin measured, and comparative analysis was conducted in conjunction with Table 1, it was found that the content of cephalotaxin measured using the methanol solution was higher than that measured using the sulfuric acid aqueous solution.

According to the method for extracting cephalotaxus from cephalotaxus hainanensis provided in the embodiment of the application, the extraction solvent is added, and then the ultrasonic extraction device is used for extracting cephalotaxus hainanensis powder to obtain the first extraction solution, wherein the sulfuric acid aqueous solution or the methanol solution is used as the extraction solvent, so that the economic saving and the environmental friendliness can be realized, and the industrial production can be realized; centrifuging the first extracting solution, pouring out supernatant, repeatedly performing operations of adding an extraction solvent, ultrasonic extraction, centrifugation and pouring out supernatant after centrifugation is finished for 1-4 times, combining the supernatant to obtain a second extracting solution, and successfully separating and purifying the second extracting solution to obtain a small amount of cephalotaxin monomers by adopting a method for separating and purifying cephalotaxin by preparative high performance liquid chromatography.

The above embodiments are only used for illustrating the technical solutions of the present application, and not for limiting the same; although the present application has been described in detail with reference to the foregoing embodiments, it should be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions in the embodiments of the present application.