Method for extracting active substances of pseudoxanthium sibiricum

Abstract

The invention discloses a method for extracting active substances of pseudostellaria heterophylla. The extraction method comprises the following steps: (1) pretreating pseudoxanthium sibiricum leaves to obtain pseudoxanthium sibiricum leaf powder; (2) mixing the obtained pseudoxanthium sibiricum leaf powder with an extracting agent, and carrying out reflux extraction at 40-80 DEG C under an ultrasonic condition; (3) filtering the extracting solution, collecting filtrate, and adding a dehydrating agent into the filtrate for freezing; and (4) removing the dehydrating agent in the filtrate and then removing the extracting agent to obtain the xanthium sibiricum active substance. The extraction method overcomes the defects in the prior art, and has the advantages of low cost, high yield, simplicity in operation, short operation time and the like.

Description

Technical Field

[0001] The invention relates to a method for extracting plant active substances, in particular to a method for extracting Xanthium sibiricum active substances from Xanthium sibiricum leaves, and belongs to the field of extraction of plant active substances. Background Art

[0002] Cyclachaena xanthiifolia (Nutt.) Fresen. is an annual herbaceous plant of the Asteraceae family and the genus Cyclachaena. It has the characteristics of rapid settlement, rapid growth, rapid spread and the production of a large number of seeds, which ensures that Cyclachaena xanthiifolia is in an advantageous position in the natural competition process. After the successful invasion of Cyclachaena xanthiifolia, it willfully squeezed out native plants, occupied forest wasteland, affected the growth and renewal of flowers, plants and trees, and gradually invaded the crop area, affecting the growth of crops and reducing the quality and yield of agricultural products. In recent years, domestic and foreign scholars have studied the chemical composition of Cyclachaena xanthiifolia by TLC, HPLC, GC-MS and other methods, and found that it contains a variety of active substances, mainly including esters, coumarins, fatty acids, sugars, sterols, polyphenols, polysaccharides, proteins and other categories, and also contains other components, such as alkanes, alkaloids, terpenes, phenolic acids, flavonoids and the like. With the help of modern science and technology, the active substances of Cyclachaena xanthiifolia have been widely used in daily chemical products, herbicides, pesticides, biosorbents, feed processing, medicine and other industries.

[0003] At present, the extraction methods of active substances from Xanthium sibiricum usually adopt chromatography, water extraction, extraction, resin method and precipitation method. The yield of active substances obtained is not high, and it is time-consuming, complex, harsh, and takes a long time to operate. Therefore, providing a method for extracting active substances from Xanthium sibiricum with low cost, high yield, simple operation and short operation time is the key to solving this problem. Summary of the invention

[0004] The main purpose of the invention is to provide a method for extracting Xanthium sibiricum active substances from Xanthium sibiricum leaves, which has the advantages of low cost, high yield, simple operation, short operation time and the like.

[0005] To achieve the above object, the technical solution adopted by the present invention includes:

[0006] A method for extracting active substances from Xanthium sibiricum, comprising:

[0007] (1) pre-treating Xanthium sibiricum leaves to obtain Xanthium sibiricum leaf powder; (2) mixing the obtained Xanthium sibiricum leaf powder with an extractant and performing reflux extraction at 40-80° C. under ultrasonic conditions; (3) filtering the extract to collect the filtrate, adding a dehydrating agent to the filtrate and freezing it; (4) removing the dehydrating agent from the filtrate and then removing the extractant to obtain the Xanthium sibiricum active substance.

[0008] In a preferred embodiment of the present invention, the method of pre-treating the Xanthium sibiricum leaves to obtain the Xanthium sibiricum leaf powder in step (1) comprises: drying the Xanthium sibiricum leaves, crushing them, and sieving them; wherein the drying method is preferably shade drying, and the sieving is performed using a 40-mesh sieve.

[0009] In a preferred embodiment of the present invention, in step (2), the obtained Xanthium sibiricum leaf powder is mixed with an extractant and subjected to reflux extraction at 60° C. under ultrasonic conditions.

[0010] In a preferred embodiment of the present invention, the ultrasonic power of the ultrasonic condition in step (2) is 200-400W, and most preferably, the ultrasonic power of the ultrasonic condition is 300W.

[0011] In a preferred embodiment of the present invention, the extractant in step (2) is ethanol with a volume fraction of 30% to 70% (v / v), and preferably, the extractant is 60% ethanol.

[0012] In a preferred embodiment of the present invention, in step (2), the Xanthium sibiricum leaf powder and the extractant are mixed at a ratio of 1:(20-35) in terms of g:ml; most preferably, the Xanthium sibiricum leaf powder and the extractant are mixed at a ratio of 1:30.

[0013] In a preferred embodiment of the present invention, the reflux extraction time in step (2) is 120-240 min, and most preferably, the reflux extraction time is 180 min.

[0014] In a preferred embodiment of the present invention, the dehydrating agent in step (3) is anhydrous sodium sulfate.

[0015] In a preferred embodiment of the present invention, the freezing temperature in step (3) is -20°C; the freezing time can be 4-24 hours, preferably 8-12 hours.

[0016] In a preferred embodiment of the present invention, in step (4), a rotary evaporator is used to remove the extractant in the filtrate; wherein the operating temperature of the rotary evaporator is preferably 50°C.

[0017] According to the extraction test results of Examples 1-10, it can be seen that in Example 8, when the solid-liquid ratio is 1 g:30 mL, the extractant is 60% ethanol, and the reflux extraction time is 180 min, the extraction rate of the active substance of Xanthium sibiricum is 32.5%; compared with other examples, the extraction rate of the active substance of Xanthium sibiricum in Example 8 is at least increased by 31 percentage points; therefore, the optimal extraction parameters during the reflux extraction in step (2) of the present invention are: the solid-liquid ratio is 1 g:30 mL, the extractant is 60% ethanol, and the reflux extraction time is 180 min.

[0018] Compared with the prior art, the present invention mainly has the following beneficial effects:

[0019] The method of the invention has low cost, high yield, simple operation, short operation time, and the added auxiliary agent is a conventional raw material with a small amount and a small content in the finished product. The promotion and application of the method of the invention will play an important role in promoting the further utilization of the active substances of Xanthium sibiricum and the development of related industries. DETAILED DESCRIPTION

[0020] The present invention will be further described below in conjunction with specific embodiments, and the advantages and features of the present invention will become clearer as the description proceeds. However, it should be understood that the embodiments are exemplary only and do not constitute any limitation to the scope of the present invention. It should be understood by those skilled in the art that the details and forms of the technical solution of the present invention may be modified or replaced without departing from the spirit and scope of the present invention, but these modifications or replacements all fall within the protection scope of the present invention.

[0021] Example 1 Extraction of Xanthium sibiricum Active Substances

[0022] (1) drying the Xanthium sibiricum leaf raw material in the shade, crushing it, and sieving it through a 40-mesh sieve to obtain Xanthium sibiricum leaf powder;

[0023] (2) According to the solid-liquid ratio of 1 g: 20 mL, 5 g of Xanthium sibiricum leaf powder and 100 mL of 60% ethanol by volume were fully mixed to obtain a solution to be extracted; the solution to be extracted was placed in an ultrasonic water bath with a water bath temperature of 60° C. and an ultrasonic power of 300 W for cooling and reflux extraction for 180 min; after reflux in the water bath, the filtrate was filtered and collected, and an extraction solvent (i.e., 60% ethanol) of the same volume and concentration was added to the filter residue, and the extraction was repeated 3 times, and the filtrate collected by the extraction was combined;

[0024] (3) Add anhydrous sodium sulfate to the filtrate to absorb moisture, and transfer to a -20°C refrigerator and freeze overnight;

[0025] (4) filtering the anhydrous sodium sulfate in the filtrate after freezing overnight, transferring the filtrate to a rotary evaporator and evaporating the extractant ethanol at a temperature of 50° C. to obtain the Xanthium sibiricum active substance;

[0026] After testing and calculation, the extraction rate of active substances in the Xanthium sibiricum of this embodiment was 20.7%.

[0027] Example 2 Extraction of Xanthium sibiricum Active Substances

[0028] The difference from Example 1 is that the volume fraction of ethanol in step (2) is 70%; the rest is the same as Example 1.

[0029] After testing and calculation, the extraction rate of the active substance of Xanthium sibiricum in this example was 22.0%.

[0030] Example 3 Extraction of Xanthium sibiricum Active Substances

[0031] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:25 mL, the volume fraction of ethanol is 30%, and the ultrasonic extraction time is 120 min; the rest is the same as Example 1.

[0032] After testing and calculation, the extraction rate of the active substance of Xanthium sibiricum in this example was 17.6%.

[0033] Example 4 Extraction of Xanthium sibiricum Active Substances

[0034] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:25 mL; the rest is the same as Example 1.

[0035] After testing and calculation, the extraction rate of the active substance of Xanthium sibiricum in this example was 22.4%.

[0036] Example 5 Extraction of Xanthium sibiricum Active Substances

[0037] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:30 mL, the volume fraction of ethanol is 30%, and the ultrasonic extraction time is 120 min; the rest is the same as Example 1.

[0038] After testing and calculation, the extraction rate of active substances in the Xanthium sibiricum of this embodiment was 20.2%.

[0039] Example 6 Extraction of Xanthium sibiricum Active Substances

[0040] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:30 mL, and the volume fraction of ethanol is 30%; the rest is the same as Example 1.

[0041] After testing and calculation, the extraction rate of active substances in the Xanthium sibiricum of this embodiment was 20.4%.

[0042] Example 7 Extraction of Xanthium sibiricum Active Substances

[0043] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:30 mL, and the ultrasonic extraction time is 120 min; the rest is the same as Example 1.

[0044] After testing and calculation, the extraction rate of active substances in the Xanthium sibiricum of this embodiment was 24.8%.

[0045] Example 8 Extraction of Xanthium sibiricum Active Substances

[0046] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:30 mL; the rest is the same as Example 1.

[0047] After testing and calculation, the extraction rate of the active substance of Xanthium sibiricum in this example was 32.5%.

[0048] Example 9 Extraction of Xanthium sibiricum Active Substances

[0049] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:35 mL, and the ultrasonic extraction time is 120 min; the rest is the same as Example 1.

[0050] After testing and calculation, the extraction rate of the active substance of Xanthium sibiricum in this example was 21.0%.

[0051] Example 10 Extraction of Xanthium sibiricum Active Substances

[0052] The difference from Example 1 is that in step (2), the material-liquid ratio is 1 g:35 mL, and the ultrasonic extraction time is 240 min; the rest is the same as Example 1.

[0053] After testing and calculation, the extraction rate of the active substance of Xanthium sibiricum in this example was 22.4%.

[0054] The summary results of the reflux extraction parameters and extraction rates in Examples 1-10 are shown in Table 1.

[0055] The summary is shown in Table 1 below.

[0056] Table 1 Experimental results

[0057]

[0058] According to the test results in Table 1, it can be seen that in Example 8, when the solid-liquid ratio is 1 g: 30 mL, the extractant is 60% ethanol, and the reflux extraction time is 180 min, the extraction rate of the active substance of Xanthium sibiricum is 32.5%; compared with other embodiments, the extraction rate of the active substance of Xanthium sibiricum in Example 8 is at least increased by 31 percentage points. Therefore, the optimal extraction parameters of the present invention during reflux extraction are: the solid-liquid ratio is 1 g: 30 mL, the extractant is 60% ethanol, and the reflux extraction time is 180 min.

Claims

1. A method for extracting active substances from Xanthium sibiricum, characterized in that: include: (1) pre-treating Xanthium sibiricum leaves to obtain Xanthium sibiricum leaf powder; (2) mixing the obtained Xanthium sibiricum leaf powder with an extractant and performing reflux extraction at 40-80° C. under ultrasonic conditions; (3) filtering the extract to collect the filtrate, adding a dehydrating agent to the filtrate and freezing it; (4) removing the dehydrating agent from the filtrate and then removing the extractant to obtain the Xanthium sibiricum active substance.

2. The extraction method according to claim 1, characterized in that The method of pre-treating the Xanthium sibiricum leaves to obtain the Xanthium sibiricum leaf powder in step (1) comprises: drying the Xanthium sibiricum, crushing it, and sieving it; wherein the drying method is preferably shade drying, and the sieving is performed using a 40-mesh sieve.

3. The extraction method according to claim 1, characterized in that In step (2), the Xanthium sibiricum leaf powder is mixed with an extractant and subjected to reflux extraction at 60° C. under ultrasonic conditions.

4. The extraction method according to claim 1 or 3, characterized in that The ultrasonic power of the ultrasonic condition is 200-400W, preferably, the ultrasonic power of the ultrasonic condition is 300W.

5. The extraction method according to claim 1 or 3, characterized in that The extractant in step (2) is 30% to 70% ethanol, preferably, the extractant is 60% ethanol.

6. The extraction method according to claim 1 or 3, characterized in that In terms of g:ml, in step (2), the Xanthium sibiricum leaf powder and the extractant are mixed in a ratio of 1:(20-35); preferably, the Xanthium sibiricum leaf powder and the extractant are mixed in a ratio of 1:

30.

7. The extraction method according to claim 1 or 3, characterized in that The reflux extraction time in step (2) is 120-240 min. Preferably, the reflux extraction time in step (2) is 180 min.

8. The extraction method according to claim 1, characterized in that The dehydrating agent described in step (3) is anhydrous sodium sulfate.

9. The extraction method according to claim 1, characterized in that The freezing temperature in step (3) is -20°C; the freezing time is 4-24 hours, preferably 8-12 hours.

10. The extraction method according to claim 1, characterized in that In step (4), a rotary evaporator is used to remove the extractant in the filtrate; wherein the temperature of the rotary evaporator during operation is 50°C.

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