阅读说明：本技术 一种天然槟榔碱提取方法 (Method for extracting natural arecoline ) 是由 史载锋 张大帅 张小朋 韩立志 于 2020-10-26 设计创作，主要内容包括：本发明公开了一种天然槟榔碱提取方法。本发明中,本发明涉及一种从槟榔中提取槟榔碱的方法：用氢溴酸与槟榔提取液中的槟榔碱反应,使之生成槟榔碱氢溴酸盐；槟榔碱氢溴酸盐是一种白色的结晶体,将槟榔碱氢溴酸盐分离出来后,再利用沉淀反应法使槟榔碱氢溴酸盐脱溴,从而可以得油状液态槟榔碱。采用了本方法,可以将槟榔碱和槟榔次碱进行分离,从而提高了槟榔碱的产品纯度,避免了其内部混入的槟榔次碱对槟榔碱的质量造成影响；槟榔碱氢溴酸盐分离出来后,再利用沉淀反应法使槟榔碱氢溴酸盐脱溴,从而可以得油状液态槟榔碱,该操作相对于常规操作,操作更加简便易行,减少了工作人员的操作负担。(The invention discloses a method for extracting natural arecoline. The invention relates to a method for extracting arecoline from areca, which comprises the following steps: reacting hydrobromic acid with arecoline in the areca extract to generate arecoline hydrobromide; the arecoline hydrobromide is a white crystal, which is separated out and then debrominated by a precipitation reaction method, so as to obtain oily liquid arecoline. By adopting the method, the arecoline and the arecoline can be separated, so that the product purity of the arecoline is improved, and the influence of the arecoline mixed in the arecoline on the quality of the arecoline is avoided; after the arecoline hydrobromide is separated out, the arecoline hydrobromide is debrominated by a precipitation reaction method, so that oily liquid arecoline can be obtained.)

1. A method for extracting natural arecoline is characterized by comprising the following steps: the natural arecoline extraction method needs to use the following raw materials and properties: 1-3 kg of betel nut sample, 2-4L of absolute ethyl alcohol, carbon tetrachloride, concentrated ammonia water, anhydrous sodium sulfate powder, activated carbon powder and 4% AgNO 3. Ethanol solution, 48% hydrobromic acid, one refrigerator, one grinder, one filter device and one PH detector.

2. The method for extracting arecoline according to claim 1, wherein: the method for extracting the natural arecoline comprises the following steps:

s1, taking one grinding machine, adding 1-3 kg of betel nut sample into the grinding machine, then preparing 1-3 kg of ground betel nut sample, heating and refluxing for 1h by using 2L of absolute ethyl alcohol, and filtering to obtain an extracting solution;

s2, after the step S1 is finished, recovering the remaining ethanol, standing the concentrated solution for cooling, adding concentrated ammonia water after the concentrated solution is completely cooled, adding the concentrated ammonia water into the concentrated solution, detecting the concentrated solution by using a PH detector while adding the concentrated ammonia water, and stopping adding the ammonia water until the pH is adjusted to be = 10;

s3, carrying out water bath on the concentrated solution prepared in the step S2, and then concentrating under reduced pressure to obtain total alkali; heating and dissolving total alkali in 50mL of absolute ethyl alcohol, cooling, adding 48% hydrobromic acid into the interior of the compression coat, and detecting the pH value by using a pH detector until the pH value is = 4;

s4, drying the solution obtained in the step S4 by using anhydrous sodium sulfate, concentrating the solution to 10mL in a water bath, placing the solution in a refrigerator, and standing the solution for a period of time to obtain yellowish arecoline hydrobromide crystals;

s5, heating and dissolving the crystal obtained in the step S4 in 100mL of absolute ethyl alcohol, adding 10g of activated carbon into the crystal for decoloring, refluxing for 0.5h by a water bath heating method, and then filtering;

s6, washing the activated carbon with hot absolute ethyl alcohol for 2 times, concentrating and cooling again to separate out crystals to obtain white arecoline hydrobromide;

s7: heating and dissolving arecoline hydrobromide in anhydrous ethanol, dropwise adding 4% AgNO3 and ethanol solution (90% ethanol and 10% water), and filtering to obtain precipitate;

s8: distilling the solution obtained in the step S7 again to obtain reddish brown oily arecoline, and collecting the reddish brown oily arecoline obtained by secondary distillation.

3. The method for extracting arecoline according to claim 1, wherein: in step S1, the residue left after the primary filtration is extracted 3 times as above, and the extract liquid obtained by each filtration is collected, and the four finally collected extract liquids are combined and stored.

4. The method for extracting arecoline according to claim 1, wherein: in the step S2, during the process of adding ammonia water, carbon tetrachloride may be added into the concentrated solution, and a glass stirring rod may be used to perform multiple stirring extractions, and the extracted solution may be dried with anhydrous sodium sulfate after the extraction.

5. The method for extracting arecoline according to claim 1, wherein: the arecoline obtained in the step S6 can form an ion pair with the bromosylvite green, the ion pair can be quantitatively extracted by chloroform, and the bromosylvite green can be dissociated and separated out for color development after potassium hydroxide absolute ethyl alcohol solution is added, so that the absorbance of the solution at the wavelength of 618nm can be detected by adopting a spectrophotometry, and the purity of the arecoline can be determined according to a standard curve method.

6. The method for extracting arecoline according to claim 1, wherein: in step S8, 1Kg of fresh betel nut is dried in a drying oven at 80 ℃ to 0.5Kg of dry betel nut, arecoline is extracted according to the experimental method, and compared with the fresh betel nut, when the fresh betel nut is dried, the arecoline content is reduced by about 53%, which is caused by the evaporation of arecoline with water vapor during the drying process.

Technical Field

The invention belongs to the technical field of alkaloid extraction, and particularly relates to a method for extracting natural arecoline.

Background

The arecoline in the areca has important bactericidal action, and the content of the arecoline is about 0.1 to 0.5 percent. At present, the arecoline is extracted by an organic solvent or polar solution, but the arecoline can be mixed and dissolved with water, ethanol and the like in any proportion, is a yellow oily liquid and is very easy to oxidize, and particularly the arecoline and the arecoline have similar structures and can not be separated by a conventional method, so that the high-purity arecoline is difficult to obtain.

As the arecoline is an oily product, the content of the arecoline in the areca is very low (0.1-0.5 percent) and the arecoline is easy to oxidize, and particularly the arecoline and the arecoline have similar structures and can not be separated by a conventional method, the membrane separation or resin adsorption column or distillation process is adopted in the extraction method, so that the high-purity arecoline is difficult to obtain. In view of the problems, the inventors have invented a method for obtaining high-purity arecoline with simple separation operation.

Disclosure of Invention

The invention aims to: in order to solve the problems, a method for extracting natural arecoline is provided.

The technical scheme adopted by the invention is as follows: a method for extracting natural arecoline needs to use the following raw materials and properties: 1-3 kg of betel nut sample, 2-4L of absolute ethyl alcohol, carbon tetrachloride, concentrated ammonia water, anhydrous sodium sulfate powder, activated carbon powder and 4% AgNO 3. Ethanol solution, 48% hydrobromic acid, one refrigerator, one grinder, one filter device and one PH detector.

In a preferred embodiment, the method for extracting natural arecoline comprises the following steps:

s1, taking one grinding machine, adding 1-3 kg of betel nut sample into the grinding machine, then preparing 1-3 kg of ground betel nut sample, heating and refluxing for 1h by using 2L of absolute ethyl alcohol, and filtering to obtain an extracting solution;

s2, after the step S1 is finished, recovering the remaining ethanol, standing the concentrated solution for cooling, adding concentrated ammonia water after the concentrated solution is completely cooled, adding the concentrated ammonia water into the concentrated solution, detecting the concentrated solution by using a pH detector while adding the concentrated ammonia water, and stopping adding the ammonia water until the pH value is adjusted to 10;

s3, carrying out water bath on the concentrated solution prepared in the step S2, and then concentrating under reduced pressure to obtain total alkali; heating and dissolving total alkali in 50mL of absolute ethyl alcohol, cooling, adding 48% hydrobromic acid into the interior of the compression coat, and detecting the pH value to be 4 by using a pH detector;

s4, drying the solution obtained in the step S4 by using anhydrous sodium sulfate, concentrating the solution to 10mL in a water bath, placing the solution in a refrigerator, and standing the solution for a period of time to obtain yellowish arecoline hydrobromide crystals;

s5, heating and dissolving the crystal obtained in the step S4 in 100mL of absolute ethyl alcohol, adding 10g of activated carbon into the crystal for decoloring, refluxing for 0.5h by a water bath heating method, and then filtering;

s6, washing the activated carbon with hot absolute ethyl alcohol for 2 times, concentrating and cooling again to separate out crystals to obtain white arecoline hydrobromide;

s7: heating and dissolving arecoline hydrobromide in absolute ethyl alcohol, and dropwise adding AgNO3 with the mass fraction of 4%. Ethanol solution (90% ethanol, 10% water), filtering the precipitate;

s8: distilling the solution obtained in the step S7 again to obtain reddish brown oily arecoline, and collecting the reddish brown oily arecoline obtained by secondary distillation.

In a preferred embodiment, in step S1, the residue left after the primary filtration is extracted 3 times as above, the extract obtained from each filtration is collected, and the four finally collected extracts are combined and stored.

In a preferred embodiment, in the step S2, during the adding of the ammonia water, carbon tetrachloride may be added into the concentrated solution, and the concentrated solution may be extracted with stirring for a plurality of times by using a glass stirring rod, and the extract may be dried with anhydrous sodium sulfate after the extraction.

In a preferred embodiment, the arecoline obtained in step S6 may form an ion pair with the bromosyllabinol green, and the ion pair may be quantitatively extracted by chloroform. After the potassium hydroxide absolute ethyl alcohol solution is added, the bromopotassium phenol green can be dissociated to separate out color, so that the absorbance of the solution at the wavelength of 618nm can be detected by adopting a spectrophotometry method. And determining the purity of the arecoline according to a standard curve method.

In a preferred embodiment, in step S8, 1Kg of fresh betel nut is taken and dried in an oven at 80 ℃ to 0.5Kg of dry betel nut, arecoline is extracted according to the experimental method, and compared with the fresh betel nut, when the fresh betel nut is dried, the arecoline content is reduced by about 53%, because the arecoline is evaporated with water vapor during the drying process.

In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:

1. according to the method, the arecoline and the arecoline can be separated, so that the product purity of the arecoline is improved, and the influence of the arecoline mixed in the arecoline on the quality of the arecoline is avoided.

2. In the invention, after the arecoline hydrobromide is separated out, the arecoline hydrobromide is debrominated by a precipitation reaction method, so that oily liquid arecoline can be obtained.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but 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 invention.

The first embodiment is as follows:

a method for extracting natural arecoline needs to use the following raw materials and properties: 1-3 kg of betel nut sample, 2-4L of absolute ethyl alcohol, carbon tetrachloride, concentrated ammonia water, anhydrous sodium sulfate powder, activated carbon powder and 4% AgNO 3. Ethanol solution, 48% hydrobromic acid, one refrigerator, one grinder, one filter device and one PH detector.

The method for extracting the natural arecoline comprises the following steps:

s1, taking one grinding machine, adding 1kg of betel nut sample into the grinding machine, then preparing 1kg of ground betel nut sample, heating and refluxing for 1h by using 2L of absolute ethyl alcohol, filtering to obtain an extracting solution, extracting the residue left after primary filtering for 3 times in the step S1 by the method, collecting the extracting solution filtered each time, and merging and storing the four finally collected extracting solutions;

s2, after the step S1 is finished, recovering the remaining ethanol, standing the concentrated solution for cooling, adding concentrated ammonia water after the concentrated solution is completely cooled, adding the concentrated ammonia water into the concentrated solution, detecting the concentrated solution by using a pH detector while adding the concentrated ammonia water, stopping adding the ammonia water until the pH value is adjusted to 10, in the step S2, adding carbon tetrachloride into the concentrated solution in the ammonia water adding process, simultaneously stirring and extracting for multiple times by using a glass stirring rod, and drying the extracting solution after extracting by using anhydrous sodium sulfate;

s3, carrying out water bath on the concentrated solution prepared in the step S2, and then concentrating under reduced pressure to obtain total alkali; heating and dissolving total alkali in 50mL of absolute ethyl alcohol, cooling, adding 48% hydrobromic acid into the interior of the compression coat, and detecting the pH value to be 4 by using a pH detector;

s4, drying the solution obtained in the step S4 by using anhydrous sodium sulfate, concentrating the solution to 10mL in a water bath, placing the solution in a refrigerator, and standing the solution for a period of time to obtain yellowish arecoline hydrobromide crystals;

s5, heating and dissolving the crystal obtained in the step S4 in 100mL of absolute ethyl alcohol, adding 10g of activated carbon into the crystal for decoloring, refluxing for 0.5h by a water bath heating method, and then filtering;

s6, washing the activated carbon with hot absolute ethyl alcohol for 2 times, concentrating and cooling again, and precipitating crystals to obtain white arecoline hydrobromide, wherein the arecoline obtained in the step S6 can form an ion pair with potassium bromate green, and the ion pair can be quantitatively extracted by chloroform. After the potassium hydroxide absolute ethyl alcohol solution is added, the bromopotassium phenol green can be dissociated to separate out color, so that the absorbance of the solution at the wavelength of 618nm can be detected by adopting a spectrophotometry method. Determining the purity of the arecoline according to a standard curve method;

s7: heating and dissolving arecoline hydrobromide in absolute ethyl alcohol, and dropwise adding AgNO3 with the mass fraction of 4%. Ethanol solution (90% ethanol, 10% water), filtering the precipitate

S8: distilling the solution obtained in the step S7 again to obtain reddish brown oily arecoline, and then distilling again to obtain reddish brown oily arecoline, and collecting the reddish brown oily arecoline to finish the preparation of the process, wherein in the step S8, 1Kg of fresh areca is dried in a drying oven at 80 ℃ to 0.5Kg of dried areca, arecoline is extracted according to the experimental method, and compared with the fresh areca, when the fresh areca is dried, the arecoline content is reduced by about 53 percent, which is caused by the evaporation of water vapor in the drying process.

Example two:

a method for extracting natural arecoline needs to use the following raw materials and properties: 1-3 kg of betel nut sample, 2-4L of absolute ethyl alcohol, carbon tetrachloride, concentrated ammonia water, anhydrous sodium sulfate powder, activated carbon powder and 4% AgNO 3. Ethanol solution, 48% hydrobromic acid, one refrigerator, one grinder, one filter device and one PH detector.

The method for extracting the natural arecoline comprises the following steps:

s1, taking one grinding machine, adding 1kg of betel nut sample into the grinding machine, then preparing 2kg of ground betel nut sample, heating and refluxing for 1h by using 4L of absolute ethyl alcohol, filtering to obtain an extracting solution, extracting the residue left after primary filtering for 3 times in the step S1 by the method, collecting the extracting solution filtered each time, and merging and storing the four finally collected extracting solutions;

s2, after the step S1 is finished, recovering the remaining ethanol, standing the concentrated solution for cooling, adding concentrated ammonia water after the concentrated solution is completely cooled, adding the concentrated ammonia water into the concentrated solution, detecting the concentrated solution by using a pH detector while adding the concentrated ammonia water, stopping adding the ammonia water until the pH value is adjusted to 10, in the step S2, adding carbon tetrachloride into the concentrated solution in the ammonia water adding process, simultaneously stirring and extracting for multiple times by using a glass stirring rod, and drying the extracting solution after extracting by using anhydrous sodium sulfate;

s3, carrying out water bath on the concentrated solution prepared in the step S2, and then concentrating under reduced pressure to obtain total alkali; heating and dissolving total alkali in 50mL of absolute ethyl alcohol, cooling, adding 48% hydrobromic acid into the interior of the compression coat, and detecting the pH value to be 4 by using a pH detector;

s4, drying the solution obtained in the step S4 by using anhydrous sodium sulfate, concentrating the solution to 10mL in a water bath, placing the solution in a refrigerator, and standing the solution for a period of time to obtain yellowish arecoline hydrobromide crystals;

s5, heating and dissolving the crystal obtained in the step S4 in 100mL of absolute ethyl alcohol, adding 10g of activated carbon into the crystal for decoloring, refluxing for 0.5h by a water bath heating method, and then filtering;

s6, washing the activated carbon with hot absolute ethyl alcohol for 2 times, concentrating and cooling again, and precipitating crystals to obtain white arecoline hydrobromide, wherein the arecoline obtained in the step S6 can form an ion pair with potassium bromate green, and the ion pair can be quantitatively extracted by chloroform. After the potassium hydroxide absolute ethyl alcohol solution is added, the bromopotassium phenol green can be dissociated to separate out color, so that the absorbance of the solution at the wavelength of 618nm can be detected by adopting a spectrophotometry method. Determining the purity of the arecoline according to a standard curve method;

s7: heating and dissolving arecoline hydrobromide in absolute ethyl alcohol, and dropwise adding AgNO3 with the mass fraction of 4%. Ethanol solution (90% ethanol, 10% water), filtering the precipitate

S8: distilling the solution obtained in the step S7 again to obtain reddish brown oily arecoline, and then distilling again to obtain reddish brown oily arecoline, and collecting the reddish brown oily arecoline to finish the preparation of the process, wherein in the step S8, 1Kg of fresh areca is dried in a drying oven at 80 ℃ to 0.5Kg of dried areca, arecoline is extracted according to the experimental method, and compared with the fresh areca, when the fresh areca is dried, the arecoline content is reduced by about 53 percent, which is caused by the evaporation of water vapor in the drying process.

Example three:

a method for extracting natural arecoline needs to use the following raw materials and properties: 1-3 kg of betel nut sample, 2-4L of absolute ethyl alcohol, carbon tetrachloride, concentrated ammonia water, anhydrous sodium sulfate powder, activated carbon powder and 4% AgNO 3. Ethanol solution, 48% hydrobromic acid, one refrigerator, one grinder, one filter device and one PH detector.

The method for extracting the natural arecoline comprises the following steps:

s1, taking one grinding machine, adding 1kg of betel nut sample into the grinding machine, then preparing 3kg of ground betel nut sample, heating and refluxing for 1h by using 6L of absolute ethyl alcohol, filtering to obtain an extracting solution, extracting the residue left after primary filtering for 3 times in the step S1 by the method, collecting the extracting solution filtered each time, and merging and storing the four finally collected extracting solutions;

s2, after the step S1 is finished, recovering the remaining ethanol, standing the concentrated solution for cooling, adding concentrated ammonia water after the concentrated solution is completely cooled, adding the concentrated ammonia water into the concentrated solution, detecting the concentrated solution by using a pH detector while adding the concentrated ammonia water, stopping adding the ammonia water until the pH value is adjusted to 10, in the step S2, adding carbon tetrachloride into the concentrated solution in the ammonia water adding process, simultaneously stirring and extracting for multiple times by using a glass stirring rod, and drying the extracting solution after extracting by using anhydrous sodium sulfate;

s3, carrying out water bath on the concentrated solution prepared in the step S2, and then concentrating under reduced pressure to obtain total alkali; heating and dissolving total alkali in 50mL of absolute ethyl alcohol, cooling, adding 48% hydrobromic acid into the interior of the compression coat, and detecting the pH value to be 4 by using a pH detector;

s4, drying the solution obtained in the step S4 by using anhydrous sodium sulfate, concentrating the solution to 10mL in a water bath, placing the solution in a refrigerator, and standing the solution for a period of time to obtain yellowish arecoline hydrobromide crystals;

s5, heating and dissolving the crystal obtained in the step S4 in 100mL of absolute ethyl alcohol, adding 10g of activated carbon into the crystal for decoloring, refluxing for 0.5h by a water bath heating method, and then filtering;

s6, washing the activated carbon with hot absolute ethyl alcohol for 2 times, concentrating and cooling again, and precipitating crystals to obtain white arecoline hydrobromide, wherein the arecoline obtained in the step S6 can form an ion pair with potassium bromate green, and the ion pair can be quantitatively extracted by chloroform. After the potassium hydroxide absolute ethyl alcohol solution is added, the bromopotassium phenol green can be dissociated to separate out color, so that the absorbance of the solution at the wavelength of 618nm can be detected by adopting a spectrophotometry method. Determining the purity of the arecoline according to a standard curve method;

s7: heating and dissolving arecoline hydrobromide in absolute ethyl alcohol, and dropwise adding AgNO3 with the mass fraction of 4%. Ethanol solution (90% ethanol, 10% water), filtering the precipitate

S8: distilling the solution obtained in the step S7 again to obtain reddish brown oily arecoline, and then distilling again to obtain reddish brown oily arecoline, and collecting the reddish brown oily arecoline to finish the preparation of the process, wherein in the step S8, 1Kg of fresh areca is dried in a drying oven at 80 ℃ to 0.5Kg of dried areca, arecoline is extracted according to the experimental method, and compared with the fresh areca, when the fresh areca is dried, the arecoline content is reduced by about 53 percent, which is caused by the evaporation of water vapor in the drying process.

It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Moreover, the terms "comprises," "comprising," or 014, and any other variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising an … …" does not exclude the presence of other identical elements in a process, method, article, or apparatus that comprises the element.

The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will 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 of the embodiments of the present invention.