Method for targeted extraction of nicotine in waste tobacco powder by ionic liquid

Abstract

The invention belongs to the technical field of tobacco chemistry, and particularly discloses a method for targeted extraction of nicotine in waste tobacco powder by using ionic liquid as a solvent, and the method comprises the following steps: preparing extract liquor; sieving and drying the tobacco powder, placing the tobacco powder in a pressure-resistant pipe, adding an ionic liquid, and stirring; adding an extracting solution into the reacted material, stirring and extracting, centrifuging, and taking supernate; analyzing the nicotine extraction rate by using a gas chromatographic method; and screening ionic liquid types and reaction conditions: setting the reaction temperature to be 90 DEG C, the time to be 0.5 h and the dosage of the ionic liquid to be 3.5 mmol. With the adoption of the nicotine extraction method, the extraction rate of nicotine can be effectively improved under the condition that an organic solvent is not used, meanwhile, the extraction time can be remarkably shortened, the use of a large amount of solvent is reduced, the ionic liquid can be recycled for multiple times, the method is green and environment-friendly, the production cost can be reduced, and industrial production is facilitated.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of tobacco chemistry, and particularly relates to a method for extracting nicotine in discarded tobacco powder by using ionic liquid as a target. BACKGROUND

[0002] Nicotine, also known as nicotine, is an important medicine and chemical raw material, and is expected to become an effective drug for treating Alzheimer's disease, Parkinson's disease and depression. At the same time, it is also an ideal high-efficiency insecticide in the field of green food, and can be used to prepare biological pesticides, so the demand is huge.

[0003] Nicotine is mainly extracted from tobacco or discarded tobacco stems and leaves. At present, the extraction methods of nicotine include steam distillation, organic solvent extraction, ion exchange resin method, membrane separation technology, microwave extraction method, subcritical fluid extraction method, supercritical fluid extraction method, ultrasonic extraction method, etc. Among them, the solvent extraction method is widely used in industrial production due to its simple operation and low cost.

[0004] The main process of the solvent extraction method is: alkali immersion -> organic solvent extraction -> distillation refining. However, a large amount of organic solvents with high toxicity and easy evaporation such as petroleum ether and industrial hexane are used in the process, which will pollute the environment and harm human health. In addition, the volatilization of organic solvents can also cause safety accidents. The method using organic solvents as extractants also has the problem of solvent residue, which will pollute the final product with organic matter.

[0005] Ionic liquid refers to an organic molten salt composed of organic cations and organic anions or inorganic anions, which is in liquid state below 100 DEG C. It has the advantages of non-volatility, low toxicity, good thermal stability and structural designability. In particular, the structural designability can endow it with flexible properties and different functions. For example, ionic liquids with good solubility can be designed according to the structure of target substances to realize efficient and green extraction of target substances, which has high development and utilization value in the field of extraction and separation. SUMMARY

[0006] The purpose of the present application is to provide a method for extracting nicotine in discarded tobacco powder by using ionic liquid as a target, so as to solve the problems existing in the background art.

[0007] To achieve the above-mentioned purpose, the present application is realized by the following technical scheme:

[0008] A method for extracting nicotine in discarded tobacco powder by using ionic liquid as a target, comprising the following steps:

[0009] S1, placing isoquinoline in a volumetric flask, adding ethyl acetate to constant volume, and preparing an extraction solution containing 0.04% g / ml of isoquinoline internal standard;

[0010] S2, the pulverized and sieved dried tobacco dust is sent into a pressure-resistant tube, and an ionic liquid is added in a mass ratio of 1:13-1:15, and then stirring is performed in an oil bath;

[0011] S3, an extraction liquid is added to the reacted material, and the extraction is fully stirred, and the extracted liquid is absorbed, and centrifuged by a centrifuge to obtain a nicotine supernatant;

[0012] S4, the nicotine supernatant is taken for gas chromatography-mass spectrometry analysis, and a sharp and clear nicotine peak and an internal standard peak are obtained in the figure, and the nicotine extraction rate is calculated;

[0013] S5, different ionic liquids are replaced, and steps S2 to S4 are repeated, and the ionic liquid with the highest nicotine extraction rate and the parameter condition are screened out.

[0014] Further, the ionic liquid is respectively 1-butyl-3-methylimidazolium chloride, 1-ethyl-3-methylimidazolium chloride, 1-butyl-2,3-dimethylimidazolium chloride, 1-hydroxyethyl-3-methylimidazolium chloride, 1-butyl-3-ethylimidazolium chloride, 1-ethyl-3-methylimidazolium iodide, 1-butyl-3-methylimidazolium bromide, 1,3-dibutylimidazolium chloride, 1-butyl-3-methylimidazolium acetate, 1-ethyl-3-methylimidazolium acetate, 1-hydroxyethyl-3-methylimidazolium acetate, 1-butyl-2,3-dimethylimidazolium acetate, 1-butyl-3-methylimidazolium trifluoroacetate, 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3-methylimidazolium tetrafluoroborate and 1-ethyl-3-methylimidazolium tetrafluoroborate.

[0015] The material used in the method can be various substances containing nicotine, including but not limited to tobacco leaves, cured tobacco, tobacco stems, and tobacco processing waste. The ionic liquid in the method can be recycled, which not only avoids waste of solvent, but also improves the extraction rate of nicotine.

[0016] Further, the reaction time is 0-12 h, and preferably 0.5 h.

[0017] Further, the reaction temperature is 40-140 ℃, and preferably 90 ℃.

[0018] Further, the amount of the ionic liquid used is 0-3.5 mmol, and the preferred amount is 3.5 mmol.

[0019] Further, the preferred pulverization mesh number of the tobacco waste is 50-150 mesh.

[0020] The method does not require the use of any organic solvent, and can achieve effective extraction of nicotine contained in tobacco dust. Through detection, the obtained substance is nicotine, and the nicotine extraction rate is as high as 99.99%, effectively avoiding the use of organic solvents and the adverse effects thereof.

[0021] The beneficial effects of the present application are:

[0022] 1) The method for extracting nicotine by using ionic liquid as solvent provided by the present application uses commercially available ionic liquid as solvent, which is cheap and easy to obtain, and is suitable for industrial continuous production.

[0023] 2) The method for extracting nicotine by using ionic liquid as solvent provided by the present application can obtain high yield by using tobacco waste as raw material. The ionic liquid in the method is continuously recycled in the method, and no three wastes are generated, which is environmentally friendly, easy to operate, and suitable for large-scale production and application. DETAILED DESCRIPTION

[0024] The technical solutions of the present application will be described in detail below in combination with the embodiments. The following embodiments are only exemplary and can only be used to explain and illustrate the technical solutions of the present application, but cannot be interpreted as a limitation of the technical solutions of the present application. Any modifications, equivalent replacements and improvements made within the spirit and principles of the present application shall be included in the protection scope of the present application.

[0025] In the following examples, the experimental methods are conventional methods unless otherwise specified. The reagents and materials can be obtained from commercial channels unless otherwise specified.

[0026] Example 1

[0027] The reaction of extracting nicotine by using ionic liquid 1-butyl-3-methylimidazolium chloride ([BMIm][Cl]) as solvent.

[0028] 40 mg of tobacco leaves and 3.5 mmol of ionic liquid 1-butyl-3-methylimidazolium chloride ([BMIm][Cl]) were placed in a pressure tube and sealed, then moved to a 90 ℃ oil bath and stirred and heated for 0.5 h. After the reaction was completed, the mixture was cooled to room temperature, and an extraction liquid was added to the pressure tube, and the mixture was stirred and extracted. After centrifugation, the supernatant was taken and analyzed by gas chromatography-mass spectrometry, and the nicotine extraction rate was 99.99%.

[0029] Example 2

[0030] The reaction of extracting nicotine by using ionic liquid 1-ethyl-3-methylimidazolium chloride ([EMIm][Cl]) as solvent.

[0031] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-ethyl-3-methylimidazolium chloride ([EMIm][Cl]) were placed in a pressure tube and sealed; then the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h under stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 50.72%.

[0032] Example 3

[0033] The reaction of targeted extraction of nicotine with ionic liquid 1-butyl-2,3-dimethylimidazolium chloride ([BMMIm][Cl]) as a solvent.

[0034] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-butyl-2,3-dimethylimidazolium chloride ([BMMIm][Cl]) were placed in a pressure tube and sealed; then the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h under stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 43.00%.

[0035] Example 4

[0036] The reaction of targeted extraction of nicotine with ionic liquid 1-hydroxyethyl-3-methylimidazolium chloride ([HOEtMIm][Cl]) as a solvent.

[0037] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-hydroxyethyl-3-methylimidazolium chloride ([HOEtMIm][Cl]) were placed in a pressure tube and sealed; then the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h under stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 41.00%.

[0038] Example 5

[0039] The reaction of targeted extraction of nicotine with ionic liquid 1-butyl-3-ethylimidazolium chloride ([BEIm][Cl]) as a solvent.

[0040] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-butyl-3-ethylimidazolium chloride ([BEIm][Cl]) were placed in a pressure tube and sealed; then the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h under stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 58.43%.

[0041] Example 6

[0042] The reaction of targeted extraction of nicotine with ionic liquid 1-ethyl-3-methylimidazolium iodide ([EMIm][I]) as a solvent.

[0043] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-ethyl-3-methylimidazolium iodide ([EMIm][I]) were placed in a pressure tube and sealed, and then moved to a 90 ℃ oil bath for stirring and heating for 0.5 h. After the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added, and the extraction was fully stirred. After centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed. The extraction rate of nicotine was 37.16%.

[0044] Example 7

[0045] The reaction of targeted extraction of nicotine with ionic liquid 1-butyl-3-methylimidazolium bromide ([BMIm][Br]) as a solvent.

[0046] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-butyl-3-methylimidazolium bromide ([BMIm][Br]) were placed in a pressure tube and sealed, and then moved to a 90 ℃ oil bath for stirring and heating for 0.5 h. After the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added, and the extraction was fully stirred. After centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed. The extraction rate of nicotine was 51.47%.

[0047] Example 8

[0048] The reaction of targeted extraction of nicotine with ionic liquid 1,3-dibutylimidazolium chloride ([BBIm][Cl]) as a solvent.

[0049] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1,3-dibutylimidazolium chloride ([BBIm][Cl]) were placed in a pressure tube and sealed, and then moved to a 90 ℃ oil bath for stirring and heating for 0.5 h. After the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added, and the extraction was fully stirred. After centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed. The extraction rate of nicotine was 58.44%.

[0050] Example 9

[0051] The reaction of targeted extraction of nicotine with ionic liquid 1-butyl-3-methylimidazolium acetate ([BMIm][OAc]) as a solvent.

[0052] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-ethyl-3-methylimidazole acetate ([EMIm][OAc]) were placed in a pressure tube and sealed; the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h with stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 58%.

[0053] Example 10

[0054] The reaction of targeted extraction of nicotine with ionic liquid 1-ethyl-3-methylimidazole acetate ([EMIm][OAc]) as a solvent.

[0055] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-ethyl-3-methylimidazole acetate ([EMIm][OAc]) were placed in a pressure tube and sealed; the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h with stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 58%.

[0056] Example 11

[0057] The reaction of targeted extraction of nicotine with ionic liquid 1-ethyl-3-methylimidazole acetate ([EMIm][OAc]) as a solvent.

[0058] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-ethyl-3-methylimidazole acetate ([EMIm][OAc]) were placed in a pressure tube and sealed; the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h with stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 58%.

[0059] Example 12

[0060] The reaction of targeted extraction of nicotine with ionic liquid 1-ethyl-3-methylimidazole acetate ([EMIm][OAc]) as a solvent.

[0061] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-ethyl-3-methylimidazole acetate ([EMIm][OAc]) were placed in a pressure tube and sealed; the pressure tube was moved into a 90 ℃ oil bath and heated for 0.5 h with stirring; after the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added into the pressure tube, and the extraction was fully stirred; after centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed, and the extraction rate of nicotine was 58%.

[0062] Example 13

[0063] The reaction of targeted extraction of nicotine with ionic liquid 1-butyl-3-methylimidazolium trifluoroacetate ([BMIm][CF3COO]) as solvent.

[0064] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-butyl-3-methylimidazolium trifluoroacetate ([BMIm][CF3COO]) were placed in a pressure tube and sealed, and then moved to a 90 ℃ oil bath for stirring and heating for 0.5 h. After the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added, and extraction was performed by stirring. After centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed. The extraction rate of nicotine was 55.27%.

[0065] Example 14

[0066] The reaction of targeted extraction of nicotine with ionic liquid 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate ([HOEtMIm][BF4]) as solvent.

[0067] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate ([HOEtMIm][BF4]) were placed in a pressure tube and sealed, and then moved to a 90 ℃ oil bath for stirring and heating for 0.5 h. After the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added, and extraction was performed by stirring. After centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed. The extraction rate of nicotine was 16.52%.

[0068] Example 15

[0069] The reaction of targeted extraction of nicotine with ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF4]) as solvent.

[0070] 40 mg of tobacco leaves, 3.5 mmol of ionic liquid 1-butyl-3-methylimidazolium tetrafluoroborate ([BMIm][BF4]) were placed in a pressure tube and sealed, and then moved to a 90 ℃ oil bath for stirring and heating for 0.5 h. After the reaction was completed, the pressure tube was cooled to room temperature, an extraction liquid was added, and extraction was performed by stirring. After centrifugation, the supernatant was taken, and gas chromatography-mass spectrometry analysis was performed. The extraction rate of nicotine was 21.28%.

[0071] Example 16

[0072] The reaction of targeted extraction of nicotine with ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIm][BF4]) as solvent.

[0073] 40 mg tobacco leaves, 3.5 mmol of ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate ([EMIm][BF4]) were placed in a pressure tube, sealed, and then moved to a 90 ℃ oil bath for stirring and heating for 0.5 h. After the reaction was completed, the mixture was cooled to room temperature, and an extraction liquid was added to the pressure tube. The mixture was stirred and extracted, and then centrifuged to obtain the supernatant. Gas chromatography-mass spectrometry analysis showed that the extraction rate of nicotine was 17.29%.

[0074] Example 17

[0075] Cyclic test experiment of targeted extraction of nicotine using ionic liquid as a solvent.

[0076] The experimental conditions and steps were the same as in Example 1, except that the ionic liquid was replaced with the ionic liquid recovered in the example, and five repeated use experiments were performed. The extraction rates of nicotine were 100%, 100%, 99.85%, 95.49%, and 93.51%, respectively. The ionic liquid recovery process was as follows: drying in a vacuum drying box at 60 ℃ for 24 h.

[0077] Finally, it should be noted that the above examples are only used to illustrate the technical solutions of the present application and not to limit them. Although the present application has been described in detail with reference to the preferred embodiments, those skilled in the art should understand that the technical solutions of the present application can still be modified or replaced by equivalents, and these modifications or replacements should not make the modified technical solutions deviate from the spirit and scope of the technical solutions of the present application.

Claims

1. A method for targeted extraction of nicotine from waste tobacco using ionic liquids, characterized in that, Includes the following steps: S1. Place isoquinoline in a volumetric flask, add ethyl acetate to make up to volume, and prepare an extract containing 0.04% g / ml of isoquinoline internal standard; S2. The pulverized, sieved and dried tobacco powder is fed into a pressure-resistant tube, and ionic liquid is added at a mass ratio of 1:13 to 1:

15. The mixture is then stirred in an oil bath. S3. Add the extract to the reacted material, stir thoroughly to extract, collect the extracted liquid, centrifuge it to obtain the nicotine-containing supernatant. S4. Take the nicotine supernatant for gas chromatography-mass spectrometry analysis. The figure shows sharp and distinct nicotine peaks and internal standard peaks. Calculate the nicotine extraction rate. S5. Change to different ionic liquids and repeat steps S2 to S4 to screen out the ionic liquid and parameter conditions with the highest nicotine extraction rate.

2. The method for targeted extraction of nicotine from waste tobacco using ionic liquids according to claim 1, characterized in that, The ionic liquids are 1-butyl-3-methylimidazolium chloride, 1-ethyl-3-methylimidazolium chloride, 1-butyl-2,3-dimethylimidazolium chloride, 1-hydroxyethyl-3-methylimidazolium chloride, 1-butyl-3-ethylimidazolium chloride, 1-ethyl-3-methylimidazolium iodide, 1-butyl-3-methylimidazolium bromide, 1,3-dibutylimidazolium chloride, 1-butyl-3-methylimidazolium acetate, 1-ethyl-3-methylimidazolium acetate, 1-hydroxyethyl-3-methylimidazolium acetate, 1-butyl-2,3-dimethylimidazolium acetate, 1-butyl-3-methylimidazolium trifluoroacetate, 1-hydroxyethyl-3-methylimidazolium tetrafluoroborate, 1-butyl-3-methylimidazolium tetrafluoroborate, and 1-ethyl-3-methylimidazolium tetrafluoroborate.

3. The method for targeted extraction of nicotine from waste tobacco using ionic liquids according to claim 1, characterized in that, The ionic liquid is recycled.

4. The method for targeted extraction of nicotine from waste tobacco using ionic liquids according to claim 1, characterized in that, The tobacco dust refers to various nicotine-containing substances, including but not limited to tobacco leaves, flue-cured tobacco, tobacco stems, and tobacco processing waste.

5. The method for targeted extraction of nicotine from waste tobacco using ionic liquids according to claim 4, characterized in that, The mesh size of the tobacco dust is 50-150 mesh.

6. The method for targeted extraction of nicotine from waste tobacco using ionic liquids according to claim 1, characterized in that, The reaction time is 0.1-12h, preferably 0.5h.

7. The method for targeted extraction of nicotine from waste tobacco using ionic liquids according to claim 1, characterized in that, The reaction temperature is 40-140℃, preferably 90℃.

8. The method for targeted extraction of nicotine from waste tobacco using ionic liquids according to claim 1, characterized in that, The amount of ionic liquid used is 0.5~3.5 mmol, with 3.5 mmol being the preferred amount.