CN112569311A - Fresh bamboo juice, preparation method and quality detection method thereof - Google Patents

Fresh bamboo juice, preparation method and quality detection method thereof Download PDF

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CN112569311A
CN112569311A CN202011501134.3A CN202011501134A CN112569311A CN 112569311 A CN112569311 A CN 112569311A CN 202011501134 A CN202011501134 A CN 202011501134A CN 112569311 A CN112569311 A CN 112569311A
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bamboo
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bamboo juice
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宋细忠
钱丽梅
习梅兰
于喆
尹炜
周志红
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Xinyu Fangzhu Biotechnology Co ltd
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Abstract

The invention provides fresh bamboo juice and a preparation method and a quality detection method thereof, relating to the technical field of separation and extraction; the preparation method comprises the following steps: pretreating bamboo chips by using the dicationic acidic ionic liquid solution, heating and dry distilling the pretreated bamboo chips to obtain dry distillation liquid, and condensing and collecting the dry distillation liquid to obtain fresh bamboo juice. The quality detection method comprises the following steps: the method comprises the following steps of character detection, thin-layer chromatography identification, pH value measurement, relative density measurement, total solid content measurement, amino acid content measurement and total fructose, glucose and sucrose content measurement. The bamboo utilization rate is high, the yield of the obtained fresh bamboo juice is high, and is improved by 30 to 50 percent compared with the prior art; the fresh bamboo juice has high content of guaiacol, high content of amino acid and good quality. The preparation method has the advantages of short time consumption, simple procedure, less equipment investment and low production cost, and can be applied to industrial production. The quality detection method of the invention is convenient and fast, and has high accuracy, sensitivity and repeatability.

Description

Fresh bamboo juice, preparation method and quality detection method thereof
Technical Field
The invention relates to the technical field of separation and extraction, and particularly relates to fresh bamboo juice, a preparation method and a quality detection method thereof.
Background
The fresh succus Bambusae is liquid extracted from fresh bamboo, such as water and nutrient vegetable oil, and has effects of clearing heat, eliminating phlegm, and relieving cough. The existing preparation and extraction methods of fresh bamboo juice mainly comprise a traditional fire baking method and a traditional water boiling method. The equipment used for extracting the fresh bamboo juice by the water boiling method is generally a multifunctional extraction tank, and industrial production can be formed. However, the fresh bamboo juice produced by the boiling method has low content of effective components, is easy to go moldy and go bad, the product quality can not meet the requirement of baking and dry distillation, and the process method is completely inconsistent with the traditional fresh bamboo juice processing process requirement. The traditional fire roasting method accords with the traditional processing method of fresh bamboo juice in process, but the method has serious waste of bamboo materials, low yield, low efficiency, environmental pollution and the like, and is difficult to realize high-efficiency industrial production. The dry distillation method can solve the above problems to some extent.
For example, patent No. 201611166001.9 discloses a process for preparing fresh succus Bambusae, which comprises heating bamboo as raw material, reacting in retort, collecting the resultant at low and high temperatures, washing with purified water, and mixing the liquid. The bamboo charcoal obtained after the bamboo is reacted in the retort can also be used for burning and secondary utilization, so that the bamboo is fully utilized. But the treatment process steps are more complicated, the yield of the fresh bamboo juice is lower, and the content of the guaiacol is also lower.
Ionic Liquids (ILs) are salts which are composed of positive ions and negative ions and are liquid at room temperature or use temperature, and are green solvents which have strong dissolving capacity, are non-volatile, have high thermal stability and can be designed. The ionic liquid has excellent performances in extraction and separation of food components, analysis and detection, physical property modification and the like. Research shows that the anions and cations in the ionic liquid contain different functional groups such as hydroxyl and the like to form hydrogen bonds, destroy the crystalline structure of the microcrystalline dietary fiber and enhance the solubility of the dietary fiber. Therefore, the ionic liquid has great potential for preparing fresh bamboo juice.
Disclosure of Invention
The invention aims to solve the problems, provides fresh bamboo juice with simple treatment process, high product yield and good quality and a preparation method thereof, and also provides a convenient, quick and high-accuracy fresh bamboo juice quality detection method.
In a first aspect of the object of the present invention, there is provided a method for preparing fresh bamboo juice, comprising the steps of:
s1, preprocessing: sawing off and splitting fresh bamboos to obtain bamboo chips, treating the bamboo chips for a period of time by using dicationic acidic ionic liquid solution, and then removing the dicationic acidic ionic liquid solution to obtain pretreated bamboo chips;
s2, dry distillation and extraction: placing the pretreated bamboo chips into a dry distillation device, wherein the dry distillation device comprises a heating device and a stirring device; starting the heating device to directly heat and dry-distill the pretreated bamboo chips, starting the stirring device to uniformly distribute heat generated by the heating device in the furnace body, and simultaneously enabling free water and water vapor in the bamboo materials to outwards migrate in a form of seepage flow; discharging the obtained dry distillation liquid from a discharge port of the dry distillation device;
s3, condensing and collecting: and condensing the discharged dry distillation liquid through a condenser to obtain fresh bamboo juice.
Preferably, the dicationic acidic ionic liquid solution in step S1 specifically includes: 0.1-20 parts of dicationic acidic ionic liquid and 80-150 parts of water.
Preferably, the preparation method of the dicationic acidic ionic liquid in step S1 is:
a. adding 1, 4-propane sultone into an ethanol solution of tetramethylethylenediamine under the condition of stirring, reacting for a period of time at 60-100 ℃, and separating the obtained solid intermediate product;
b. and (4) adding an acid solution into the solid intermediate product obtained in the step S1, stirring and reacting for a period of time at the temperature of 60-100 ℃, and removing the solvent and residual reactants in the reaction mixture to obtain the dicationic acidic ionic liquid.
Preferably, the processing conditions in step S1 are: the temperature is 10-40 ℃, and the soaking time is 1-6 h.
Preferably, the treatment in step S1 is ultrasonic treatment, and the ultrasonic treatment conditions are: the ultrasonic frequency is 5-15 kHz, the ultrasonic temperature is 10-40 ℃, and the ultrasonic time is 10-60 min.
Preferably, in step S2, a guide rail is arranged inside the retort device, and the guide rail is used for placing a bamboo strip cart matched with the guide rail; the pretreated bamboo chips are placed on the bamboo chip vehicle and are sent to a guide rail in the dry distillation device, and heating and dry distillation are carried out in the bamboo chip vehicle.
Preferably, the heating and dry distillation temperature in step S2 is 150-200 ℃.
Preferably, the filling amount of the pretreated bamboo chips is 30-80% of the volume of the dry distillation device.
In a second aspect of the object of the present invention, there is provided a fresh bamboo juice prepared by any one of the above-mentioned methods for preparing fresh bamboo juice.
In a third aspect of the present invention, there is provided a method for detecting quality of fresh bamboo juice, comprising: detecting characters, identifying by thin-layer chromatography, measuring pH value, measuring relative density, measuring total solid content, measuring amino acid content and measuring total content of fructose, glucose and sucrose; the content determination of the amino acid and the total content determination of the fructose, the glucose and the sucrose adopt a high performance liquid chromatography.
Preferably, the pH value is 4.4-5.5, the relative density is not lower than 1.010, the total solid content is not lower than 2.0%, the content of amino acid is not lower than 62 mu g/mL, and the total content of fructose, glucose and sucrose is not higher than 27.8 mg/mL.
Preferably, the thin layer chromatography identification comprises:
1) taking 20ml of fresh bamboo juice, adjusting the pH value to 1-2 by using dilute hydrochloric acid, shaking and extracting for 2 times by using diethyl ether, wherein 20ml of diethyl ether is used for each time, combining diethyl ether liquid, washing the diethyl ether liquid by using 20ml of 5% sodium bicarbonate solution, separating and drying a diethyl ether layer, and adding methanol lml into residues to dissolve the residues to obtain a sample solution; adding methanol into 2, 6-dimethoxyphenol reference substance to obtain 1 mg/lml solution as reference substance solution; pipette 5. mu.l of each of the two solutions, spot on the same silica gel G thin layer plate, and mix with toluene: ethyl acetate: formic acid is used as a developing agent, developed, taken out, dried and sprayed with 5 wt% ferric trichloride ethanol solution; judging whether spots with the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution;
2) extracting fresh succus Bambusae 10ml with water saturated n-butanol under shaking for 3 times (15 ml each time), mixing n-butanol solutions, evaporating to dryness, and dissolving the residue with methanol 1ml to obtain sample solution; adding methanol into (+) -lyoniresinol-3 alpha-O-beta-D-glucopyranoside reference substance to obtain a solution containing 1mg per 1ml, and using the solution as a reference substance solution; pipetting 5 mul of each of the two solutions, dropping the solution on the same silica gel G thin layer plate, adding chloroform: methanol: formic acid is used as a developing agent, the mixture is developed, taken out, dried in the air, sprayed with 10 wt% phosphomolybdic acid ethanol solution, and heated at 105 ℃ until the spots are clearly developed; and judging whether spots with the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution.
Preferably, the amino acid content determination comprises:
1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filling agent; taking acetonitrile-0.1 mol/L sodium acetate solution which is used for adjusting the pH value to 6.5 by using acetic acid as a mobile phase A, and taking acetonitrile-water as a mobile phase B for gradient elution; the flow rate was 1.0ml per minute; the column temperature was 40 ℃; the detection wavelength is 254nm, and the number of theoretical plates is not lower than 4000 calculated according to an alanine peak;
2) preparation of control solutions: taking a proper amount of a serine reference substance, a glycine reference substance, an arginine reference substance, a threonine reference substance, an alanine reference substance and a proline reference substance, precisely weighing, adding 0.1mol/L hydrochloric acid solution to prepare a mixed solution containing 120 mu g of serine, 12 mu g of glycine, 150 mu g of arginine, 30 mu g of threonine, 80 mu g of alanine and 50 mu g of proline in each 1ml, precisely weighing 1ml of the mixed reference solution, adding 0.5ml of an acetonitrile solution of 1mol/L triethylamine and 0.5ml of an acetonitrile solution of 0.1mol/L phenyl isothiocyanate, shaking uniformly, placing for 1 hour in a dark place, adding 2ml of n-hexane, shaking, placing for 10 minutes, centrifuging a lower layer solution, filtering, and taking a subsequent filtrate to obtain the product;
3) preparation of a test solution: precisely measuring 1ml of fresh bamboo juice, adding 0.5ml of acetonitrile solution of 1mol/L triethylamine and 0.5ml of acetonitrile solution of 0.1mol/L phenyl isothiocyanate, shaking up, standing for 1 hour in the dark, adding 2ml of n-hexane, shaking up, standing for 10 minutes, centrifuging to obtain a lower layer solution, filtering, and taking a subsequent filtrate to obtain the extract;
4) the determination method comprises the following steps: precisely sucking 2 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
Preferably, the total fructose, glucose and sucrose content determination comprises:
1) chromatographic conditions and system applicability test: the column length is 25cm, the inner diameter is 4.6mm, and the particle size of the filler is 3 μm; acetonitrile-water is used as a mobile phase; detection by an evaporative light scattering detector. The theoretical pole number is not lower than 4000 calculated according to the fructose peak;
2) preparation of control solutions: taking appropriate amount of D-fructose, D-anhydrous glucose and sucrose as reference substances, and adding water to obtain solution containing 0.2mg per lml;
3) preparation of a test solution: precisely measuring fresh succus Bambusae 2ml, placing in 50ml measuring flask, adding water to dilute to scale, shaking, filtering, and collecting filtrate;
4) the determination method comprises the following steps: precisely absorbing 5 and 20 mul of reference solution and 5-10 mul of test solution, respectively, injecting into a liquid chromatograph, measuring, and calculating by an external standard two-point method logarithmic equation to obtain the final product.
The invention can obtain the following beneficial effects:
1. the bamboo chips treated by the ionic liquid can accelerate the dissolution and extraction of the effective components in the bamboo chips and improve the bioavailability of the bamboo chips. The ionic liquid used in the invention has good biocompatibility and good catalytic activity, can improve the internal environment of the bamboo chips, assist and promote the destruction of cell wall structures of biomass, promote the decrystallization of bamboo chip fibers and is beneficial to the dissolution of effective components; in addition, the invention uses the acidic ionic liquid, the aqueous solution of which has certain acidity, synergistically promotes the decrystallization of the bamboo chip fiber, and accelerates the dissolution of the effective components.
2. The bamboo utilization rate is high, the yield of the obtained fresh bamboo juice is high, and is improved by 30 to 50 percent compared with the prior art; the fresh bamboo juice has high content of guaiacol, high content of amino acid and good quality.
3. The preparation method has the advantages of short time consumption, simple procedure, less equipment investment and low production cost, and can be applied to industrial production.
4. The quality detection method of the invention is convenient and fast, and has high accuracy, sensitivity and repeatability.
Drawings
FIG. 1 is a flow chart of a method for preparing fresh bamboo juice according to the present invention;
FIG. 2 is a schematic view showing the construction of a retort and a condenser according to the present invention;
fig. 3 is a schematic structural view of the bamboo chip cart of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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 chemical reagents and laboratory equipment used in the preferred embodiment of the invention are commercially available.
The preparation process of dicationic acidic ionic liquid is shown in figure 2, and ionic liquid [ Bs ] is used2TMEDA][CF3SO3]2Is an example.
Adding tetramethylethylenediamine and ethanol into a reactor respectively, and preheating at 70 ℃; dropwise adding 1, 4-butane sultone under the stirring condition, and continuously stirring for 8 hours after dropwise adding is finished to obtain a large amount of intermediate products. After the reaction is finished, the intermediate product is repeatedly washed by ether for 3-5 times to remove unreacted raw materials, and then the intermediate product is dried in a vacuum drying oven at 80 ℃ for 12 hours.
The intermediate product was added to the reactor, preheated at 70 ℃, and then the triflic acid solution was added dropwise to the reactor, with continued stirring for 10 h. Finally, the product obtained is washed 3-5 times with acetone to remove possible unreacted intermediate products, and dried in vacuum at 80 ℃ for 10h to obtain [ Bs ]2TMEDA][CF3SO3]2The yield was about 92%.
According to the method, the intermediate product reacts with sulfuric acid solution, phosphoric acid solution, hydrochloric acid solution, nitric acid solution, trifluoromethanesulfonic acid solution or hexafluorophosphoric acid solution respectively for 10h at 75 ℃ to prepare ionic liquid [ Bs%2TMEDA][HSO4]2、[Bs2TMEDA][H2PO4]2、[Bs2TMEDA]Cl2、[Bs2TMEDA][NO3]2The yields of the four ionic liquids were 92%, 90%, 92%, respectively.
As shown in fig. 2 to 3, the dry distillation device 1 used in the preparation method of the present invention includes a heating device 12 and a stirring device 13, the heating device 12 is disposed on the outer surface of the dry distillation device 1 and is used for heating the dry distillation device 1, the stirring device 13 is used for uniformly distributing the heat generated by the heating device 12 in the dry distillation device 1, and simultaneously, free water and water vapor in bamboo wood are both transferred outwards in the form of a seepage flow, so that the dry distillation quality is high; the stirring device 13 is mechanically sealed with the retort 1. One end of the dry distillation device 1 is provided with a feeding door 14, a plurality of discharging ports 16 for discharging fresh bamboo juice are arranged below the dry distillation device 1, a bottom plate 17 is arranged inside the dry distillation device 1, and a guide rail 18 is arranged on the bottom plate 17; the bottom plate 17 is used for installing a guide rail 18, the guide rail 18 is used for placing a bamboo chip cart 11 matched with the guide rail 18, and the bamboo chip cart 11 is used for containing bamboo chips to be subjected to dry distillation; the discharge port 16 is connected with the condenser 2 through the first pipeline 4, and the bottom of the condenser 2 is provided with a cooling water inlet 21 and the top is provided with a cooling water outlet 22.
The stirring device 13 includes a motor 131 and a fan 132, and a power input end of the fan 132 is electrically connected to a power output end of the motor 131. The stirring device 13 has a simple structure and high working efficiency.
The motor 131 is a reduction motor.
Wherein, a temperature detector 15 is arranged above the dry distillation device 1, so that the temperature in the dry distillation furnace can be monitored in real time, and the temperature can be controlled conveniently according to the actual production condition.
Wherein, the bamboo chip cart 11 is provided with holes 111 for the fresh bamboo juice to flow down, so that the fresh bamboo juice can be collected more conveniently and rapidly.
Wherein, the dry distillation device 1 is internally provided with a safety interlocking device 19, and the safety interlocking device 19 is connected with the feeding door 14, the heating device 12 and the stirring device 13. Once an accident happens, such as the feeding door is opened during the heating and dry distillation, the heating and stirring are automatically stopped; or when the feeding door is not closed, the heating device and the stirring device are not started. By arranging the safety interlocking device, the dangerous situation is prevented from happening.
Wherein, the outer surface of the dry distillation device 1 is also provided with a heat preservation layer. The heat loss can be effectively reduced by the heat insulation layer, and energy conservation is realized.
Wherein, the drain hole 16 is equipped with 1 ~ 5, preferably 3, does benefit to the blowing operation.
Wherein, the electric heater of the heating device 12 is provided with an electric heating interface 121 on the heating device 12. The electric heating mode is safer and more reliable, and the heating power can be controlled, so that the temperature can be controlled conveniently according to the actual production condition.
Wherein, the condenser 2 is a tubular condenser or a plate condenser, and has high cooling efficiency and good effect.
The dicationic acidic ionic liquid prepared by the above method was used in the following examples.
The dry distillation apparatus 1 and the condenser 2 described above were used in the following examples.
Example 1:
as shown in fig. 1, a method for preparing fresh bamboo juice comprises the following steps:
s1, preprocessing: cutting fresh bamboo, splitting to obtain bamboo pieces, and treating with dicationic acidic ionic liquid solution ([ Bs)2TMEDA][NO3]20.5 part of ionic liquid and 100 parts of water) is soaked in the bamboo chips at the temperature of 25 ℃ for 3 hours, then the bamboo chips are fished out and washed by water to remove possible residual dicationic acidic ionic liquid solution, thus obtaining pretreated bamboo chips;
s2, dry distillation and extraction: placing pretreated bamboo chips on a bamboo chip trolley 11 and feeding the pretreated bamboo chips onto a guide rail 18 in a dry distillation device 1, wherein the filling amount of the pretreated bamboo chips is 50% of the volume of the dry distillation device 1, pushing the bamboo chip trolley 11 to a proper position, starting a heating device 12 to directly heat and dry distill the pretreated bamboo chips on the bamboo chip trolley 11, starting a stirring device 13 to uniformly distribute heat generated by the heating device 12 in a furnace body 11, simultaneously enabling free water and water vapor in the bamboo chips to outwards migrate in a form of osmotic flow, and controlling the temperature of heating and dry distill to be 170 ℃; discharging the obtained dry distillation liquid from a discharge port 16 of the dry distillation device 1;
s3, condensing and collecting: and condensing the discharged dry distillation liquid through a condenser 2 to obtain fresh bamboo juice.
The yield of fresh bamboo juice in this example was 46.6%.
Example 2:
as shown in fig. 1, a method for preparing fresh bamboo juice comprises the following steps:
s1, preprocessing: cutting fresh bamboo, splitting to obtain bamboo pieces, and treating with dicationic acidic ionic liquid solution ([ Bs)2TMEDA][H2PO4]22 parts of ionic liquid and 100 parts of water) for carrying out ultrasonic treatment on the bamboo chips for a period of time, wherein the ultrasonic frequency is 5kHz, the ultrasonic temperature is 25 ℃, and the ultrasonic time is 40 min; then fishing out the bamboo chips, and washing the bamboo chips with waterRemoving possible residual dication type acidic ionic liquid solution to obtain pretreated bamboo chips;
s2, dry distillation and extraction: placing pretreated bamboo chips on a bamboo chip trolley 11 and feeding the pretreated bamboo chips onto a guide rail 18 in a dry distillation device 1, wherein the filling amount of the pretreated bamboo chips is 50% of the volume of the dry distillation device 1, pushing the bamboo chip trolley 11 to a proper position, starting a heating device 12 to directly heat and dry distill the pretreated bamboo chips on the bamboo chip trolley 11, starting a stirring device 13 to uniformly distribute heat generated by the heating device 12 in a furnace body 11, simultaneously enabling free water and water vapor in the bamboo chips to outwards migrate in a form of osmotic flow, and controlling the temperature of heating and dry distill to be 170 ℃; discharging the obtained dry distillation liquid from a discharge port 16 of the dry distillation device 1;
s3, condensing and collecting: and condensing the discharged dry distillation liquid through a condenser 2 to obtain fresh bamboo juice.
The yield of fresh bamboo juice in this example was 49.5%.
Example 3:
as shown in fig. 1, a method for preparing fresh bamboo juice comprises the following steps:
s1, preprocessing: cutting fresh bamboo, splitting to obtain bamboo pieces, and treating with dicationic acidic ionic liquid solution ([ Bs)2TMEDA][CF3SO3]25 parts of ionic liquid and 100 parts of water) for carrying out ultrasonic treatment on the bamboo chips for a period of time, wherein the ultrasonic frequency is 10kHz, the ultrasonic temperature is 25 ℃, and the ultrasonic time is 30 min; then fishing out the bamboo chips, and washing the bamboo chips with water to remove possible residual dication type acidic ionic liquid solution to obtain pretreated bamboo chips;
s2, dry distillation and extraction: placing pretreated bamboo chips on a bamboo chip trolley 11 and feeding the pretreated bamboo chips onto a guide rail 18 in a dry distillation device 1, wherein the filling amount of the pretreated bamboo chips is 50% of the volume of the dry distillation device 1, pushing the bamboo chip trolley 11 to a proper position, starting a heating device 12 to directly heat and dry distill the pretreated bamboo chips on the bamboo chip trolley 11, starting a stirring device 13 to uniformly distribute heat generated by the heating device 12 in a furnace body 11, simultaneously enabling free water and water vapor in the bamboo chips to outwards migrate in a form of osmotic flow, and controlling the temperature of heating and dry distill to be 180 ℃; discharging the obtained dry distillation liquid from a discharge port 16 of the dry distillation device 1;
s3, condensing and collecting: and condensing the discharged dry distillation liquid through a condenser 2 to obtain fresh bamboo juice.
The yield of fresh bamboo juice in this example was 53.5%.
Example 4:
as shown in fig. 1, a method for preparing fresh bamboo juice comprises the following steps:
s1, preprocessing: cutting fresh bamboo, splitting to obtain bamboo pieces, and treating with dicationic acidic ionic liquid solution ([ Bs)2TMEDA][HSO4]28 parts of ionic liquid and 100 parts of water) for carrying out ultrasonic treatment on the bamboo chips for a period of time, wherein the ultrasonic frequency is 15kHz, the ultrasonic temperature is 30 ℃, and the ultrasonic time is 15 min; then fishing out the bamboo chips, and washing the bamboo chips with water to remove possible residual dication type acidic ionic liquid solution to obtain pretreated bamboo chips;
s2, dry distillation and extraction: placing pretreated bamboo chips on a bamboo chip trolley 11 and feeding the pretreated bamboo chips onto a guide rail 18 in a dry distillation device 1, wherein the filling amount of the pretreated bamboo chips is 50% of the volume of the dry distillation device 1, pushing the bamboo chip trolley 11 to a proper position, starting a heating device 12 to directly heat and dry distill the pretreated bamboo chips on the bamboo chip trolley 11, starting a stirring device 13 to uniformly distribute heat generated by the heating device 12 in a furnace body 11, simultaneously enabling free water and water vapor in the bamboo chips to outwards migrate in a form of osmotic flow, and controlling the temperature of heating and dry distill to be 180 ℃; discharging the obtained dry distillation liquid from a discharge port 16 of the dry distillation device 1;
s3, condensing and collecting: and condensing the discharged dry distillation liquid through a condenser 2 to obtain fresh bamboo juice.
The yield of fresh bamboo juice in this example was 51.3%.
Example 5:
as shown in fig. 1, a method for preparing fresh bamboo juice comprises the following steps:
s1, preprocessing: cutting fresh bamboo, splitting to obtain bamboo pieces, and treating with dicationic acidic ionic liquid solution ([ Bs)2TMEDA]Cl 215 parts of ionic liquid and 100 parts of water) is soaked in the bamboo chips for 2 hours at the temperature of 25 ℃, then the bamboo chips are fished out and are added with waterWashing the bamboo chips to remove possible residual dication type acidic ionic liquid solution to obtain pretreated bamboo chips;
s2, dry distillation and extraction: placing pretreated bamboo chips on a bamboo chip trolley 11 and feeding the pretreated bamboo chips onto a guide rail 18 in a dry distillation device 1, wherein the filling amount of the pretreated bamboo chips is 50% of the volume of the dry distillation device 1, pushing the bamboo chip trolley 11 to a proper position, starting a heating device 12 to directly heat and dry distill the pretreated bamboo chips on the bamboo chip trolley 11, starting a stirring device 13 to uniformly distribute heat generated by the heating device 12 in a furnace body 11, simultaneously enabling free water and water vapor in the bamboo chips to outwards migrate in a form of osmotic flow, and controlling the temperature of heating and dry distill to be 180 ℃; discharging the obtained dry distillation liquid from a discharge port 16 of the dry distillation device 1;
s3, condensing and collecting: and condensing the discharged dry distillation liquid through a condenser 2 to obtain fresh bamboo juice.
The yield of fresh bamboo juice in this example was 47.8%.
Example 6:
the quality detection of the fresh bamboo juice obtained in the embodiment 1-5 is respectively carried out, and comprises the following steps: the method comprises the following steps of character detection, thin-layer chromatography identification, pH value measurement, relative density measurement, total solid content measurement, amino acid content measurement and total fructose, glucose and sucrose content measurement. Wherein, the content determination of amino acid and the total content determination of fructose, glucose and sucrose adopt high performance liquid chromatography.
Character detection
The fresh bamboo juice obtained in the examples 1-5 is light yellow to reddish brown liquid; has bamboo fragrance and slightly sweet taste.
Secondly, the thin-layer chromatography identification comprises the following steps:
1) taking 20ml of fresh bamboo juice, adjusting the pH value to 1-2 by using dilute hydrochloric acid, shaking and extracting for 2 times by using diethyl ether, wherein 20ml of diethyl ether is used for each time, combining diethyl ether liquid, washing the diethyl ether liquid by using 20ml of 5% sodium bicarbonate solution, separating and drying a diethyl ether layer, and adding methanol lml into residues to dissolve the residues to obtain a sample solution; methanol was added to a 2,6 dimethoxyphenol control to prepare a 1mg per lml solution as a control solution.
The two solutions were pipetted at 5. mu.l each, and spotted on the same silica gel G thin layer plate, and tested by thin layer chromatography (0502, fourth general rule of pharmacopoeia 2015 edition): ethyl acetate: formic acid 7: 1: 0.1 is developing agent, taking out, airing and spraying 5 wt% ferric trichloride ethanol solution; in the test sample chromatograms of examples 1 to 5, spots of the same color were observed at the positions corresponding to the control chromatogram.
2) Extracting fresh succus Bambusae 10ml with water saturated n-butanol under shaking for 3 times (15 ml each time), mixing n-butanol solutions, evaporating to dryness, and dissolving the residue with methanol 1ml to obtain sample solution; additionally, a (+) -lyoniresinol-3 alpha-O-beta-D-glucopyranoside reference substance is taken and added with methanol to prepare a solution containing 1mg per 1ml as a reference substance solution.
The two solutions were pipetted at 5. mu.l each, and spotted on the same silica gel G thin layer plate by thin layer chromatography (0502 of the four Proc. of the Chinese pharmacopoeia 2015 edition) using chloroform: methanol: formic acid mass ratio 4: 1: 0.1 is a developing agent, is developed, is taken out, is dried in the air, is sprayed with 10 wt% phosphomolybdic acid ethanol solution, and is heated at 105 ℃ until the spots are clearly developed; in the test sample chromatograms of examples 1 to 5, spots of the same color were observed at the positions corresponding to the control chromatogram.
The thin-layer chromatography identification result shows that the fresh bamboo juice obtained in the examples 1-5 contains guaiacol, and the guaiacol content is found to be high by observing the area size and the color depth of the obtained spots.
Third, pH value determination
The pH values of the fresh bamboo juice obtained in examples 1 to 5 were all 4.4 to 5.5 (0631 in the four general rules of the Chinese pharmacopoeia 2015 edition) measured by using a commercially available pH meter.
IV, determination of relative Density
Refer to the four general rules 0601 of the pharmacopoeia 2015 year edition. The relative density of the fresh bamboo juice obtained in examples 1-5 is not less than 1.010.
Fifthly, total solid content determination
Precisely measuring 25ml of fresh succus Bambusae, placing in an evaporation dish with constant weight, completely evaporating in water bath, and drying at 105 deg.C for 5 hr. The fresh bamboo juice obtained in examples 1 to 5 had a total solid content of not less than 2.0%.
Sixthly, the amino acid content determination comprises the following steps:
1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica is used as a filler, the column length is 25cm, the inner diameter is 4.6mm, and the particle size is 5 micrometers; using acetonitrile-0.1 mol/L sodium acetate solution with pH value adjusted to 6.5 by acetic acid in a mass ratio of 7:93 as a mobile phase A, and acetonitrile-water in a mass ratio of 4:1 as a mobile phase B, and carrying out gradient elution according to the specification in table 1; the flow rate was 1.0ml per minute; the column temperature was 40 ℃; the detection wavelength is 254nm, and the number of theoretical plates should not be lower than 4000 calculated according to alanine peak.
TABLE 1
Time (minutes) Mobile phase A (%) Mobile phase B (%)
0～18 100→99 0→1
18～25 99→94 1→6
25～32 94→80 6→20
32～52 80→70 20→30
52～52.2 70→0 30→100
52.2～62 0 100
62.0～62.2 0→100 100→0
62.2～70 100 0
2) Preparation of control solutions: taking a proper amount of a serine reference substance, a glycine reference substance, an arginine reference substance, a threonine reference substance, an alanine reference substance and a proline reference substance, precisely weighing, adding 0.1mol/L hydrochloric acid solution to prepare a mixed solution containing 120 mu g of serine, 12 mu g of glycine, 150 mu g of arginine, 30 mu g of threonine, 80 mu g of alanine and 50 mu g of proline in each 1ml, precisely weighing 1ml of the mixed reference solution, adding 0.5ml of an acetonitrile solution of 1mol/L triethylamine and 0.5ml of an acetonitrile solution of 0.1mol/L phenyl isothiocyanate, shaking uniformly, placing for 1 hour in a dark place, adding 2ml of n-hexane, shaking, placing for 10 minutes, centrifuging for 5 minutes, taking a lower layer solution, filtering, and taking a subsequent filtrate to obtain the product.
3) Preparation of a test solution: precisely measuring 1ml of fresh bamboo juice, adding 0.5ml of acetonitrile solution of 1mol/L triethylamine and 0.5ml of acetonitrile solution of 0.1mol/L phenyl isothiocyanate, shaking uniformly, standing for 1 hour in the dark, adding 2ml of n-hexane, shaking, standing for 10 minutes, centrifuging for 5 minutes, taking the lower layer solution, filtering, and taking the subsequent filtrate to obtain the bamboo juice.
4) The determination method comprises the following steps: precisely sucking 2 μ l of each of the reference solution and the sample solution, injecting into liquid chromatograph, and measuring.
Seventhly, the total content determination of fructose, glucose and sucrose comprises the following steps:
1) chromatographic conditions and system applicability test: to be provided with
Figure BDA0002843634270000132
Omega SUGAR
Figure BDA0002843634270000133
A chromatographic column with a column length of 25cm, an inner diameter of 4.6mm and a filler particle size of 3 μm; according to the mass ratio of acetonitrile to water of 85: 15 is a mobile phase; detection by an evaporative light scattering detector. The theoretical pole number is not lower than 4000 calculated according to the fructose peak;
2) preparation of control solutions: taking appropriate amount of D-fructose, D-anhydrous glucose and sucrose as reference substances, and adding water to obtain solution containing 0.2mg per lml;
3) preparation of a test solution: precisely measuring fresh succus Bambusae 2ml, placing in 50ml measuring flask, adding water to dilute to scale, shaking, filtering, and collecting filtrate;
4) the determination method comprises the following steps: precisely absorbing 5 and 20 mul of reference solution and 5-10 mul of test solution, respectively, injecting into a liquid chromatograph, measuring, and calculating by an external standard two-point method logarithmic equation to obtain the final product.
The results of some quality indexes of the fresh bamboo juice prepared in examples 1 to 5 are shown in table 2.
TABLE 2
Figure BDA0002843634270000131
Figure BDA0002843634270000141
The quality test results in table 2 show that: the fresh bamboo juice product provided by the embodiment of the invention has a pH value of 4.4-5.5, a relative density of not less than 1.010, a total solid content of not less than 2.0%, an amino acid content of not less than 62 mu g/mL, and a total content of fructose, glucose and sucrose of not more than 27.8 mg/mL. Among them, the quality test results of example 3 are the best, and the best example shows that the promotion effect on the extraction of the fresh bamboo juice is the best under the condition.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (10)

1. A method for preparing fresh bamboo juice is characterized by comprising the following steps:
s1, preprocessing: sawing off and splitting fresh bamboos to obtain bamboo chips, treating the bamboo chips for a period of time by using dicationic acidic ionic liquid solution, and then removing the dicationic acidic ionic liquid solution to obtain pretreated bamboo chips;
s2, dry distillation and extraction: placing the pretreated bamboo chips into a dry distillation device (1), wherein the dry distillation device (1) comprises a heating device (12) and a stirring device (13); starting the heating device (12) to directly heat and dry distill the pretreated bamboo chips, starting the stirring device (13) to enable heat generated by the heating device (12) to be uniformly distributed in the furnace body (11), and simultaneously enabling free water and water vapor in the bamboo chips to be outwards transferred in a form of seepage flow; discharging the obtained dry distillation liquid from a discharge port (16) of the dry distillation device (1);
s3, condensing and collecting: and condensing the discharged dry distillation liquid through a condenser (2) to obtain fresh bamboo juice.
2. The method of claim 1, wherein the dicationic acidic ionic liquid solution in step S1 specifically comprises: 0.1-20 parts of dicationic acidic ionic liquid and 80-150 parts of water.
3. The method of claim 1, wherein the dicationic acidic ionic liquid of step S1 is prepared by:
a. adding 1, 4-propane sultone into an ethanol solution of tetramethylethylenediamine under the condition of stirring, reacting for a period of time at 60-100 ℃, and separating the obtained solid intermediate product;
b. and (4) adding an acid solution into the solid intermediate product obtained in the step S1, stirring and reacting for a period of time at the temperature of 60-100 ℃, and removing the solvent and residual reactants in the reaction mixture to obtain the dicationic acidic ionic liquid.
4. The method of claim 1, wherein the treatment conditions in step S1 are as follows: the temperature is 10-40 ℃, and the soaking time is 1-6 h.
5. The method of claim 1, wherein the step S1 is performed by ultrasonic treatment under the following conditions: the ultrasonic frequency is 5-15 kHz, the ultrasonic temperature is 10-40 ℃, and the ultrasonic time is 10-60 min.
6. The method for preparing fresh bamboo juice as claimed in claim 1, wherein the retort unit (1) is provided with a guide rail (18) inside in step S2, the guide rail (18) is used for placing a bamboo strip cart (11) matched with the guide rail (18); the pretreated bamboo chips are placed on the bamboo chip vehicle (11) and are conveyed to a guide rail (18) in the dry distillation device (1), and heating and dry distillation are carried out in the bamboo chip vehicle (11).
7. The method of claim 1, wherein the heating and dry distillation in step S2 is performed at a temperature of 150-200 ℃.
8. Fresh bamboo juice prepared by the method according to any one of claims 1 to 7.
9. A quality detection method of fresh bamboo juice is characterized by comprising the following steps: detecting characters, identifying by thin-layer chromatography, measuring pH value, measuring relative density, measuring total solid content, measuring amino acid content and measuring total content of fructose, glucose and sucrose; the content determination of the amino acid and the total content determination of the fructose, the glucose and the sucrose adopt a high performance liquid chromatography.
10. The method of claim 9, further comprising at least one of the following additional technical features:
the pH value is 4.4-5.5, the relative density is not lower than 1.010, the total solid content is not lower than 2.0%, the content of amino acid is not lower than 62 mu g/mL, and the total content of fructose, glucose and sucrose is not higher than 27.8 mg/mL;
the thin layer chromatography identification comprises: 1) taking 20ml of fresh bamboo juice, adjusting the pH value to 1-2 by using dilute hydrochloric acid, shaking and extracting for 2 times by using diethyl ether, wherein 20ml of diethyl ether is used for each time, combining diethyl ether liquid, washing the diethyl ether liquid by using 20ml of 5% sodium bicarbonate solution, separating and drying a diethyl ether layer, and adding methanol lml into residues to dissolve the residues to obtain a sample solution; adding methanol into 2, 6-dimethoxyphenol reference substance to obtain 1 mg/lml solution as reference substance solution; pipette 5. mu.l of each of the two solutions, spot on the same silica gel G thin layer plate, and mix with toluene: ethyl acetate: formic acid (7: 1: 0.1) is used as a developing agent, developed, taken out, dried and sprayed with 5 wt% ferric trichloride ethanol solution; judging whether spots with the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution; 2) extracting fresh succus Bambusae 10ml with water saturated n-butanol under shaking for 3 times (15 ml each time), mixing n-butanol solutions, evaporating to dryness, and dissolving the residue with methanol 1ml to obtain sample solution; adding methanol into (+) -lyoniresinol-3 alpha-O-beta-D-glucopyranoside reference substance to obtain a solution containing 1mg per 1ml, and using the solution as a reference substance solution; pipetting 5 mul of each of the two solutions, dropping the solution on the same silica gel G thin layer plate, adding chloroform: methanol: formic acid (mass ratio is 4: 1: 0.1) is used as a developing agent, the developing agent is developed, taken out and dried in the air, 10 wt% phosphomolybdic acid ethanol solution is sprayed, and the mixture is heated at 105 ℃ until the spots are clearly developed; judging whether spots with the same color appear in the chromatogram of the test solution at the positions corresponding to the chromatograms of the reference solution;
the amino acid content determination comprises the following steps: 1) chromatographic conditions and system applicability test: octadecylsilane chemically bonded silica was used as a filler (column length 25cm, inner diameter 4.6mm, particle diameter 5 μm); using acetonitrile-0.1 mol/L sodium acetate solution (mass ratio of 7:93) which is used for adjusting the pH value to 6.5 by using acetic acid as a mobile phase A, and using acetonitrile-water (mass ratio of 4:1) as a mobile phase B for gradient elution; the flow rate was 1.0ml per minute; the column temperature was 40 ℃; the detection wavelength is 254nm, and the number of theoretical plates is not lower than 4000 calculated according to an alanine peak; 2) preparation of control solutions: taking a proper amount of a serine reference substance, a glycine reference substance, an arginine reference substance, a threonine reference substance, an alanine reference substance and a proline reference substance, precisely weighing, adding 0.1mol/L hydrochloric acid solution to prepare a mixed solution containing 120 mu g of serine, 12 mu g of glycine, 150 mu g of arginine, 30 mu g of threonine, 80 mu g of alanine and 50 mu g of proline in each 1ml, precisely weighing 1ml of the mixed reference solution, adding 0.5ml of an acetonitrile solution of 1mol/L triethylamine and 0.5ml of an acetonitrile solution of 0.1mol/L phenyl isothiocyanate, shaking uniformly, placing for 1 hour in a dark place, adding 2ml of n-hexane, shaking, placing for 10 minutes, centrifuging a lower layer solution, filtering, and taking a subsequent filtrate to obtain the product; 3) preparation of a test solution: precisely measuring 1ml of fresh bamboo juice, adding 0.5ml of acetonitrile solution of 1mol/L triethylamine and 0.5ml of acetonitrile solution of 0.1mol/L phenyl isothiocyanate, shaking up, standing for 1 hour in the dark, adding 2ml of n-hexane, shaking up, standing for 10 minutes, centrifuging to obtain a lower layer solution, filtering, and taking a subsequent filtrate to obtain the extract; 4) the determination method comprises the following steps: precisely sucking 2 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, and measuring;
the total content determination of the fructose, the glucose and the sucrose comprises the following steps: 1) chromatographic conditions and system applicability test: the column length is 25cm, the inner diameter is 4.6mm, and the particle size of the filler is 3 μm; acetonitrile-water (mass ratio 85: 15) is used as a mobile phase; detection by an evaporative light scattering detector. The theoretical pole number is not lower than 4000 calculated according to the fructose peak; 2) preparation of control solutions: taking appropriate amount of D-fructose, D-anhydrous glucose and sucrose as reference substances, and adding water to obtain solution containing 0.2mg per lml; 3) preparation of a test solution: precisely measuring fresh succus Bambusae 2ml, placing in 50ml measuring flask, adding water to dilute to scale, shaking, filtering, and collecting filtrate; 4) the determination method comprises the following steps: precisely absorbing 5 and 20 mul of reference solution and 5-10 mul of test solution, respectively, injecting into a liquid chromatograph, measuring, and calculating by an external standard two-point method logarithmic equation to obtain the final product.
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115166088A (en) * 2022-07-06 2022-10-11 江西省药品检验检测研究院 Method for identifying blended fresh bamboo juice based on linear relation of sugar content
CN115287087A (en) * 2022-08-23 2022-11-04 铜鼓县伟升实业有限公司 Automatic control dry distillation fresh bamboo strip pressureless box type fresh bamboo juice extraction device
CN115447921A (en) * 2022-08-11 2022-12-09 江西李氏烤鲜竹沥药业有限公司 Bamboo chip raw material storage method for baking fresh bamboo juice
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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115166088A (en) * 2022-07-06 2022-10-11 江西省药品检验检测研究院 Method for identifying blended fresh bamboo juice based on linear relation of sugar content
CN115447921A (en) * 2022-08-11 2022-12-09 江西李氏烤鲜竹沥药业有限公司 Bamboo chip raw material storage method for baking fresh bamboo juice
CN115287087A (en) * 2022-08-23 2022-11-04 铜鼓县伟升实业有限公司 Automatic control dry distillation fresh bamboo strip pressureless box type fresh bamboo juice extraction device
CN115287087B (en) * 2022-08-23 2024-05-24 铜鼓县伟升实业有限公司 Automatic control dry distillation fresh bamboo strip pressureless box type fresh bamboo juice extracting device
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