CN109621926A - A kind of pair of putrescine has the Nanowire d type molecular engram film and preparation method thereof of efficient selective - Google Patents
A kind of pair of putrescine has the Nanowire d type molecular engram film and preparation method thereof of efficient selective Download PDFInfo
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- CN109621926A CN109621926A CN201910090339.8A CN201910090339A CN109621926A CN 109621926 A CN109621926 A CN 109621926A CN 201910090339 A CN201910090339 A CN 201910090339A CN 109621926 A CN109621926 A CN 109621926A
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
- B01J20/28038—Membranes or mats made from fibers or filaments
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
- B01D15/08—Selective adsorption, e.g. chromatography
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/50—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyalcohols, polyacetals or polyketals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/39—Electrospinning
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D2323/46—Impregnation
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Abstract
The invention discloses the Nanowire d type molecular engram films and preparation method thereof that a kind of pair of putrescine has efficient selective, preparation method is: by polyvinyl alcohol, stirring and dissolving is in deionized water at 85-95 DEG C, then 1 is added at 65-75 DEG C, 4- butanediol stirs to get spinning solution, then puts into the 12-21 for being 0.51-0.60 mm with internal diameter#The syringe of syringe needle, places a syringe in electrostatic spinning machine, and spinning prepares micro/nano fibrous membrane material, is eluted with methanol, and ninhydrin solution is then added dropwise and obtains a kind of novel nanofiber molecular engram film.Trace micro/nano fibrous membrane material prepared by the present invention is nano-level thin-membrane, has good adsorption capacity to putrescine, has certain regeneration service performance.Raw material is very safe macromolecule organic material, have many advantages, such as it is nontoxic, without side-effects, have good biocompatibility, be widely used in field of biomedicine.
Description
Technical field
The present invention devises the Nanowire d type molecular engram film that a kind of pair of putrescine has efficient selective, belongs to function height
Molecular material field.
Background technique
Putrescine is a kind of toxic diamines of stench, is generated by ornithine.Putrescine is ubiquitous in food, is especially sending out
In ferment food (such as cheese, beer, grape wine etc.), meat products and aquatic products.The content of putrescine is considered as freshness in food
Index.Putrescine is received significant attention and is studied in fields such as agricultural, food safety detection, tumour and animal husbandry.Putrescine has
The potentiality that enhancing human antibody's level and better nutrient absorption utilize reduce fruit and fall rate and improve fruit quality and detection
The functions such as cancerous tissue have been documented.However, excessive putrescine also results in low blood pressure, the diseases such as tetanus and quadriplegia
Disease can also generate carcinogen by reacting with nitrite, inhibit histamine and the relevant metabolic enzyme activity of tyrasamine.Therefore, fixed
Amount detection putrescine becomes an important topic.Molecular imprinting technology can be prepared with having single-minded identification to target molecule
Polymer provides a kind of effective, quick and easy method for the detection of putrescine.However, molecular imprinting technology synthesis is big
Most imprinted materials show low sensitivity and the speed of response is due to being difficult to obtain accessibility and permeability.Nano material and
The combined use of molecular engram is the effective ways for overcoming these difficult.Electrostatic spinning is a kind of simple and general technology, is led to
Cross the continuous fiber using electrostatic field production diameter range from several microns to tens nanometer.Due to the random deposition of fiber, gained
Tunica fibrosa has high-specific surface area and high porosity.Since putrescine is generated forever with reacting for ninhydrin by the irreversible approach of two steps
Long covalent bond, therefore, it is difficult to remove putrescine, so selecting 1,4-butanediol as template analog.This patent is with polyvinyl alcohol
For spinning substrate, spin trace nano fibrous membrane, by the color developing effect of ninhydrin come it is more convenient, effectively detect putrescine
Adsorbance.
Summary of the invention
It is an object of the invention in view of the shortcomings of the prior art, providing nanometer of a kind of pair of putrescine with efficient selective
Fibrous type molecular engram film.Nanofiber molecular engram film prepared by the present invention has nanostructure, is capable of providing more traces and knows
The adsorption capacity of target putrescine is improved in other site.
To achieve the above object, the technical solution adopted by the present invention is that:
A kind of pair of putrescine has the preparation method of the Nanowire d type molecular engram film of efficient selective, comprising the following steps:
(1) 1.2-4.2 g polyvinyl alcohol (PVA) is dissolved in 25.755-28.755 mL deionized water at 85-95 DEG C,
Then 0-165 mg 1,4-butanediol (BDO) template is added at 65-75 DEG C, stirring and dissolving obtains spinning solution；
(2) spinning solution for obtaining (1) extracts 5-10 mL with 10-20 mL syringe, and putting on internal diameter is 0.51-0.60 mm
12-21#Syringe needle, then the syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning, spinning condition are as follows:
Positive voltage: 9-21 Kv；Spinning distance: 10-30 cm；Drum rotation speed: 300-900 r/min；In spinning temperature: 20-27 DEG C,
Spinning humidity: spinning 2-3 h prepares micro/nano fibrous membrane material under 50-68 %；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
Moisture is removed at DEG C；
(4) 10-20 mL methanol is added in the fiber block of drying and carries out standing elution, change an eluent, first time 5-7 h,
It carries out impregnating 1-4 h again, finally takes out and place room temperature volatile dry, 265-365 μ L 0.850-1.150 mg/g is then added dropwise
Ninhydrin solution obtains trace micro/nano fibrous membrane material.
The trace micro/nano fibrous membrane material is measured to the adsorbance and adsorptive selectivity of putrescine by software I mage J,
Specific measurement method are as follows:
(1) adsorbance: the tunica fibrosa of the mm of 3 mm × 3 is attached at the top of culture dish, is added in the pallet of the bottom of culture dish
The putrescine solution of 50-70 μ L 0-0.650 mg/mL, two culture dishes mutually clasp sealing, and colour developing is adsorbed at 60-70 DEG C
35-45 min is calculated putrescine adsorbance by following formula and trace is imitated with the gray value to develop the color on software I mage J measurement tunica fibrosa
Rate:
Q e =(164.7-Y)/3.76
IE=Q MIP /Q NIP
Wherein,Q e (μ g/cm2) andYBe putrescine adsorption liquid equilibrium concentration and corresponding gray value,Q MIP It is trace Nanowire
The adsorbance of film is tieed up,Q NIP It is the adsorbance of non-trace nano fibrous membrane, IE is the imprinting efficiency of nano fibrous membrane.
(2) adsorptive selectivity: the concentration of configuration cadaverine, spermidine or spermine is the mixed solution of 0.620 mg/mL, is taken
The tunica fibrosa of the mm of 3 mm × 3 is in the 60 positive overhead of μ L mixed solution, 40 min of absorption colour developing, the absorption to putrescine at 65 DEG C
Selectivity calculates as follows:
K D =Q e /C e
SF=K D1/K D2
Wherein,K D It is static allocation coefficient；Q e (μ g/cm2) andC e (mg/mL) trace nano fibrous membrane adsorption equilibrium is respectively represented
When adsorbance and adsorption liquid concentration；SF is separation factor；K D1 WithK D2 The respectively static allocation coefficient of template molecule
With the static allocation coefficient for competing biological amine molecule.
The invention has the following advantages that
(1) present invention has nontoxic to the human body, without side-effects and biological using the nano fibrous membrane that polyvinyl alcohol is spun by substrate
The advantages of compatibility, can be improved absorption of the imprinted material to target putrescine simultaneous with the molecular engram material of imprinted sites
Ability；
(2) it can produce the object of bluish violet in printing process containing ninhydrin substance on the nano fibrous membrane that the present invention is spun into
Matter is conducive to the observation adsorbed for putrescine, thus convenient and effective detection, absorption putrescine；
(3) present invention utilizes electrostatic spinning technique, so that site accessibility and permeability, are conducive to improve nano fibrous membrane
Sensibility and the speed of response, with shorter time adsorption saturation putrescine.
Trace micro/nano fibrous membrane material prepared by the present invention is nano-level thin-membrane in homogeneous thickness, is had to putrescine good
Adsorption capacity, renewable recycling are selected, and preparation process is simple, at low cost, stability is good, nontoxic and potential biology
Characteristic can be widely used for the adsorbing separation of putrescine, have wide biological medicine prospect.
Detailed description of the invention
Fig. 1 is the absorption colour developing figure of the made micro/nano fibrous membrane material of embodiment 1；
Fig. 2 is the absorption colour developing figure of the made micro/nano fibrous membrane material of comparative example 1；
The influence that Fig. 3 adsorbs putrescine for the adsorption time of embodiment 1 and the made micro/nano fibrous membrane material of comparative example 1.
Specific embodiment
In order to make content of the present invention easily facilitate understanding, the present invention will be further described for following embodiment,
But protection scope of the present invention is not limited to these embodiments.
Embodiment 1
(1) 3 g polyvinyl alcohol (PVA) are dissolved in 26.955 mL deionized waters at 90 DEG C, are then added at 70 DEG C
0.045 mg 1,4-butanediol (BDO) template, stirring and dissolving obtain spinning solution；
(2) spinning solution for obtaining (1) extracts 5 mL with 20 mL syringes, and puts on internal diameter as the 21 of 0.51 mm#Needle
Then syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning by head, spinning condition are as follows: positive voltage: 15
Kv；Spinning distance: 15 cm；Drum rotation speed: 600 r/min；In spinning temperature: 20-27 DEG C, spinning humidity: being spun under 50-68 %
2 h of silk prepare micro/nano fibrous membrane material；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
It is dried at DEG C；
(4) 10 mL methanol are added in the fiber block of drying and carry out standing elution, change an eluent, for the first time 6 h, then into
Row impregnates 2 h, finally takes out and places room temperature volatile dry, 315 μ L, 0.984 mg/g ninhydrin solution is then added dropwise, is printed
Mark micro/nano fibrous membrane material.
(5) obtained trace nano fibrous membrane is hanged to filling 60 μ L, 0.620 mg/mL putrescine solution and control induction
Distance is 0.4 cm, 40 min of absorption colour developing at being 65 DEG C in environment temperature.
Comparative example 1
(1) 3 g polyvinyl alcohol (PVA) are dissolved in 26.955 mL deionized waters at 90 DEG C, stirring and dissolving obtains spinning
Liquid；
(2) spinning solution for obtaining (1) extracts 5 mL with 20 mL syringes, and puts on internal diameter as the 21 of 0.51 mm#Needle
Then syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning by head, spinning condition are as follows: positive voltage: 15
Kv；Spinning distance: 15 cm；Drum rotation speed: 600 r/min；In spinning temperature: 20-27 DEG C, spinning humidity: being spun under 50-68 %
2 h of silk prepare micro/nano fibrous membrane material；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
It is dried at DEG C；
(4) 10 mL methanol are added in the fiber block of drying and carry out standing elution, change an eluent, for the first time 6 h, then into
Row impregnates 2 h, finally takes out and places room temperature volatile dry, 315 μ L, 0.984 mg/g ninhydrin solution is then added dropwise, obtains non-
Trace micro/nano fibrous membrane material.
(5) obtained non-trace nano fibrous membrane is hanged to filling 60 μ L, 0.620 mg/mL putrescine solution and control sense
Should be apart from for 0.4 cm, 40 min of absorption colour developing at being 65 DEG C in environment temperature.
Embodiment 1 and the made nano-fiber material of comparative example 1 absorption colour developing figure are as illustrated in fig. 1 and 2, as seen from the figure,
A kind of royal purple color substance, and the indigo plant of embodiment 1 is all presented in the micro/nano fibrous membrane material surface that embodiment 1 and comparative example 1 synthesize
Purple doubles, and area is bigger, this illustrates that trace nano fibrous membrane has very strong adsorption capacity.Non- trace nano fibrous membrane
Absorption and recognition performance to putrescine are as shown in Fig. 2, figure it is seen that be added without template analog 1,4-butanediol advantageous
In the non-specific adsorption of putrescine.When adsorption time is 40 min, the adsorbance of embodiment 1 is up to 32.31 μ g/cm2, comparison
Example 1 is 14.32 μ g/cm2, it is evident that embodiment 1 is higher than comparative example 1, and imprinting efficiency is up to 2.25.It can be seen that the present invention due to
1,4-butanediol is template analog, binding molecule engram technology and electrostatic spinning technique, effectively improves trace Nanowire
Tie up the specific adsorption ability of film, it can be seen that, which can be used as the excellent material of putrescine absorption and identification
Material.
Adsorptive selectivity
Putrescine, cadaverine, spermidine or the spermine for weighing 62.0 mg respectively are dissolved in 100 mL ethyl alcohol, and configuration is 0.620 mg/
The mixed solution of mL takes trace nano fibrous membrane made from the embodiment 1 of the mm of 3 mm × 3 to be suspended in 60 μ L mixed solutions and controls
Distance of reaction processed is 0.4 cm, 40 min of absorption colour developing at 65 DEG C.
Experimental calculation data are as follows: putrescineK D1 =33.07624 μg/cm2/0.620 mg/mL；CadaverineK D2 =29.08688 μ
g/cm2/0.620 mg/mL；SpermidineK D3 =16.49823 μg/cm2/0.620 mg/mL；SpermineK D4 =15.25709 μg/
cm2/0.620 mg/mL；That is putrescine SF1=1, cadaverine SF2=1.13715；Spermidine SF3=2.00484；Spermine SF4=2.16793。
The result shows that the value with SF is bigger, illustrating trace nano fibrous membrane more has high efficiency selected performance, spermidine and
The SF value of spermine is all larger than 2, target molecule can be distinguished simply by colour developing degree, cadaverine is similar to putrescine structure, causes
Adsorbance is close, but according to the SF of cadaverine, and can be distinguished.
Embodiment 2
(1) 3 g polyvinyl alcohol (PVA) are dissolved in 26.925 mL deionized waters at 90 DEG C, are then added at 70 DEG C
0.075 mg 1,4-butanediol (BDO) template, stirring and dissolving obtain spinning solution；
(2) spinning solution for obtaining (1) extracts 5 mL with 20 mL syringes, and puts on internal diameter as the 21 of 0.51 mm#Needle
Then syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning by head, spinning condition are as follows: positive voltage: 15
Kv；Spinning distance: 15 cm；Drum rotation speed: 600 r/min；In spinning temperature: 20-27 DEG C, spinning humidity: being spun under 50-68 %
2 h of silk prepare micro/nano fibrous membrane material；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
It is dried at DEG C；
(4) 10 mL methanol are added in the fiber block of drying and carry out standing elution, change an eluent, for the first time 6 h, then into
Row impregnates 2 h, finally takes out and places room temperature volatile dry, 315 μ L, 0.984 mg/g ninhydrin solution is then added dropwise, is printed
Mark micro/nano fibrous membrane material.
(5) obtained trace nano fibrous membrane is hanged to filling 60 μ L, 0.620 mg/mL putrescine solution and control induction
Distance is 0.4 cm, 40 min of absorption colour developing at being 65 DEG C in environment temperature.
Embodiment 3
(1) 3 g polyvinyl alcohol (PVA) are dissolved in 26.925 mL deionized waters at 90 DEG C, are then added at 70 DEG C
0.075 mg 1,4-butanediol (BDO) template, stirring and dissolving obtain spinning solution；
(2) spinning solution for obtaining (1) extracts 5 mL with 20 mL syringes, and puts on internal diameter as the 21 of 0.51 mm#Needle
Then syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning by head, spinning condition are as follows: positive voltage: 15
Kv；Spinning distance: 15 cm；Drum rotation speed: 600 r/min；In spinning temperature: 20-27 DEG C, spinning humidity: being spun under 50-68 %
2 h of silk prepare micro/nano fibrous membrane material；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
It is dried at DEG C；
(4) 10 mL methanol are added in the fiber block of drying and carry out standing elution, change an eluent, for the first time 6 h, then into
Row impregnates 2 h, finally takes out and places room temperature volatile dry, 290 μ L, 0.984 mg/g ninhydrin solution is then added dropwise, is printed
Mark micro/nano fibrous membrane material.
(5) obtained trace nano fibrous membrane is hanged to filling 60 μ L, 0.620 mg/mL putrescine solution and control induction
Distance is 0.4 cm, 40 min of absorption colour developing at being 65 DEG C in environment temperature.
Embodiment 4
(1) 2.4 g polyvinyl alcohol (PVA) are dissolved in 27.555 mL deionized waters at 90 DEG C, are then added at 70 DEG C
Enter 0.045 mg 1,4-butanediol (BDO) template, stirring and dissolving obtains spinning solution；
(2) spinning solution for obtaining (1) extracts 5 mL with 20 mL syringes, and puts on internal diameter as the 21 of 0.51 mm#Needle
Then syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning by head, spinning condition are as follows: positive voltage: 15
Kv；Spinning distance: 15 cm；Drum rotation speed: 600 r/min；In spinning temperature: 20-27 DEG C, spinning humidity: being spun under 50-68 %
2 h of silk prepare micro/nano fibrous membrane material；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
It is dried at DEG C；
(4) 10 mL methanol are added in the fiber block of drying and carry out standing elution, change an eluent, for the first time 6 h, then into
Row impregnates 2 h, finally takes out and places room temperature volatile dry, 315 μ L, 0.984 mg/g ninhydrin solution is then added dropwise, is printed
Mark micro/nano fibrous membrane material.
(5) obtained trace nano fibrous membrane is hanged to filling 60 μ L, 0.620 mg/mL putrescine solution and control induction
Distance is 0.4 cm, 40 min of absorption colour developing at being 65 DEG C in environment temperature.
Embodiment 5
(1) 2.4 g polyvinyl alcohol (PVA) are dissolved in 26.925 mL deionized waters at 90 DEG C, are then added at 70 DEG C
Enter 0.075 mg 1,4-butanediol (BDO) template, stirring and dissolving obtains spinning solution；
(2) spinning solution for obtaining (1) extracts 5 mL with 20 mL syringes, and puts on internal diameter as the 21 of 0.51 mm#Needle
Then syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning by head, spinning condition are as follows: positive voltage: 15
Kv；Spinning distance: 15 cm；Drum rotation speed: 600 r/min；In spinning temperature: 20-27 DEG C, spinning humidity: being spun under 50-68 %
2 h of silk prepare micro/nano fibrous membrane material；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
It is dried at DEG C；
(4) 10 mL methanol are added in the fiber block of drying and carry out standing elution, change an eluent, for the first time 6 h, then into
Row impregnates 2 h, finally takes out and places room temperature volatile dry, 315 μ L, 0.984 mg/g ninhydrin solution is then added dropwise, is printed
Mark micro/nano fibrous membrane material.
(5) obtained trace nano fibrous membrane is hanged to filling 60 μ L, 0.620 mg/mL putrescine solution and control induction
Distance is 0.4 cm, 40 min of absorption colour developing at being 65 DEG C in environment temperature.
The foregoing is merely presently preferred embodiments of the present invention, it is all according to the done equivalent change of scope of the present invention patent with repair
Decorations, are all covered by the present invention.
Claims (6)
1. the preparation method that a kind of pair of putrescine has the Nanowire d type molecular engram film of efficient selective, which is characterized in that packet
Include following steps:
(1) 1.2-4.2 g polyvinyl alcohol is dissolved in 25.755-28.755 mL deionized water at 85-95 DEG C, is then existed
0.045-165 mg 1,4-butanediol template is added at 65-75 DEG C, stirring and dissolving obtains spinning solution；
(2) spinning solution for obtaining (1) extracts 5-10 mL with 10-20 mL syringe, and putting on internal diameter is 0.51-0.60 mm
12-21#Syringe needle, then the syringe with spinning solution is placed in electrostatic spinning machine and carries out spinning, spinning condition are as follows:
Positive voltage: 9-21 Kv；Spinning distance: 10-30 cm；Drum rotation speed: 300-900 r/min；In spinning temperature: 20-27 DEG C,
Spinning humidity: spinning 2-3 h prepares micro/nano fibrous membrane material under 50-68 %；
(3) nano fibrous membrane that (2) obtain is removed, the fiber block of the mm of 3 mm × 3 is cut into blade, is then placed on baking oven 60
It is dried at DEG C；
(4) 10-20 mL eluent is added in the fiber block of drying and carries out standing elution, elution time 5-7 h is changed and once washed
De- liquid, then carry out impregnating 1-4 h, it finally takes out and places room temperature volatile dry, 265-365 μ L 0.850-1.150 is then added dropwise
Mg/g ninhydrin solution obtains trace micro/nano fibrous membrane material.
2. the preparation side that a kind of pair of putrescine as described in claim 1 has the Nanowire d type molecular engram film of efficient selective
Method, it is characterised in that: the volume that the deionized water in step (1) is added is 25.755-28.755 mL；Polyvinyl alcohol dosage is
1.2-4.2 g。
3. the preparation side that a kind of pair of putrescine as described in claim 1 has the Nanowire d type molecular engram film of efficient selective
Method, it is characterised in that: step (2) syringe is 10-20 mL；Internal diameter is the 12-21 of 0.51-0.60 mm#Syringe needle；Spinning
The positive voltage of condition is 9-21 Kv；Spinning distance is 10-30 cm；Drum rotation speed is 300-900 r/min.
4. the preparation side that a kind of pair of putrescine as described in claim 1 has the Nanowire d type molecular engram film of efficient selective
Method, it is characterised in that: the spinning temperature in step (2) is 20-27 DEG C；Spinning humidity is 50-68 %;The spinning time is 2-3
h。
5. the preparation side that a kind of pair of putrescine as described in claim 1 has the Nanowire d type molecular engram film of efficient selective
Method, it is characterised in that: the gel in step (3) is cut into the mm threadiness of 3 mm × 3.
6. the preparation side that a kind of pair of putrescine as described in claim 1 has the Nanowire d type molecular engram film of efficient selective
Method, it is characterised in that: the volume of the eluent in step (4) is 10-20 mL, and eluent is methanol；Elution time for the first time be
5-7h, second is 1-4 h；It is 265-365 μ L, concentration 0.850-1.150mg/g that volume, which is added, in ninhydrin solution.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910090339.8A CN109621926A (en) | 2019-01-30 | 2019-01-30 | A kind of pair of putrescine has the Nanowire d type molecular engram film and preparation method thereof of efficient selective |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910090339.8A CN109621926A (en) | 2019-01-30 | 2019-01-30 | A kind of pair of putrescine has the Nanowire d type molecular engram film and preparation method thereof of efficient selective |
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| CN109621926A true CN109621926A (en) | 2019-04-16 |
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