CN106198661A - Electrochemical determination method of phenylethylamine - Google Patents
Electrochemical determination method of phenylethylamine Download PDFInfo
- Publication number
- CN106198661A CN106198661A CN201610612908.7A CN201610612908A CN106198661A CN 106198661 A CN106198661 A CN 106198661A CN 201610612908 A CN201610612908 A CN 201610612908A CN 106198661 A CN106198661 A CN 106198661A
- Authority
- CN
- China
- Prior art keywords
- electrode
- phenethylamine
- solution
- gold
- determination method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- BHHGXPLMPWCGHP-UHFFFAOYSA-N Phenethylamine Chemical compound NCCC1=CC=CC=C1 BHHGXPLMPWCGHP-UHFFFAOYSA-N 0.000 title claims abstract description 118
- 238000000034 method Methods 0.000 title claims abstract description 42
- 239000000243 solution Substances 0.000 claims abstract description 76
- 229940117803 phenethylamine Drugs 0.000 claims abstract description 54
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000010931 gold Substances 0.000 claims abstract description 21
- 229910052737 gold Inorganic materials 0.000 claims abstract description 21
- WGTASENVNYJZBK-UHFFFAOYSA-N 3,4,5-trimethoxyamphetamine Chemical compound COC1=CC(CC(C)N)=CC(OC)=C1OC WGTASENVNYJZBK-UHFFFAOYSA-N 0.000 claims abstract description 11
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000012670 alkaline solution Substances 0.000 claims abstract description 5
- 238000012417 linear regression Methods 0.000 claims abstract description 5
- 229910021607 Silver chloride Inorganic materials 0.000 claims abstract description 4
- 238000000840 electrochemical analysis Methods 0.000 claims abstract description 4
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims abstract description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 69
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 229920001661 Chitosan Polymers 0.000 claims description 29
- 150000001412 amines Chemical class 0.000 claims description 14
- ZBKIUFWVEIBQRT-UHFFFAOYSA-N gold(1+) Chemical compound [Au+] ZBKIUFWVEIBQRT-UHFFFAOYSA-N 0.000 claims description 12
- 241000251468 Actinopterygii Species 0.000 claims description 11
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims description 11
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 9
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 238000013019 agitation Methods 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 6
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 6
- 239000012279 sodium borohydride Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 208000035126 Facies Diseases 0.000 claims description 5
- 238000002203 pretreatment Methods 0.000 claims description 5
- 235000014101 wine Nutrition 0.000 claims description 5
- 230000033228 biological regulation Effects 0.000 claims description 4
- HEDRZPFGACZZDS-UHFFFAOYSA-N chloroform Substances ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000005374 membrane filtration Methods 0.000 claims description 4
- 125000004108 n-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 239000012047 saturated solution Substances 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- 238000005034 decoration Methods 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 230000008439 repair process Effects 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 6
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims 3
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 claims 1
- 239000002253 acid Substances 0.000 claims 1
- 239000003513 alkali Substances 0.000 claims 1
- 239000003292 glue Substances 0.000 claims 1
- 238000012956 testing procedure Methods 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 8
- 230000004044 response Effects 0.000 abstract description 2
- 235000013305 food Nutrition 0.000 description 9
- 230000000035 biogenic effect Effects 0.000 description 8
- KIDHWZJUCRJVML-UHFFFAOYSA-N putrescine Chemical compound NCCCCN KIDHWZJUCRJVML-UHFFFAOYSA-N 0.000 description 8
- ATHGHQPFGPMSJY-UHFFFAOYSA-N spermidine Chemical compound NCCCCNCCCN ATHGHQPFGPMSJY-UHFFFAOYSA-N 0.000 description 8
- PFNFFQXMRSDOHW-UHFFFAOYSA-N spermine Chemical compound NCCCNCCCCNCCCN PFNFFQXMRSDOHW-UHFFFAOYSA-N 0.000 description 8
- NTYJJOPFIAHURM-UHFFFAOYSA-N Histamine Chemical compound NCCC1=CN=CN1 NTYJJOPFIAHURM-UHFFFAOYSA-N 0.000 description 6
- VHRGRCVQAFMJIZ-UHFFFAOYSA-N cadaverine Chemical compound NCCCCCN VHRGRCVQAFMJIZ-UHFFFAOYSA-N 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- DZGWFCGJZKJUFP-UHFFFAOYSA-N tyramine Chemical compound NCCC1=CC=C(O)C=C1 DZGWFCGJZKJUFP-UHFFFAOYSA-N 0.000 description 6
- 229910004042 HAuCl4 Inorganic materials 0.000 description 5
- 239000005700 Putrescine Substances 0.000 description 4
- VYFYYTLLBUKUHU-UHFFFAOYSA-N dopamine Chemical compound NCCC1=CC=C(O)C(O)=C1 VYFYYTLLBUKUHU-UHFFFAOYSA-N 0.000 description 4
- 229940063673 spermidine Drugs 0.000 description 4
- 229940063675 spermine Drugs 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 229960001340 histamine Drugs 0.000 description 3
- 239000002858 neurotransmitter agent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229960003732 tyramine Drugs 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 229960003638 dopamine Drugs 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000000796 flavoring agent Substances 0.000 description 2
- 235000013355 food flavoring agent Nutrition 0.000 description 2
- 230000036039 immunity Effects 0.000 description 2
- 235000013372 meat Nutrition 0.000 description 2
- 239000012074 organic phase Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- RQEUFEKYXDPUSK-UHFFFAOYSA-N 1-phenylethylamine Chemical compound CC(N)C1=CC=CC=C1 RQEUFEKYXDPUSK-UHFFFAOYSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 208000027418 Wounds and injury Diseases 0.000 description 1
- 229920006221 acetate fiber Polymers 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 125000001931 aliphatic group Chemical group 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 150000001413 amino acids Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 239000000935 antidepressant agent Substances 0.000 description 1
- 229940005513 antidepressants Drugs 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 235000013405 beer Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000004071 biological effect Effects 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 229940124630 bronchodilator Drugs 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 210000004027 cell Anatomy 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 235000013351 cheese Nutrition 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000019219 chocolate Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 210000003722 extracellular fluid Anatomy 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000021107 fermented food Nutrition 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 150000002343 gold Chemical class 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 125000000623 heterocyclic group Chemical group 0.000 description 1
- 208000014674 injury Diseases 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 235000013622 meat product Nutrition 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 230000001537 neural effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 description 1
- 102000039446 nucleic acids Human genes 0.000 description 1
- 108020004707 nucleic acids Proteins 0.000 description 1
- 150000007523 nucleic acids Chemical class 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 235000021134 protein-rich food Nutrition 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000003196 psychodysleptic agent Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 235000013580 sausages Nutrition 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
- -1 tryptamines Chemical compound 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Biological Materials (AREA)
Abstract
The invention relates to the technical field of electroanalytical chemistry, and particularly discloses an electrochemical determination method of phenylethylamine. The method specifically comprises the following steps: s11, constructing a three-electrode electrochemical test system by using a gold electrode modified by colloidal gold as a working electrode, a platinum wire electrode as an auxiliary electrode and an Ag/AgCl electrode as a reference electrode; s12, placing the three-electrode system in an alkaline solution, scanning by using an i-t curve method when the initial potential is 0.08-0.12V, adding the solution to be detected after the baseline is stable, scanning until the baseline is stable, and measuring the current difference of the response of phenethylamine on the electrodes; and S13, calculating the content of the phenylethylamine according to a linear regression equation of the current difference of the phenylethylamine on the electrode and the concentration of the phenylethylamine. The method can quickly detect the content of the phenethylamine, and has the advantages of low detection limit, strong anti-interference performance and good reproducibility.
Description
Technical field
The present invention relates to Electroanalytical Chemistry technical field, be specifically related to the electrochemical determination method of a kind of phenethylamine.
Background technology
Biogenic amine is the general name of a nitrogenous small molecular weight compounds of class.Architectural feature according to biogenic amine is divided into 3 big classes:
(1) aliphatic, such as cadaverine, putrescine, spermidine, spermine etc.；(2) aromatic series, such as phenethylamine, tyramine etc.；(3) heterocyclic, such as color
Amine, histamine etc..Biogenic amine is present in various vegeto-animal tissue, and it is normal active component in biologic artifact, dynamic
Plant part has important physiological action.Such as, spermine, spermidine, putrescine and cadaverine etc. are all in biological activity cell
An indispensable part, plays pivotal role in terms of regulation protein and the synthesis of nucleic acid and biomembranous stability.
Additionally, biogenic amine is also universally present in numerous food, especially fermented food and protein rich food.As: meat system
Product, aquatic products, cheese, sausage, medicated beer, wine etc..Biogenic amine main in food includes: histamine, tyramine, β-phenethylamine,
Multiple monoamine and the polyamine substances such as cadaverine, putrescine, tryptamines, spermine and spermidine.At the protein content such as meat products, aquatic products more
In abundant food, the enzyme produced due to related microorganisms can be catalyzed to be sloughed the carboxyl of free amino acid and produces biogenic amine, institute
Height with Content of Biogenic Amines is closely related with its quality.
Phenethylamine is also known as 2-phenethylamine or β-phenethylamine, and molecular formula is C8H11N, its chemical constitution is relatively simple, and it belongs to virtue
Fragrant race amine substance.It is widely present in the food such as chocolate, milk, meat and wine, especially after fermentable
Food.In human body, phenethylamine is a kind of alkaloid and monoamine neurotransmitter, it is possible to promote dopamine in extracellular fluid
Level, the activation of suppression dopamine neuronal, is used for treating depression simultaneously.In human brain, β-phenethylamine have neuromodulator,
Neurotransmitter and the effect of spike amine.Phenethylamine, as important medicine and dyestuff intermediate, is pharmaceutically being mainly used in synthesis
Following medicine: beta stimulant, antidepressants, psychedelic drug, god enter to feel exciting agent, fall appetite agent, bronchodilator etc..Phenethylamine class
Material pharmacologically can use as important drugs, but, if phenethylamine is present in excess in food, then health can be caused
Certain injury.Therefore, the content detecting the biogenic amine in food such as fermentation based food, animal-derived food and wine is the heaviest
Want.
Summary of the invention
The technical problem to be solved is, contains to overcome shortage in prior art can quickly detect phenethylamine
The method of amount, it is provided that the electrochemical determination method of a kind of phenethylamine.The method is when being used for detecting phenethylamine, and detection speed is fast,
Detection limit is low.
Above-mentioned technical problem to be solved by this invention, is achieved by the following technical programs:
The electrochemical determination method of a kind of phenethylamine, uses the gold electrode that gold colloidal is modified, and when initial potential is 0.1V, uses
I-t curve method measures the content of phenethylamine.
The present invention shows through the substantial amounts of experimentation of inventor, the gold electricity that the gold colloidal using the present invention to prepare is modified
Pole, uses i-t curve method to measure phenethylamine under conditions of of the present invention, it is possible to quickly the phenethylamine in detection sample contains
Amount, and detection limit is low, strong interference immunity, favorable reproducibility.
Preferably, the electrochemical determination method of described phenethylamine, specifically comprise the steps of:
S11. with gold colloidal modify gold electrode as working electrode, platinum electrode is auxiliary electrode, and Ag/AgCl electrode is reference
Electrode, builds three-electrode electro Chemical test system；
S12. three-electrode system is placed in alkaline solution, sweeps when initial potential is 0.08 ~ 0.12V with i-t curve method
Retouch, after baseline stability, add solution to be measured, then scan to stable, measure the difference between current that phenethylamine responds on electrode；
S13. the difference between current (-I, nA) responded on electrode according to phenethylamine is linear with phenethylamine concentration (c, μm ol/L)
Regression equation, calculates the content of phenethylamine.
It is further preferred that the alkaline solution described in step S12 is pH value is the NaOH solution of 12 ~ 13；At the beginning of described
Beginning current potential is 0.08 ~ 0.10V.
It is further preferred that the equation of linear regression described in step S13 is-I=7.783c+1.181(R=
0.997).
Preferably, the gold electrode that the gold colloidal described in step S11 is modified is prepared into by the method comprised the steps of
Arrive:
S21. dissolving chitosan in and being made into chitosan content in the acetic acid solution that volume fraction is 0.5 ~ 2.0% is 1 ~ 3mg/mL
Chitosan acetic acid solution；
S22. in chitosan acetic acid solution, add the gold chloride (HAuCl of 5 ~ 15 mmol/L4) solution, stir 20 ~ 40min,
Chitosan acetic acid solution and gold chloride (HAuCl4) volume ratio of solution is 1.5 ~ 31；
The most under agitation it is added dropwise over the aqueous solution of 0.05 ~ 0.2mol/L sodium borohydride, until solution becomes transparent wine
Redness, obtains colloidal gold solution；
S24. depletion electrode, after polishing, cleaning, drips colloidal gold solution in gold electrode surfaces, the most i.e. obtains gold colloidal and repair
The gold electrode of decorations.
Join it is further preferred that step S21 dissolves chitosan in the acetic acid solution that volume fraction is 1.0 ~ 2.0%
The chitosan acetic acid solution becoming chitosan content to be 2 ~ 3mg/mL.
Most preferably, step S21 dissolves chitosan in the acetic acid solution that volume fraction is 1.0% and be made into chitosan
Content is the chitosan acetic acid solution of 2mg/mL.
It is further preferred that step S22 adds in chitosan acetic acid solution the gold chloride of 10 ~ 15 mmol/L
(HAuCl4) solution, stir 20 ~ 30min, chitosan acetic acid solution and gold chloride (HAuCl4) volume ratio of solution is 1.5 ~ 21.
Most preferably, step S22 adds in chitosan acetic acid solution the gold chloride (HAuCl of 10mmol/L4) solution,
Stirring 30min, chitosan acetic acid solution and gold chloride (HAuCl4) volume ratio of solution is 21.
It is further preferred that step S23 is under agitation added dropwise over the aqueous solution of 0.1 ~ 0.2mol/L sodium borohydride.
Most preferably, step S23 is under agitation added dropwise over the aqueous solution of 0.1mol/L sodium borohydride.
It is further preferred that at the colloidal gold solution of gold electrode surfaces dropping 2 ~ 5 μ L in step S24.
Most preferably, step S24 drips the colloidal gold solution of 3 μ L in gold electrode surfaces.
Preferably, the electrochemical determination method of described phenethylamine, for measuring the content of phenethylamine in fish juice, its test
Also comprising pre-treatment step in step, described pre-treatment step is as follows:
Take fish juice sample, with membrane filtration, add sodium chloride and make solution saturated, measure 8 ~ 12mL saturated solution, use NaOH solution
Regulation pH to 12 ~ 13, adds n-butyl alcohol-chloroform mixed liquor that 4 ~ 6mL volume ratio is 11, shakes, is centrifuged, takes upper strata
Organic facies, repeats 2 ~ 5 times, merges organic facies, adds the NaOH solution dissolving that pH value is 12 ~ 13 after drying, obtains solution to be measured.
Most preferably, described pre-treatment step is as follows:
Take fish juice sample, with membrane filtration, add sodium chloride and make solution saturated, measure 10mL saturated solution, adjust by NaOH solution
Joint pH to 12.7, adds n-butyl alcohol-chloroform mixed liquor that 5mL volume ratio is 1:1, shakes, is centrifuged, takes upper strata organic
Phase, is repeated 2 times, and merges organic facies, adds the NaOH solution dissolving that pH value is 12.7 after drying, obtains solution to be measured.
Beneficial effect: (1) the invention provides the electrochemical determination method of a kind of brand-new phenethylamine；(2) institute of the present invention
The method stated can quickly detect the content of phenethylamine, and detection limit is low, and (embodiment data show that its detection is limited to 1.4 × 10- 8Mol/L), strong interference immunity, favorable reproducibility；(3) phenethylamine applying method of the present invention to measure in fish juice sample is accurate
Reliably.
Accompanying drawing explanation
Fig. 1 is the graph of relation between phenethylamine solution response current difference and phenethylamine concentration.
Fig. 2 is the difference between current comparison diagram of same concentrations tryptamines, phenethylamine.
Detailed description of the invention
The present invention is explained further below in conjunction with specific embodiment, but the present invention is not done any type of limit by embodiment
Fixed.
Unreceipted actual conditions person in embodiment, the condition advised according to normal condition or manufacturer is carried out.Wherein, used
Reagent or instrument unreceipted production firm person, be can by city available from conventional products.
The electrochemical determination method of embodiment 1 phenethylamine
S11. with gold colloidal modify gold electrode as working electrode, platinum electrode is auxiliary electrode, and Ag/AgCl electrode is reference
Electrode, builds three-electrode electro Chemical test system；
S12. three-electrode system is placed in alkaline solution, is scanned when initial potential is 0.10V with i-t curve method, treats
After baseline stability, add solution to be measured, then scan to stable, measure the difference between current that phenethylamine responds on electrode；
S13. the difference between current (-I, nA) responded on electrode according to phenethylamine is linear with phenethylamine concentration (c, μm ol/L)
Regression equation, calculates the content of phenethylamine；Described equation of linear regression is-I=7.783c+1.181(R=
0.997)；
The gold electrode that gold colloidal described in step S11 is modified is prepared by the method comprised the steps of:
S21. dissolve chitosan in and the acetic acid solution that volume fraction is 1.0% is made into shell that chitosan content is 2mg/mL gathers
Sugar acetic acid solution；
S22. in chitosan acetic acid solution, add the gold chloride (HAuCl of 10 mmol/L4) solution, stir 30min, chitosan
Acetic acid solution and gold chloride (HAuCl4) volume ratio of solution is 21；
The most under agitation it is added dropwise over the aqueous solution of 0.1mol/L sodium borohydride, until solution becomes transparent claret,
Obtain colloidal gold solution；
S24. depletion electrode, after polishing, cleaning, at the colloidal gold solution of gold electrode surfaces dropping dropping 3 μ L, be after drying
Obtain the gold electrode that gold colloidal is modified.
Embodiment 2 electrochemical property test
(1) standard curve is set up
Use the method described in embodiment 1, investigate phenethylamine current-responsive on the gold electrode that gold colloidal is modified in solution
Situation of change.As it is shown in figure 1, the difference between current that phenethylamine responds on electrode (-I, nA) and phenethylamine concentration (c, μm ol/L)
4.13 × 10-8~4.72×10-6In good linear relationship in the range of mol/L, its equation of linear regression is :-I=
7.783c+1.181(R=0.997), signal to noise ratios based on three times (S/N=3), obtain this modified gold electrode to phenethylamine
Detection is limited to 1.4 × 10-8mol/L。
(2) anti-interference test
According to the method described in embodiment 1, the tyramine of 10 times of phenethylamine concentration, histamine, spermine, spermidine, putrescine, corpse are investigated
Amine and the tryptamines disturbed condition to measuring phenethylamine.Result shows, in addition to tryptamines, and the survey to phenethylamine of the above other biological amine
Fixed all without substantially interfering with.
The interference analysis of tryptamines: with 2.49 × 10-7Mol/L, 5.8 × 10-7Mol/L, 1.23 × 10-6Mol/L phenethylamine is molten
Liquid is comparison, has investigated the same concentrations tryptamines disturbed condition to mensuration phenethylamine, and result is as shown in Figure 2.
Result shows, the current differential of same concentrations tryptamines is compared with phenethylamine, and phenethylamine is significantly greater, and tryptamines exists
Less interference, and tryptamines content in aquatic products and flavoring agent thereof is relatively fewer, so in follow-up sample test temporarily
Do not consider the impact of tryptamines.
(3) repeatability test
It is 1.66 × 10 by the method described in embodiment 1 to concentration-7mol/L、3.32×10-7The phenethylamine solution of mol/L is carried out
Measuring, parallel assay 6 times simultaneously, the current differential that 6 times measure is as shown in table 1.
Data from table are learnt, measuring concentration with modified electrode is 1.66 × 10-7Mol/L and 3.32 × 10-7mol/L
Relative standard deviation (RSD) during phenethylamine solution is respectively 4.7% and 4.0%.Result shows, the making of this modified electrode reappears
Property is good.
The mensuration of phenethylamine in embodiment 3 fish juice
Take the fish juice flavoring agent bought in supermarket in clean small beaker, burn in 50mL with 0.22 μm acetate fiber membrane filtration
In Bei, gained filtrate adds sodium chloride and makes solution saturated.Measure 10.00mL saturated solution in 50mL centrifuge tube, use
1.0mol/L NaOH solution regulation pH to 12, adds 5.0mL n-butyl alcohol-chloroform (1 1) mixed liquor, vortex oscillation
5min, is centrifuged 10min in 3600r/min, takes upper organic phase, and need to be repeated twice, merges twice solution.Mixed liquor is put
Steam near dry in 60 DEG C of water-baths, then dry up with nitrogen.Being eventually adding 1mL pH 12.7 NaOH solution makes residue dissolve, institute
Obtain solution solution the most to be measured.Then according to the method described in embodiment 1 measures phenethylamine content.
It is 1.85 × 10 that result records the concentration of phenethylamine in this fish juice test sample liquid-7Mol/L, draws this sample through conversion
In product, the content of phenethylamine is 1.11 × 10-5mol/L.For verifying the accuracy of the method, fish juice sample is carried out mark-on recovery
Experiment (table 2).Variable concentrations (1.66 × 10 in fish juice sample-7mol/L、3.31×10-7Mol/L) mark-on of phenethylamine reclaims
Rate is 90.0% ~ 110.8%, and its RSD is respectively 4.8% and 6.2%.Illustrate that the method is accurately and reliably.
Claims (10)
1. the electrochemical determination method of a phenethylamine, it is characterised in that use the gold electrode that gold colloidal is modified, at initial potential
During for 0.1V, i-t curve method is used to measure the content of phenethylamine.
The electrochemical determination method of phenethylamine the most according to claim 1, it is characterised in that specifically comprise the steps of:
S11. with gold colloidal modify gold electrode as working electrode, platinum electrode is auxiliary electrode, and Ag/AgCl electrode is reference
Electrode, builds three-electrode electro Chemical test system；
S12. three-electrode system is placed in alkaline solution, sweeps when initial potential is 0.08 ~ 0.12V with i-t curve method
Retouch, after baseline stability, add solution to be measured, then scan to stable, measure the difference between current that phenethylamine responds on electrode；
S13. the difference between current responded on electrode according to phenethylamine and the equation of linear regression of phenethylamine concentration, calculate benzene second
The content of amine.
The electrochemical determination method of phenethylamine the most according to claim 2, it is characterised in that the alkali described in step S12
Property solution be pH value be the NaOH solution of 12 ~ 13；Described initial potential is 0.08 ~ 0.10V.
The electrochemical determination method of phenethylamine the most according to claim 2, it is characterised in that the line described in step S13
Property regression equation is-I=7.783c+1.181.
The electrochemical determination method of phenethylamine the most according to claim 2, it is characterised in that the glue described in step S11
The gold electrode that body gold is modified is prepared by the method comprised the steps of:
S21. dissolving chitosan in and being made into chitosan content in the acetic acid solution that volume fraction is 0.5 ~ 2.0% is 1 ~ 3mg/mL
Chitosan acetic acid solution；
S22. in chitosan acetic acid solution, add the chlorauric acid solution of 5 ~ 15 mmol/L, stir 20 ~ 40min, chitosan second
The volume ratio of acid solution and chlorauric acid solution is 1.5 ~ 31；
The most under agitation it is added dropwise over the aqueous solution of 0.05 ~ 0.2mol/L sodium borohydride, until solution becomes transparent wine
Redness, obtains colloidal gold solution；
S24. depletion electrode, after polishing, cleaning, drips colloidal gold solution in gold electrode surfaces, the most i.e. obtains gold colloidal and repair
The gold electrode of decorations.
The electrochemical determination method of phenethylamine the most according to claim 5, it is characterised in that by chitosan in step S21
It is dissolved in the acetic acid solution that volume fraction is 1.0 ~ 2.0% and is made into the chitosan acetic acid solution that chitosan content is 2 ~ 3mg/mL.
The electrochemical determination method of phenethylamine the most according to claim 5, it is characterised in that at chitosan in step S22
Adding the chlorauric acid solution of 10 ~ 15 mmol/L in acetic acid solution, stir 20 ~ 30min, chitosan acetic acid solution and gold chloride are molten
The volume ratio of liquid is 1.5 ~ 21.
The electrochemical determination method of phenethylamine the most according to claim 5, it is characterised in that in step S23 under agitation
It is added dropwise over the aqueous solution of 0.1 ~ 0.2mol/L sodium borohydride.
The electrochemical determination method of phenethylamine the most according to claim 5, it is characterised in that at gold electrode in step S24
The colloidal gold solution of surface dropping 2 ~ 5 μ L.
The electrochemical determination method of phenethylamine the most according to claim 2, it is characterised in that be used for measuring benzene in fish juice
The content of ethamine, also comprises pre-treatment step in its testing procedure, described pre-treatment step is as follows:
Take fish juice sample, with membrane filtration, add sodium chloride and make solution saturated, measure 8 ~ 12mL saturated solution, use NaOH solution
Regulation pH to 12 ~ 13, adds n-butyl alcohol-chloroform mixed liquor that 4 ~ 6mL volume ratio is 11, shakes, is centrifuged, takes upper strata
Organic facies, repeats 2 ~ 5 times, merges organic facies, adds the NaOH solution dissolving that pH value is 12 ~ 13 after drying, obtains solution to be measured.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610612908.7A CN106198661A (en) | 2016-07-29 | 2016-07-29 | Electrochemical determination method of phenylethylamine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610612908.7A CN106198661A (en) | 2016-07-29 | 2016-07-29 | Electrochemical determination method of phenylethylamine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106198661A true CN106198661A (en) | 2016-12-07 |
Family
ID=57497373
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610612908.7A Pending CN106198661A (en) | 2016-07-29 | 2016-07-29 | Electrochemical determination method of phenylethylamine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106198661A (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050120668A (en) * | 2003-03-25 | 2005-12-22 | 플루오로테크닉스 피티와이 리미티드 | Method of enhancing fluorescence |
| EP1750126A1 (en) * | 2004-05-26 | 2007-02-07 | Ajinomoto Co., Inc. | Method and apparatus for analyzing aminofunctional compound |
| CN101458223A (en) * | 2008-12-26 | 2009-06-17 | 江南大学 | Preparation of quantitative rapid detecting sensor of microcapsule algae toxin and applications |
| CN101639457A (en) * | 2009-08-06 | 2010-02-03 | 武汉思达创新医药科技有限公司 | Application of screen printing electrode in the determination of 5-hydroxytryptamine |
| CN102213687A (en) * | 2010-04-09 | 2011-10-12 | 中国科学院海洋研究所 | Impedance sensor for detecting microbes quickly and construction method thereof |
| CN104020197A (en) * | 2014-06-09 | 2014-09-03 | 天津科技大学 | Ractopamine molecular-imprinting piezoelectric sensor and preparation method and application thereof |
| CN104880497A (en) * | 2015-06-12 | 2015-09-02 | 仲恺农业工程学院 | Chemically modified electrode for detecting cefalexin and electrochemical determination method of cefalexin |
-
2016
- 2016-07-29 CN CN201610612908.7A patent/CN106198661A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR20050120668A (en) * | 2003-03-25 | 2005-12-22 | 플루오로테크닉스 피티와이 리미티드 | Method of enhancing fluorescence |
| EP1750126A1 (en) * | 2004-05-26 | 2007-02-07 | Ajinomoto Co., Inc. | Method and apparatus for analyzing aminofunctional compound |
| CN101458223A (en) * | 2008-12-26 | 2009-06-17 | 江南大学 | Preparation of quantitative rapid detecting sensor of microcapsule algae toxin and applications |
| CN101639457A (en) * | 2009-08-06 | 2010-02-03 | 武汉思达创新医药科技有限公司 | Application of screen printing electrode in the determination of 5-hydroxytryptamine |
| CN102213687A (en) * | 2010-04-09 | 2011-10-12 | 中国科学院海洋研究所 | Impedance sensor for detecting microbes quickly and construction method thereof |
| CN104020197A (en) * | 2014-06-09 | 2014-09-03 | 天津科技大学 | Ractopamine molecular-imprinting piezoelectric sensor and preparation method and application thereof |
| CN104880497A (en) * | 2015-06-12 | 2015-09-02 | 仲恺农业工程学院 | Chemically modified electrode for detecting cefalexin and electrochemical determination method of cefalexin |
Non-Patent Citations (2)
| Title |
|---|
| 刘海峰等: "壳聚糖-胶体金修饰丝网印刷电极测定过氧化氢", 《上海交通大学学报（农业科学版）》 * |
| 金根娣等: "积分脉冲安培法测定苯乙胺", 《应用化学》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102288669A (en) | Electrochemical method based on graphene-modified electrode for simultaneous determination of rutin and quercetin | |
| CN103343126B (en) | Ractopamine hydrochloride aptamers and the aptamers electrochemica biological sensor detecting Ractopamine hydrochloride | |
| CN103424448A (en) | Method for detecting trace ochratoxin A (OTA) by adopting electrochemical aptamer sensor | |
| CN106290537B (en) | The method for detecting L-type Tryptophan concentration in solution | |
| CN108120761B (en) | Electrochemical biosensors based on peptidomimetics with electrocatalytic activity for acetylcholinesterase detection | |
| CN102788827A (en) | One-step preparation method for electro-deposition acetylcholinesterase biosensor | |
| CN102608188A (en) | Preparation method of current mode immunosensor used for detecting pesticide residue | |
| CN103115949B (en) | Preparation method of enzyme biosensor for detecting pesticide residues | |
| CN106248770A (en) | A kind of electrochemical method of quick detection fenifrothion pesticide residues | |
| CN105891309B (en) | The method for detecting L-type Tryptophan concentration in solution | |
| CN101858918B (en) | Method for detecting ractopamine in animal-derived food by microgap array electrode-based electrochemical immunosensor | |
| CN105223260B (en) | Electrochemical sensor of trace quick detection butyl p-hydroxybenzoate and preparation method thereof | |
| CN114910535A (en) | Method for high-sensitivity and rapid detection of alpha-hydroxy sanshool based on cell electrochemical taste sensor | |
| CN105403612A (en) | Method for rapidly detecting pesticide residue based on plant esterase | |
| CN107102052B (en) | Based on the uric acid electrochemical sensor containing active copper carbon dots and its application | |
| CN102608190A (en) | Preparation method of acetylcholinesterase sensor used for detecting pesticide residue | |
| CN105301077A (en) | Preparation method of aptamer sensor for detecting chlorpyrifos | |
| CN106093173A (en) | A kind of electrochemical sensor, preparation method and the application in quickly detection AFB1 thereof | |
| CN106198661A (en) | Electrochemical determination method of phenylethylamine | |
| CN102809598B (en) | Thermal polymerization preparation method for electrochemical sensor for rapidly detecting epigallocatechin-3-gallate (EGCG) | |
| CN105044172B (en) | A kind of preparation method of the biology sensor based on AChE enzyme directional at-tachments | |
| CN104109676B (en) | The electrochemica biological sensor of versicolorin aptamers and correlation | |
| CN108535344B (en) | A kind of biosensor and its construction method for Electrochemical Detection phosphorylation beta-amyloid protein | |
| CN107703296B (en) | Ultra-sensitive electrochemical immunosensor for multi-residue detection of sulfonamides | |
| CN110006970A (en) | Preparation method of electrochemical sensor for dopamine detection and products thereof and application |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20161207 |
|
| RJ01 | Rejection of invention patent application after publication |