CN103575795B - A kind of method detecting TYR content in beer sample - Google Patents
A kind of method detecting TYR content in beer sample Download PDFInfo
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- CN103575795B CN103575795B CN201310533339.3A CN201310533339A CN103575795B CN 103575795 B CN103575795 B CN 103575795B CN 201310533339 A CN201310533339 A CN 201310533339A CN 103575795 B CN103575795 B CN 103575795B
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Abstract
The invention discloses a kind of method detecting TYR content in beer sample.Adopt three-electrode system, at room temperature, respectively with 4,5-dichloro o-phenylenediamine nickel complex-graphene oxide modified glassy carbon electrode is working electrode, saturated calomel electrode is contrast electrode, and platinum electrode is auxiliary electrode, and in the PBS buffer solution of the TYR containing variable concentrations, (pH=7.0) carries out cyclic voltammetry scan, record variable concentrations TYR oxidation peak current value, result shows that TYR concentration is 1.0 × 10
-6~ 1.0 × 10
-3within the scope of mol/L, its concentration and oxidation peak current value have good linear relationship, drawing curve, and regression equation is Ip(A)=0.319C(mmol/L)+0.179, related coefficient is 0.995(n=5), detect and be limited to 2.3 × 10
-7mol/L(S/N=3); Utilize cyclic voltammetric method accordingly, TYR content can be measured.The present invention detects sensitive, quick.
Description
Technical field
The present invention relates to a kind of method utilizing chemically modified electrode to detect TYR content fast, particularly detect the method for TYR content in beer sample.
Background technology
TYR belongs to nonessential amino acid, is one of important amino acid in body needed for synthetic protein, exists at nature tyrosine with TYR.TYR, for promoting that the metabolism of human body has very important effect, also can produce neurotransmitter.Show according to the study, TYR has and prevents human senility, the effect of prevention dementia, and the accurate content measuring tyrosine in tissue and body fluid accurately is all significant in clinical medicine, nutrition.The current assay method to tyrosine mainly contains the methods such as Enzyme Catalytic Spectrophotometry, chromatography, chemoluminescence method, fluorometry, electrochemical methods according to the literature, and wherein electrochemical methods has the advantages such as advantage of lower cost, analytic process are comparatively simple, accuracy is high, quick.The development research of the sensitivity of electrochemical analysis method, preci-sion and accuracy and novel modified electrode is closely related, Schiff base transition metal complex is a kind of electron mediator of widespread use, there is the effect promoting electron transmission, the application of electron mediator improves sensitivity, the preci-sion and accuracy of electrochemical process detection, facilitates developing rapidly of Electroanalytical Chemistry.
Summary of the invention
The object of the present invention is to provide a kind of method detecting TYR content in beer sample.
Detect the research method of TYR content: adopt three-electrode system, at room temperature, be working electrode respectively with glass-carbon electrode, saturated calomel electrode is contrast electrode, platinum electrode is auxiliary electrode, all measurements all in the PBS buffer solution of the TYR containing variable concentrations (pH=7.0) carry out, adopt cyclic voltammetry scanning, sweep velocity 0.1V/s, sweep limit is+0.2V ~+1.4V.
Interference experiment result shows, measure relative error be no more than ± 5% time, 10 times of arginine, DL-Alanine, L-glutamic acid, Serine, glycocoll; 100 times of magnesium nitrates, aluminium nitrate, copper nitrate, barium nitrates; 50 times of ferric nitrates do not disturb the test of TYR concentration.
Concrete steps are:
1. get 10 mg nano graphene oxides and 0.05mmol (37.78mg) 4,5-dichloro o-phenylenediamine contracting 3,5-Dibromosalicylaldehyde Schiff base nickel complex is dissolved in dimethyl formamide (DMF) solution, and ultrasonic disperse obtains homogeneous Schiff base nickel complex-nano graphene oxide suspending liquid for 2 hours.
2. glass-carbon electrode is being placed with Al successively
2o
3polishing on the chamois leather of powder, after intermediate water drip washing, distinguishes ultrasonic cleaning 3 minutes, infrared drying successively in absolute ethyl alcohol, intermediate water; Glass-carbon electrode drips 3,5-Dibromosalicylaldehyde Schiff base nickel complex-nano graphene oxide suspending liquid, and infrared lamp is dried, and obtains 4,5-dichloro o-phenylenediamine nickel complex-graphene oxide modified glassy carbon electrode, is placed in 4 DEG C of refrigerators and preserves stand-by.
3. adopt three-electrode system, at room temperature, respectively with step (2) gained 4,5-dichloro o-phenylenediamine nickel complex-graphene oxide modified glassy carbon electrode is working electrode, saturated calomel electrode is contrast electrode, and platinum electrode is auxiliary electrode, and in the PBS buffer solution of the TYR containing variable concentrations, (pH=7.0) carry out cyclic voltammetry scan, record variable concentrations TYR oxidation peak current value, result shows that TYR concentration is 1.0 × 10
-6~ 1.0 × 10
-3within the scope of mol/L, its concentration and oxidation peak current value have good linear relationship, drawing curve, and equation of linear regression is
ip=0.319C+0.179,
ithe unit of p is A and ampere, and the unit of C is mmol/L, and related coefficient is 0.995(n=5), detect and be limited to 2.3 × 10
-7mol/L(S/N=3), wherein n is that sample parallel measures number of times, and S is relative standard deviation, and N is the slope of linear equation.
4. accurately measure beer 5.00mL respectively, 50mL is settled to pH=7.0 PBS buffer solution, measure the oxidation peak current value of 50mL solution with step (2) gained 4,5-dichloro o-phenylenediamine nickel complex-graphene oxide modified glassy carbon electrode, substitute into equation of linear regression
ip=0.319C+ 0.179,
ithe unit of p is A and ampere, and the unit of C is mmol/L, calculates the content of TYR in the concentration of TYR and beer sample.
The present invention is with 4,5-dichloro o-phenylenediamine Schiff base nickel complex-nano graphene oxide is electrode modification agent, prepare modified glassy carbon electrode, have studied the electrochemical properties of TYR on modified electrode and assay method, and be applied to the content of the TYR detected in beer sample, detect sensitive, quick.
Accompanying drawing explanation
Fig. 1 is the working curve diagram of embodiments of the invention.
Embodiment
Embodiment:
1. get 10 mg nano graphene oxides and 0.05mmol (37.78mg) 4,5-dichloro o-phenylenediamine contracting 3,5-Dibromosalicylaldehyde Schiff base nickel complex is dissolved in dimethyl formamide (DMF) solution, ultrasonic disperse obtains 3,5-homogeneous Dibromosalicylaldehyde Schiff base nickel complex-nano graphene oxide suspending liquid for 2 hours.
2. glass-carbon electrode is being placed with Al successively
2o
3polishing on the chamois leather of powder, after intermediate water drip washing, distinguishes ultrasonic cleaning 3 minutes, infrared drying successively in absolute ethyl alcohol, intermediate water; Glass-carbon electrode drips 3 of step (1) gained, 5-Dibromosalicylaldehyde Schiff base nickel complex-nano graphene oxide suspending liquid, infrared lamp is dried, and obtains 4,5-dichloro o-phenylenediamine nickel complex-graphene oxide modified glassy carbon electrode, is placed in 4 DEG C of refrigerators and preserves stand-by.
3. adopt three-electrode system, at room temperature, respectively with 4 of step (2) gained, 5-dichloro o-phenylenediamine nickel complex-graphene oxide modified glassy carbon electrode is working electrode, saturated calomel electrode is contrast electrode, and platinum electrode is auxiliary electrode, and in the PBS buffer solution of the TYR containing variable concentrations, (pH=7.0) carry out cyclic voltammetry scan, record variable concentrations TYR oxidation peak current value, result shows that TYR concentration is 1.0 × 10
-6~ 1.0 × 10
-3within the scope of mol/L, its concentration and oxidation peak current value have good linear relationship, and drawing curve (see figure 1), regression equation is
ip=0.319C+ 0.179,
ithe unit of p is A and ampere, and the unit of C is mmol/L, and related coefficient is 0.995(n=5), detect and be limited to 2.3 × 10
-7mol/L(S/N=3), n is that sample parallel measures number of times, and S is relative standard deviation, and N is the slope of linear equation.
4. select three kinds of beer to carry out sample analysis.Accurately measure beer 5.00mL respectively, 50mL is settled to pH=7.0 PBS buffer solution, measure the oxidation peak current value of 50mL solution with 4, the 5-dichloro o-phenylenediamine nickel complexes-graphene oxide modified glassy carbon electrode of step (2) gained, substitute into equation of linear regression
ip=0.319C+ 0.179,
ithe unit of p is A and ampere, and the unit of C is mmol/L, calculates the content of TYR in the concentration of TYR and beer sample.In 50mL sample solution, add standard TYR solution, carry out recovery testu, the results are shown in Table 1.Relative standard deviation RSD is at 1.26%-4.02%, and recovery of standard addition, between 96.00% ~ 102.50%, shows that the preci-sion and accuracy of this method is better.
The test result of TYR content in table 1 beer
Claims (1)
1. detect a method for TYR content in beer sample, it is characterized in that concrete steps are:
(1) 10 mg nano graphene oxide and 0.05mmol and 37.78mg4 are got, 5-dichloro o-phenylenediamine contracting 3,5-Dibromosalicylaldehyde Schiff base nickel complex is dissolved in dimethyl formamide solution, ultrasonic disperse obtains 4 in 2 hours, 5-dichloro o-phenylenediamine contracting 3,5-Dibromosalicylaldehyde Schiff base nickel complex-nano graphene oxide suspending liquid;
(2) glass-carbon electrode is being placed with Al successively
2o
3polishing on the chamois leather of powder, after intermediate water drip washing, distinguishes ultrasonic cleaning 3 minutes, infrared drying successively in absolute ethyl alcohol, intermediate water; 4 of step (1) gained are dripped again on glass-carbon electrode, 5-dichloro o-phenylenediamine contracting 3,5-Dibromosalicylaldehyde Schiff base nickel complex-nano graphene oxide suspending liquid, infrared lamp is dried, obtain 4,5-dichloro o-phenylenediamine contracting 3,5-Dibromosalicylaldehyde Schiff base nickel complex-graphene oxide modified glassy carbon electrode, is placed in 4 DEG C of refrigerators and preserves stand-by;
(3) three-electrode system is adopted, at room temperature, respectively with step (2) gained 4,5-dichloro o-phenylenediamine contracting 3,5-Dibromosalicylaldehyde Schiff base nickel complex-graphene oxide modified glassy carbon electrode is working electrode, saturated calomel electrode is contrast electrode, platinum electrode is auxiliary electrode, cyclic voltammetry scan is carried out in the PBS buffer solution of the TYR in pH=7.0 containing variable concentrations, record variable concentrations TYR oxidation peak current value, result shows that TYR concentration is 1.0 × 10
-6~ 1.0 × 10
-3within the scope of mol/L, its concentration and oxidation peak current value have good linear relationship, drawing curve, and equation of linear regression is
ip=0.319C+0.179,
ithe unit of p is A and ampere, and the unit of C is mmol/L, and related coefficient is 0.995, n=5, detects and is limited to 2.3 × 10
-7mol/L, S/N=3, wherein n is that sample parallel measures number of times, and S is relative standard deviation, and N is the slope of linear equation;
(4) beer 5.00mL is accurately measured respectively, 50mL is settled to pH=7.0 PBS buffer solution, measure the oxidation peak current value of 50mL solution with step (2) gained 4,5-dichloro o-phenylenediamine nickel complex-graphene oxide modified glassy carbon electrode, substitute into equation of linear regression
ip=0.319C+ 0.179,
ithe unit of p is A and ampere, and the unit of C is mmol/L, calculates the content of TYR in the concentration of TYR and beer sample.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106990155A (en) * | 2017-06-07 | 2017-07-28 | 广西师范学院 | The method for detecting tyrosine concentration in solution |
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| CN106990155B (en) * | 2017-06-07 | 2019-06-07 | 广西师范学院 | The method for detecting tyrosine concentration in solution |
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Effective date of registration: 20211221 Address after: 271000 Han Ming Tang Road, Eastern New Area, Taishan District, Tai'an City, Shandong Province Patentee after: SHANDONG TAISHAN BEER CO.,LTD. Address before: 541004 the Guangxi Zhuang Autonomous Region Guilin Construction Road No. 12 Patentee before: GUILIN University OF TECHNOLOGY |
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Address after: No. 99, Keji North Street, Mount Taishan District, Tai'an, Shandong 271000 Patentee after: Mount Taishan Beer Co.,Ltd. Address before: 271000 Han Ming Tang Road, Eastern New Area, Taishan District, Tai'an City, Shandong Province Patentee before: SHANDONG TAISHAN BEER CO.,LTD. |