CN104020159A - Method for detecting tetracarboxyl phenyl porphyrin - Google Patents
Method for detecting tetracarboxyl phenyl porphyrin Download PDFInfo
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- CN104020159A CN104020159A CN201410188007.0A CN201410188007A CN104020159A CN 104020159 A CN104020159 A CN 104020159A CN 201410188007 A CN201410188007 A CN 201410188007A CN 104020159 A CN104020159 A CN 104020159A
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- phenyl porphyrin
- electrochemiluminescence
- porphyrin
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Abstract
The invention discloses a method for detecting tetracarboxyl phenyl porphyrin. The method comprises the following steps: adding K2S2O8 as a co-reagent into liquid to be detected, and then carrying out electrochemical luminescence scanning on the liquid to be detected. tetracarboxyl phenyl porphyrin can generate a stable and strong electrochemical luminescence signal under the action of the co-reagent K2S2O8. The tetracarboxyl phenyl porphyrin has a good linear relation in the range of concentration of 2.0*10<-7> mol.L<-1> to 1.0*10<-5> mol.L<-1>, and the detection limit is 7.0*10<-8> mol.L<-1>.
Description
Technical field
The invention belongs to compound test field, be specifically related to a kind of method that detects tetracarboxylic phenyl porphyrin.
Background technology
Porphyrin and metal complex thereof are extensively present in occurring in nature, and as the iron porphyrin in myoglobins, haemoglobin, the magnesium porphyrin in chlorophyll, the cobalt porphyrin in cobalamin etc., they and vital movement are closely related, are called as " pigment of life ".Therefore, to the detection of porphyrin compound in biosome for porpharia and the diagnosis of other porphyrin associated conditions, the monitoring of environmental pollution etc. have great importance, the problem that the person that is also chemical research shows great attention to all the time.Tetracarboxylic phenyl porphyrin is one of important water-soluble porphyrin compound, at aspects such as analytical chemistry, molecular recognition, exploration photosynthesis mechanism, raising photosynthetic efficiencies, has important application, has caused people's concern.The detection method of the porphyrin compound of bibliographical information mainly contains at present: spectrophotometric method, fluorescence method, high performance liquid chromatography, mass spectroscopy, chromatograph-mass spectrometer coupling method, the methods such as capillary electrophoresis separation-fluorescence detection, thin-layered chromatography, the narrow collimation method of fluorescence and magnetic circular dichroism (mcd) method, but these methods are all fast and convenient not, and the operation and maintenance more complicated of instrument system, the expense of test is also higher, can not get penetration and promotion.Therefore, develop fast and convenient, expense is lower, and sensitive porphyrin detection method is extremely important.
Summary of the invention
The object of the invention is to overcome the problem that existing detection tetracarboxylic phenyl porphyrin exists, a kind of method of quick, cheap detection tetracarboxylic phenyl porphyrin is provided.
It is as follows that the present invention realizes the technical scheme that above-mentioned purpose adopts:
Detect a method for tetracarboxylic phenyl porphyrin, comprise the steps: to add the K as coreagent in liquid to be detected
2s
2o
8, then liquid to be detected is carried out to electrochemiluminescence scanning.
Further, K in liquid to be detected
2s
2o
8concentration be 1-50mmol/L, be preferably 20-30mmol/L.
The present invention finds that tetracarboxylic phenyl porphyrin (TCPP) is at coreagent K
2s
2o
8effect under, can produce stable and strong electrochemical luminescence signals, utilize this electrochemiluminescence character of TCPP can detect TCPP itself, or using TCPP as electrochemiluminescence reagent, be used for detecting some to the influential material of the luminous intensity of TCPP, as amine substance.
As tetracarboxylic phenyl porphyrin quantitatively detects: electrochemiluminescence scanning obtains luminous intensity, then by the typical curve of luminous intensity and tetracarboxylic phenyl porphyrin concentration, can draw the concentration of tetracarboxylic phenyl porphyrin in corresponding liquid to be detected.In tetracarboxylic phenyl porphyrin concentration, be 2.0 * 10
7molL
-1～1.0 * 10
5molL
-1in scope, there is good linear relationship, detect and be limited to 7.0 * 10
8molL
-1.
Accompanying drawing explanation
Fig. 1 is the electrochemiluminescence figure under different operating electrode.
Fig. 2 is the electrochemiluminescence figure under different coreagents.
Fig. 3 is different K
2s
2o
8electrochemiluminescence figure under concentration.
Fig. 4 is the electrochemiluminescence figure under different pH values.
Fig. 5 is the electrochemiluminescence figure under different TCPP concentration.
Embodiment
In order to be illustrated more clearly in content of the present invention, below in conjunction with accompanying drawing and specific embodiment, the present invention is further described again.
The present invention adds coreagent K in sample liquid
2s
2o
8thereby, make tetracarboxylic phenyl porphyrin (full name: 5,10,15,20-tetra-(4-carboxyl phenyl) porphyrin, abbreviation: TCPP, No. CAS: 14609-54-2) produce strong electrochemical luminescence signals, and this luminous signal has good stability and reappearance.
Electrochemiluminescence test of the present invention is to carry out on MPI-A type Capillary Zone Electrophoresis with Electrochemical luminescence analyzer (Xi'an Rui Mai high tech electron company limited).
Electrochemiluminescence scanning adopts traditional three-electrode system while detecting, and usings glass-carbon electrode or gold electrode as working electrode, the saturated KCl of platinum filament and Ag/AgCl() electrode is respectively as to electrode and contrast electrode.Current potential all be take the saturated KCl of Ag/AgCl() electrode is reference value.
Adopt the pH of Sai Duolisi Sartorius basic pH meter PB-10 acidometer (Shanghai people and scientific instrument company limited) working sample liquid.
The automatic dual pure water distiller of quartz ampoule heated type (1810B, Asian-Pacific Glass-Tech. Co., Shanghai City) is for the preparation of redistilled water.
Detecting step is as follows:
1) with alundum (Al2O3) polishing powder (0.30 μ m, 0.05 μ m, Shanghai Chen Hua instrument reagent company), successively glass-carbon electrode, gold electrode are carried out to polishing, then use ethanol, the redistilled water ultrasonic cleaning of 95v%, nitrogen dries up, standby.
2) with liquid-transfering gun, pipette 100 μ L containing the solution of TCPP, join in the centrifuge tube of 1.5 mL, then move into 0.1 molL that 700 μ L pH are 7
-1pBS buffer solution, shakes up, then moves into 200 μ L K in solution
2s
2o
8solution, mixes, and obtains sample liquid.
3) pipette the above-mentioned sample liquid of 400 μ L in sample cell, with MPI-A type Capillary Zone Electrophoresis with Electrochemical luminescence analyzer, at-0.2V, between-1.5V, with cyclic voltammetry, carry out electrochemiluminescence scanning.
4) while quantitatively detecting, the TCPP solution repeating step 2 of available series normal concentration) and 3), first draw the typical curve of concentration-luminous intensity (getting peak value), then measure the electrochemiluminescence intensity (getting peak value) of liquid to be detected, by typical curve, draw the concentration of TCPP in liquid to be detected.
In sample liquid, TCPP concentration is 4 * 10
5molL
-1, K
2s
2o
8concentration is 0.02 molL
-1, during pH=7, working electrode is respectively the electrochemiluminescence figure of gold electrode (a), glass-carbon electrode (b), as shown in Figure 1, visible, adopts glass-carbon electrode as working electrode better effects if.
K in sample liquid
2s
2o
8use H
2o
2or water (not adding coreagent) is when substitute, and take glass-carbon electrode as working electrode, as shown in Figure 2, the TCPP concentration of sample liquid is 4 * 10 to electrochemiluminescence scanning result
5molL
-1, pH is 7, wherein, a is for containing 0.02 molL
-1k
2s
2o
8, b is for containing 0.02 molL
-1h
2o
2, c is not for containing coreagent.Can find out, not add K
2s
2o
8, or that add is H
2o
2, all there is no electrochemical luminescence signals, only add K
2s
2o
8just produced strong, stable luminous signal.
In sample liquid, TCPP concentration is 4 * 10
5molL
-1, pH is 7 o'clock, take glass-carbon electrode as working electrode, K
2s
2o
8concentration is by 1 * 10
3molL
-1be adjusted to 5 * 10
-2molL
-1electrochemiluminescence figure, as shown in Figure 3, wherein, the point in figure is distinguished corresponding K from left to right
2s
2o
8concentration be 1 * 10
3molL
-1, 5 * 10
3molL
-1, 1 * 10
-2molL
-1, 2 * 10
-2molL
-1, 3 * 10
-2molL
-1, 4 * 10
-2molL
-1, 5 * 10
-2molL
-1.Can find out K
2s
2o
8concentration rises to 3 * 10
-2molL
-1after, electrochemiluminescence intensity tends towards stability.
In sample liquid TCPP concentration, be 4 * 10
5molL
-1, K
2s
2o
8concentration is 0.02 molL
-1time, take glass-carbon electrode as working electrode, by sample pH value by 6 be adjusted to 11 o'clock electrochemiluminescence figure as shown in Figure 4, wherein, a is pH=6.0, b is pH=7.4, c is pH=8.1, d is pH=9.4, e is pH=10.7, f is pH=11.0.Can find out, when pH=6-11, all can acquire stable, strong electrochemiluminescence intensity, show, at coreagent K
2s
2o
8effect under, the electrochemiluminescence of TCPP may be irrelevant with proton.
Fig. 5 is that TCPP normal concentration is by 2.0 * 10
7molL
-1be changed to 1.0 * 10
5molL
-1electrochemiluminescence figure, wherein, K
2s
2o
8concentration is 0.02 molL
-1, pH is 7, working electrode is glass-carbon electrode, illustration is the typical curve of corresponding luminous intensity and TCPP concentration, I=371.88c-49.24, R
2=0.996, in TCPP concentration, be 2.0 * 10 as seen
7molL
-1～1.0 * 10
5molL
-1, luminous intensity and concentration have good linear relationship, detect and are limited to 7.0 * 10
8molL
-1.
Claims (4)
1. detect a method for tetracarboxylic phenyl porphyrin, comprise the steps: to add the K as coreagent in liquid to be detected
2s
2o
8, then liquid to be detected is carried out to electrochemiluminescence scanning.
2. detect according to claim 1 the method for tetracarboxylic phenyl porphyrin, it is characterized in that, K in liquid to be detected
2s
2o
8concentration be 1-50mmol/L.
3. detect according to claim 2 the method for tetracarboxylic phenyl porphyrin, it is characterized in that, K in liquid to be detected
2s
2o
8concentration be 20-30mmol/L.
4. tetracarboxylic phenyl porphyrin application in electrochemiluminescence detects as electrochemiluminescence reagent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950219A (en) * | 2017-04-21 | 2017-07-14 | 西北师范大学 | A kind of ECL new systems are to Fe3+Detection method |
| CN111239110A (en) * | 2020-02-10 | 2020-06-05 | 西北师范大学 | Construction method of porphyrin derivative with aggregation-induced emission performance applied to electrochemiluminescence system |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106950219A (en) * | 2017-04-21 | 2017-07-14 | 西北师范大学 | A kind of ECL new systems are to Fe3+Detection method |
| CN106950219B (en) * | 2017-04-21 | 2019-10-15 | 西北师范大学 | A kind of ECL new system is to Fe3+Detection method |
| CN111239110A (en) * | 2020-02-10 | 2020-06-05 | 西北师范大学 | Construction method of porphyrin derivative with aggregation-induced emission performance applied to electrochemiluminescence system |
| CN111239110B (en) * | 2020-02-10 | 2022-07-22 | 西北师范大学 | Construction method of porphyrin derivative with aggregation-induced emission performance applied to electrochemiluminescence system |
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