CN105738330B - A kind of method of content using CdTe quantum detection phenolethanolamine A - Google Patents
A kind of method of content using CdTe quantum detection phenolethanolamine A Download PDFInfo
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Abstract
The present invention relates to a kind of method of the content using CdTe quantum detection phenolethanolamine A.This method is using mercaptopropionic acid as stabilizer, and the CdTe quantum prepared by the use of microwave radiation heating means is as fluorescence probe, the fluorescence intensity enhancement effect based on phenolethanolamine A to CdTe quantum, so as to establish a kind of method for the content for measuring phenolethanolamine A.CdTe quantum is uniformly mixed by this method with test substance phenolethanolamine A in phosphate buffer, stands 15min, the fluorescence intensity of system is detected using molecular fluorescence photometer, you can realizes the trace detection to phenolethanolamine A；Its detection sensitivity is high, and easy to operate, detection time is short, and analysis cost is low, and detection limit is relatively low, and recovery of standard addition is higher.
Description
Technical field
The invention belongs to analytical chemistry field, and in particular to a kind of content using CdTe quantum detection phenolethanolamine A
Method.
Background technology
Phenolethanolamine A belongs to beta-receptor activator, the nutritional ingredient in animal body can be made to be shifted from fat to muscle, performance
Go out repartitioning function effect, and then regulate and control the metabolism of animal body, strengthen lipolysis, promote protein synthesis, significantly carry
High carcass lean meat percentage and the price of deed.But beta-receptor activator easily accumulates residual in animal tissue, particularly internal organ, its
The symptoms such as muscular tremor, arrhythmia cordis, headache can be triggered by being entered by food chain after human body, and severe patient may threat to life.Mirror
In above reason, the beta-receptor activators such as phenolethanolamine A, Clenbuterol, phenolethanolamine A amine were classified as taboo by China in 1997
The medicine only used in feed and cultivation domestic animal drinking water.But still there is culturist by its illegal use in animal husbandry at present
In, trigger medicament residue, so as to cause serious harm to consumer health.
Chinese patent literature CN104792762A discloses a kind of side that salbutamol is quantitatively detected using CdTe quantum
Method, is mixed with test substance salbutamol by the CdTe quantum of the thioacetic acid by surface modification in phosphate buffer
After closing uniformly, the fluorescence intensity of system is detected using molecular fluorescence photometer, you can realize and the trace of salbutamol is examined
Survey.However, due to salbutamol and the difference of phenolethanolamine A structures, the above method different from the mechanism of CdTe quantum effect
It can not be used for the content for detecting phenolethanolamine A.
Therefore, a kind of method of the content using CdTe quantum detection phenolethanolamine A is studied to be of great significance.
The content of the invention
For this reason, the present invention proposes a kind of method of the content using CdTe quantum detection phenolethanolamine A.
In order to solve the above technical problems, the present invention is achieved through the following technical solutions：
The present invention provides a kind of preparation method of the CdTe quantum for phenolethanolamine A detections, includes the following steps：
(1) 0.12-0.13g telluriums powder and 0.11-0.13g sodium borohydrides are weighed respectively, and adds 1-4mL high purity waters, in ice
Reaction 4h is stirred under water bath condition, obtains NaHTe solution；
(2) 0.060-0.080gCdCl is weighed2·2.5H2O is dissolved in 180-200mL high purity waters, adds 80-100 μ L mercaptos
Base propionic acid, obtains suspension；
(3) it is 10-12 with the pH of the 0.1mol/LNaOH solution adjusting suspension, under nitrogen protection, adds 200-
NaHTe solution described in 500 μ L, controls Cd2+、HTe-, mercaptopropionic acid molar ratio be 0.8~1.0:0.6~0.8:2.5~3.0,
Obtain CdTe quantum precursor solution；
(4) the CdTe quantum precursor solution is transferred in microwave dissolver, 100-160 DEG C of heating 5-20min,
Through cooling down, washing, centrifuging, up to the CdTe quantum.
The present invention also provides the CdTe quantum that above-mentioned preparation method is prepared in the content detection of phenolethanolamine A
Using.
The present invention also provides a kind of method of the content using CdTe quantum detection phenolethanolamine A, the CdTe quantum
Point is the CdTe quantum being prepared using above-mentioned preparation method, is included the following steps：
(a) fluorescence sensitivity standard curve is made：
A series of phenolethanolamine A standard solution of various concentrations is prepared, and it is moved in the colorimetric cylinder of 5mL respectively, to
1.0mL concentration is added in each colorimetric cylinder as 7.25 × 10-4The CdTe solution of mol/L, is delayed with the phosphate of pH=7.4
Solution constant volume is rushed, after shaking up, room temperature places 15min, and the fluorescence intensity F of above-mentioned each system is detected with molecular fluorescence photometer；
Meanwhile the CdTe solution for taking 1.0mL concentration to be 7.25 × 10-4mol/L is added in the colorimetric cylinder of 5mL, with the phosphorus of pH=7.4
Hydrochlorate buffer solution constant volume, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection architecture0；
Using phenolethanolamine A concentration as abscissa, with F/F0For ordinate, obtain phenolethanolamine A and CdTe quantum fluorescence is increased
Quick equation of linear regression；
(b) 1.0mL7.25 × 10 are taken respectively-4The CdTe solution of mol/L and the sample liquid of the A containing phenolethanolamine are added to 5mL
Colorimetric cylinder in, with the phosphate buffer solution constant volume of pH=7.4, shaking up makes it fully react, room temperature place 15min, with point
Sub- fluophotometer detects to obtain the fluorescence intensity of system, with the phenolethanolamine A to the linear of CdTe quantum fluorescence sensitivity
Regression equation compares, up to the content of phenolethanolamine A in the sample liquid.
Preferably, in the method for the above-mentioned content using CdTe quantum detection phenolethanolamine A of the present invention, the step
(a) and in the step (b), the testing conditions of the fluorescence intensity are：Excitation wavelength is 365nm, and excitation and transmite slit are wide
Degree is 5nm.
It is further preferred that in the method for the above-mentioned content using CdTe quantum detection phenolethanolamine A of the present invention, it is described
The concentration of phenolethanolamine A standard solution is respectively 8 μ g/L, 16 μ g/L, 32 μ g/L, 40 μ g/L, 60 μ g/L, 80 μ g/L and 120 μ g/
L。
It is further preferred that in the method for the above-mentioned content using CdTe quantum detection phenolethanolamine A of the present invention, work as institute
When the concentration range for stating phenolethanolamine A standard solution is 8 μ g/L-120 μ g/L, the phenolethanolamine A is to CdTe quantum fluorescence
The equation of linear regression F/F of enhanced sensitivity0=0.0019C+1.0321, linearly dependent coefficient 0.996.
It is further preferred that in the method for the above-mentioned content using CdTe quantum detection phenolethanolamine A of the present invention, it is described
The sample liquid of the A containing phenolethanolamine is urinated for pig.
It is further preferred that in the method for the above-mentioned content using CdTe quantum detection phenolethanolamine A of the present invention, it is described
Pig urine is by following pretreatment：
Take pig urine samples liquid, it is 7.0 to adjust pH with NaOH solution, filters and will collect filtrate, to obtain the final product.
The above technical solution of the present invention has the following advantages over the prior art：
(1) method of the content of the present invention using CdTe quantum detection phenolethanolamine A, by by surface modification mercapto
The CdTe quantum of base propionic acid, is uniformly mixed with test substance phenolethanolamine A in phosphate buffer, and room temperature is placed
15min, detects the fluorescence intensity of system using molecular fluorescence photometer, you can realize the trace detection to phenolethanolamine A, this
It is due to that the CdTe quantum surface of preparation has carboxyl, by covalent coupling, chains phenolethanolamine A so that CdTe
The surface defect of quantum dot reduces, and closely fluorescence intensity enhancing, using the change of CdTe quantum fluorescence intensity, is realized to benzene second
The quantitative detection of hydramine A；The results show that phenolethanolamine A is in the range of 8-120 μ g/L, the concentration of phenolethanolamine A and system
Fluorescence intensity F/F0Good linear relationship is presented, linearly dependent coefficient 0.996, illustrates phenolethanolamine A to CdTe quantum
Fluorescence sensitivity there is higher sensitivity and the wider range of linearity；
(2) method of the content of the present invention using CdTe quantum detection phenolethanolamine A, detection sensitivity is high, behaviour
Make simplicity, detection time is short, and analysis cost is low, and detection limit is relatively low, and recovery of standard addition is higher；
(3) method of the content of the present invention using CdTe quantum detection phenolethanolamine A, carries out pig urine pre-
Processing, effectively to remove the interference of metal ion in pig urine samples.
Brief description of the drawings
In order to make the content of the present invention more clearly understood, the specific embodiment below according to the present invention and combination
Attached drawing, the present invention is described in further detail, wherein：
Fig. 1 is the TEM figures of CdTe quantum prepared by the embodiment of the present invention 1；
Fig. 2 is fluorescence photo of the CdTe quantum of the preparation of the embodiment of the present invention 1 in the case where UV illumination is penetrated；
Fig. 3 is the fluorescence spectra of CdTe quantum prepared by the embodiment of the present invention 1；
Fig. 4 is that spectrum change is quenched to various concentrations phenolethanolamine A in CdTe quantum prepared by the embodiment of the present invention 1
Figure；
Equations of linear regression of the Fig. 5 for phenolethanolamine A in experimental example 1 of the present invention to CdTe quantum fluorescence sensitivity.
Embodiment
Technical scheme is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's all other embodiments obtained without making creative work, belong to the scope of protection of the invention.
In following embodiments of the present invention and experimental example, molecular fluorescence photometer (model：F7000, is provided by Hitachi, Ltd)；
Phenolethanolamine A standard items are purchased from sigma.
Embodiment 1
A kind of preparation method of CdTe quantum of the present embodiment, includes the following steps：
(1) 0.1276g telluriums powder and 0.1100g sodium borohydrides are weighed respectively, and adds 1mL high purity waters, use sealed membrane rapidly
Sealing is sealed, while is inserted into injection needle and is communicated with the external world, reaction 4h is stirred under the conditions of ice-water bath, 10min is stood, obtains
NaHTe solution；
Reaction equation is as follows：
4NaBH4+2Te+7H2O=2NaHTe+Na2B4O7+14H2↑
(2) 0.07gCdCl is weighed2·2.5H2O is dissolved in 190mL high purity waters, adds 80 μ L mercaptopropionic acids, is formed suspended
Liquid system；
(3) pH for first using the 0.1mol/LNaOH solution adjusting suspended liquid system is 11, leads to high pure nitrogen 30min,
Under nitrogen protection, NaHTe solution described in 200 μ L is added, controls Cd in solution2+、HTe-, mercaptopropionic acid molar ratio be 1.0:
1.0:3.0, obtain CdTe quantum presoma；
(4) the CdTe quantum presoma is transferred in microwave dissolver, power setting 800w, 100 DEG C of heating
10min, through cooling down, washing, centrifuging, up to the CdTe quantum.
A kind of method of content using CdTe quantum detection phenolethanolamine A of the present embodiment, detection sample is without benzene
The negative pig urine samples liquid (being used to detect as blind sample) of monoethanolamine A, includes the following steps：
(a) fluorescence sensitivity standard curve is made：
A series of phenolethanolamine A standard solution of various concentrations is prepared, and it is moved in the colorimetric cylinder of 5mL respectively, to
1.0mL concentration is added in each colorimetric cylinder as 7.25 × 10-4The CdTe solution of mol/L, is delayed with the phosphate of pH=7.4
Solution constant volume is rushed, after shaking up, room temperature places 15min, and the fluorescence intensity F of above-mentioned each system is detected with molecular fluorescence photometer；
Meanwhile it is 7.25 × 10 to take 1.0mL concentration-4The CdTe solution of mol/L is added in the colorimetric cylinder of 5mL, with the phosphoric acid of pH=7.4
Salt buffer solution constant volume, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection architecture0；
Using phenolethanolamine A concentration as abscissa, with F/F0For ordinate, obtain phenolethanolamine A and CdTe quantum fluorescence is increased
Quick equation of linear regression；
(b) pig urine samples liquid is taken, it is 7.0 to adjust pH with NaOH solution, filters and will collect filtrate, up to sample to be tested
Liquid；
Respectively to CdTe quantum solution described in 1.0mL, the analyte sample fluid is added in the colorimetric cylinder of 5mL, is used
The phosphate buffer solution constant volume of pH=7.4, shakes up and stands 15min, it is detected after fully reacting with molecular fluorescence photometer
The fluorescence intensity F for obtaining system is 998.0, and testing conditions are：Excitation wavelength is 365nm, and excitation and transmite slit width are
5nm, sweep speed 1200nm/min；
The equation of linear regression of CdTe quantum fluorescence sensitivity is compareed with the phenolethanolamine A, you can draw described the moon
Property pig urine samples liquid in be free of the content of phenolethanolamine A, testing result in the negative pig urine samples liquid with being free of phenolethanolamine A
The fact it is consistent.
The TEM figures of CdTe quantum manufactured in the present embodiment are as shown in Figure 1.As shown in Figure 1, the pattern of CdTe quantum is
It is spherical, good dispersion, particle diameter 4.5nm and distribution it is homogeneous.
Fluorescence photo of the CdTe quantum manufactured in the present embodiment in the case where UV illumination is penetrated is as shown in Figure 2.Can by Fig. 2
Know, CdTe quantum sends the fluorescence of Chinese red in the case where UV illumination is penetrated.
The fluorescence spectra of CdTe quantum manufactured in the present embodiment is as shown in Figure 3.From the figure 3, it may be seen that CdTe quantum
Fluorescence property is preferable, and when selecting 365nm excitations, the maximum wavelength of its fluorescent emission is located at 650nm, and peak shape symmetry is good, its
Fluorescence intensity is up to 2901.
CdTe quantum manufactured in the present embodiment to various concentrations phenolethanolamine A that spectrum change figure is quenched is as shown in Figure 4.
Wherein, curve corresponds to the concentration of phenolethanolamine A and is sequentially increased from the bottom to top, i.e.,：Nethermost curve corresponds to the dense of phenolethanolamine A
Minimum 0 is spent, the concentration that uppermost curve corresponds to phenolethanolamine A is up to 2.0 × 10-6mol/L.As shown in Figure 4, with benzene
Monoethanolamine A concentration increases to 2.0 × 10 from 0-6Mol/L, the fluorescence intensity of system progressively increase to the 24.9% of initial value.
Embodiment 2
A kind of preparation method of CdTe quantum of the present embodiment, includes the following steps：
(1) 0.12g telluriums powder and 0.1200g sodium borohydrides are weighed respectively, and adds 2mL high purity waters, are sealed with sealed membrane rapidly
Firmly seal, while be inserted into injection needle and communicated with the external world, reaction 4h is stirred under the conditions of ice-water bath, 10min is stood, obtains
NaHTe solution；
(2) 0.08gCdCl is weighed2·2.5H2O is dissolved in 180mL high purity waters, adds 100 μ L mercaptopropionic acids, is formed outstanding
Turbid system；
(3) pH for first using the 0.1mol/LNaOH solution adjusting suspended liquid system is 10, leads to high pure nitrogen 30min,
Under nitrogen protection, NaHTe solution described in 500 μ L is added, controls Cd in solution2+、HTe-, mercaptopropionic acid molar ratio be 0.9:
0.7:2.8, obtain CdTe quantum presoma；
(4) the CdTe quantum presoma is transferred in the micro-wave diminishing pot of polytetrafluoroethyllining lining, power setting
400w, 120 DEG C of heating 20min, through cooling down, washing, centrifuging, up to the CdTe quantum.
A kind of method of content using CdTe quantum detection phenolethanolamine A of the present embodiment, detection sample are positive pig
Urine samples liquid (is used to detect) as blind sample, includes the following steps：
(a) fluorescence sensitivity standard curve is made：
A series of phenolethanolamine A standard solution of various concentrations is prepared, and it is moved in the colorimetric cylinder of 5mL respectively, to
1.0mL concentration is added in each colorimetric cylinder as 7.25 × 10-4The CdTe solution of mol/L, is delayed with the phosphate of pH=7.4
Solution constant volume is rushed, after shaking up, room temperature places 15min, and the fluorescence intensity F of above-mentioned each system is detected with molecular fluorescence photometer；
Meanwhile it is 7.25 × 10 to take 1.0mL concentration-4The CdTe solution of mol/L is added in the colorimetric cylinder of 5mL, with the phosphoric acid of pH=7.4
Salt buffer solution constant volume, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection architecture0；
(b) pig urine samples liquid is taken, it is 7.0 to adjust pH with NaOH solution, filters and will collect filtrate, up to sample to be tested
Liquid；
(2) analyte sample fluid is added in the colorimetric cylinder of 5mL to CdTe quantum solution described in 1.0mL respectively,
With the phosphate buffer solution constant volume of pH=7.4, shake up and stand 15min, it is examined after fully reacting with molecular fluorescence photometer
The fluorescence intensity F for measuring system is 999.0, and testing conditions are：Excitation wavelength is 365nm, and excitation and transmite slit width are equal
For 5nm, sweep speed 1200nm/min；
Compareed with the equation of linear regression of fluorescence sensitivity curve, you can draw phenolethanolamine A in the pig urine samples liquid
Content is 10 μ g/L of ＜.
Embodiment 3
A kind of preparation method of CdTe quantum of the present embodiment, includes the following steps：
(1) 0.13g telluriums powder and 0.1300g sodium borohydrides are weighed respectively, and adds 4mL high purity waters, are sealed with sealed membrane rapidly
Firmly seal, while be inserted into injection needle and communicated with the external world, reaction 4h is stirred under the conditions of ice-water bath, 10min is stood, obtains
NaHTe solution；
(2) 0.06gCdCl is weighed2·2.5H2O is dissolved in 200mL high purity waters, adds mercaptopropionic acid, forms suspended liquid
System；
(3) pH for first using the 0.1mol/LNaOH solution adjusting suspended liquid system is 12, leads to high pure nitrogen 30min,
Under nitrogen protection, NaHTe solution described in 400 μ L is added, controls Cd in solution2+、HTe-, mercaptopropionic acid molar ratio be 0.8:
0.6:2.5, obtain CdTe quantum presoma；
(4) the CdTe quantum presoma is transferred in microwave dissolver, power setting 1200w, 160 DEG C of heating
5min, through cooling down, washing, centrifuging, up to the CdTe quantum.
A kind of method of content using CdTe quantum detection phenolethanolamine A of the present embodiment, detection sample are positive pig
Urine samples liquid (is used to detect) as blind sample, includes the following steps：
(a) fluorescence sensitivity standard curve is made：
A series of phenolethanolamine A standard solution of various concentrations is prepared, and it is moved in the colorimetric cylinder of 5mL respectively, to
1.0mL concentration is added in each colorimetric cylinder as 7.25 × 10-4The CdTe solution of mol/L, is delayed with the phosphate of pH=7.4
Solution constant volume is rushed, after shaking up, room temperature places 15min, and the fluorescence intensity F of above-mentioned each system is detected with molecular fluorescence photometer；
Meanwhile it is 7.25 × 10 to take 1.0mL concentration-4The CdTe solution of mol/L is added in the colorimetric cylinder of 5mL, with the phosphoric acid of pH=7.4
Salt buffer solution constant volume, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection architecture0；
(b) pig urine samples liquid is taken, it is 7.0 to adjust pH with NaOH solution, filters and will collect filtrate, up to sample to be tested
Liquid；
Respectively to CdTe quantum solution described in 1.0mL, the analyte sample fluid is added in the colorimetric cylinder of 5mL, is used
The phosphate buffer solution constant volume of pH=7.4, shakes up and stands 15min, it is detected after fully reacting with molecular fluorescence photometer
The fluorescence intensity F for obtaining system is 1128, and testing conditions are：Excitation wavelength is 365nm, and excitation and transmite slit width are
5nm, sweep speed 1200nm/min；
Compareed with the equation of linear regression of fluorescence sensitivity curve, you can draw phenolethanolamine in the positive pig urine samples liquid
The content of A is 51.7 μ g/L.
Experimental example 1Detection limit is tested
This experimental example follows the steps below detection limit experiment：
(1) standard solution of phenolethanolamine A is taken, using the phosphate buffer solution of pH=7.4 as solvent, dilution step by step obtains
The standard solution of phenolethanolamine A a series of, in the standard solution concentration of phenolethanolamine A be respectively 8,16,32,40,60,
80、120μg/L。
(2) the phenolethanolamine A standard solution of above-mentioned series concentration is moved in the colorimetric cylinder of 5mL respectively, to each described
1.0mL concentration is added in colorimetric cylinder as 7.25 × 10-4The CdTe solution of mol/L, is determined with the phosphate buffer solution of pH=7.4
Hold, shake up rear room temperature and place 15min, the fluorescence intensity that above-mentioned each system is detected with molecular fluorescence photometer is respectively F1=
1041st, F2=1060, F3=1093, F4=1112, F5=1152, F6=1189, F7=1250；Testing conditions are：Excitation wave
A length of 365nm, excitation and transmite slit width are 5nm；
In addition the colorimetric cylinder 1.0mL concentration for taking a 5mL is 7.25 × 10-4The CdTe solution of mol/L, with pH=7.4's
Phosphate buffer solution constant volume, above-mentioned blank sample system (being free of phenolethanolamine A) is detected after shaking up with molecular fluorescence photometer
Fluorescence intensity F0For 998.2, testing conditions are：Excitation wavelength is 365nm, and excitation and transmite slit width are 5nm；
For the phenolethanolamine A standard solution of above-mentioned series concentration, the relative intensity of fluorescence detected is respectively F1/F0
=1.043, F2/F0=1.062, F3/F0=1.091, F4/F0=1.109, F5/F0=1.151, F6/F0=1.191, F7/F0
=1.253；
(3) using phenolethanolamine A concentration as abscissa, relative intensity of fluorescence is ordinate, obtains the phenolethanolamine A to CdTe
The equation of linear regression (as shown in Figure 5) of quantum dot fluorescence enhanced sensitivity.
As shown in Figure 5, when the concentration range of the phenolethanolamine A is 8-120 μ g/L, the fluorescence sensitivity curve it is linear
Regression equation is F/F0=0.0019C+1.0321, linearly dependent coefficient 0.996.This shows that phenolethanolamine A is to CdTe quantum
The fluorescence sensitivity of point has higher sensitivity and the wider range of linearity.
By the Parallel testing of the continuous 11 progress fluorescence intensity of blank sample system.The results show that continuous 11 parallel inspections
The standard deviation of survey is 0.0015, and the detection for going out according to 3 times of standard deviation calculations this method detection phenolethanolamine A is limited to 2.37
μ g/L, detection limit are relatively low.
Experimental example 2Recovery of standard addition is tested
This experimental example follows the steps below recovery of standard addition experiment：The standard solution of phenolethanolamine A is added to sky
In white pig urine samples liquid (i.e. the negative sample liquid of pig urine), control spiked levels are respectively 10,50,100 μ g/L, according to embodiment
1 the method detects the content of phenolethanolamine A in pig urine samples liquid, carries out 6 horizontal surveies under each spiked levels, is averaged
Value.
According to the actual recovery of standard addition for adding scalar sum testing result, calculating phenolethanolamine A in pig urine samples liquid.It is specific real
Test that the results are shown in Table 1.
1 recovery of standard addition experimental result of table
| Mark-on amount (μ g/L) | 10 | 50 | 100 |
| Practical measurement average value | 10±2.7 | 50±6.4 | 100±20.8 |
| The rate of recovery (%) | 73.0~127.0 | 87.2~112.0 | 79.2~120.8 |
As shown in Table 1, the recovery of standard addition of phenolethanolamine A is 86.6%-95.8% in pig urine samples liquid, recovery of standard addition
It is higher.
Experimental example 3Accuracy is tested
This experimental example follows the steps below accuracy experiment：Measured using high performance liquid chromatography tandem mass spectrum technology real
The content of phenolethanolamine A in pig urine samples liquid described in example 3 is applied, testing result is 51.0 μ g/L.
This shows, detects the content of phenolethanolamine A in pig urine samples liquid using 3 the method for embodiment and uses efficient liquid
The result of phase chromatographic tandem mass-spectrometric technique measure is consistent, and this method accuracy is higher, and accuracy is higher.
Obviously, the above embodiments are merely examples for clarifying the description, and the restriction not to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (6)
1. a kind of method of content using CdTe quantum detection phenolethanolamine A, it is characterised in that include the following steps：
(a) fluorescence sensitivity standard curve is made：
A series of phenolethanolamine A standard solution of various concentrations is prepared, and it is moved in the colorimetric cylinder of 5mL respectively, to each
1.0mL concentration is added in the colorimetric cylinder as 7.25 × 10-4The CdTe solution of mol/L, it is molten with the phosphate-buffered of pH=7.4
Liquid constant volume, after shaking up, room temperature places 15min, with molecular fluorescence photometer difference fluorescence intensity F；Meanwhile take 1.0mL dense
Spend for 7.25 × 10-4The CdTe solution of mol/L is added in the colorimetric cylinder of 5mL, is determined with the phosphate buffer solution of pH=7.4
Hold, shake up rear room temperature and place 15min, with molecular fluorescence photometer difference fluorescence intensity F0；
Using phenolethanolamine A concentration as abscissa, with F/F0For ordinate, lines of the phenolethanolamine A to CdTe quantum fluorescence sensitivity is obtained
Property regression equation；
(b) 1.0mL7.25 × 10 are taken respectively-4The CdTe solution of mol/L and the sample liquid of the A containing phenolethanolamine are added to the ratio of 5mL
In colour tube, with the phosphate buffer solution constant volume of pH=7.4, shaking up makes it fully react, and room temperature places 15min, glimmering with molecule
Light photometer detects to obtain the fluorescence intensity of system, with linear regressions of the phenolethanolamine A to CdTe quantum fluorescence sensitivity
Equation compares, up to the content of phenolethanolamine A in the sample liquid；
The preparation method of the CdTe quantum comprises the following steps：
(1) 0.12-0.13g telluriums powder and 0.11-0.13g sodium borohydrides are weighed respectively, and adds 1-4mL high purity waters, in ice-water bath
Under the conditions of be stirred reaction 4h, obtain NaHTe solution；
(2) 0.060-0.080gCdCl is weighed2·2.5H2O is dissolved in 180-200mL high purity waters, adds 80-100 μ L sulfydryls third
Acid, obtains suspension；
(3) it is 10-12 with the pH of the 0.1mol/L NaOH solutions adjusting suspension, under nitrogen protection, adds 200-500 μ
NaHTe solution described in L, controls Cd2+、HTe-, mercaptopropionic acid molar ratio be 0.8~1.0:0.6~0.8:2.5~3.0, obtain
CdTe quantum precursor solution；
(4) the CdTe quantum precursor solution is transferred in microwave dissolver, 100-160 DEG C of heating 5-20min, through cold
But, wash, centrifuge, up to the CdTe quantum.
2. the method for the content according to claim 1 using CdTe quantum detection phenolethanolamine A, it is characterised in that
In the step (a) and the step (b), the testing conditions of the fluorescence intensity are：Excitation wavelength is 365nm, excitation and hair
It is 5nm to penetrate slit width.
3. the method for the content according to claim 1 or 2 using CdTe quantum detection phenolethanolamine A, its feature exist
In the concentration of the phenolethanolamine A standard solution is respectively 8 μ g/L, 16 μ g/L, 32 μ g/L, 40 μ g/L, 60 μ g/L, 80 μ g/L
With 120 μ g/L.
4. the method for the content according to claim 1 or 2 using CdTe quantum detection phenolethanolamine A, its feature exist
In when the concentration range of the phenolethanolamine A standard solution is 8 μ g/L-120 μ g/L, the phenolethanolamine A is to CdTe quantum
The equation of linear regression F/F of point fluorescence sensitivity0=0.0019C+1.0321, linearly dependent coefficient 0.996.
5. the method for the content according to claim 1 or 2 using CdTe quantum detection phenolethanolamine A, its feature exist
In the sample liquid of the A containing phenolethanolamine is urinated for pig.
6. the method for the content according to claim 5 using CdTe quantum detection phenolethanolamine A, it is characterised in that
The pig urine is by following pretreatment：
Take pig urine samples liquid, it is 7.0 to adjust pH with NaOH solution, filters and will collect filtrate, to obtain the final product.
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