CN105738330A - Method for detecting content of phenylethanolamine A by utilizing CdTe quantum dot - Google Patents

Method for detecting content of phenylethanolamine A by utilizing CdTe quantum dot Download PDF

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CN105738330A
CN105738330A CN201610051463.XA CN201610051463A CN105738330A CN 105738330 A CN105738330 A CN 105738330A CN 201610051463 A CN201610051463 A CN 201610051463A CN 105738330 A CN105738330 A CN 105738330A
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phenylethanolamine
cdte quantum
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cdte
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CN105738330B (en
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张金艳
魏益华
罗林广
邱素艳
廖且根
胡丽芳
魏本华
周瑶敏
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Institute Of Agricultural Products Quality Safety And Standard Jiangxi Academy Of Agricultural Sciences
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    • G01N21/62Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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Abstract

The invention relates to a method for detecting the content of phenylethanolamine A by utilizing a CdTe quantum dot. The method takes mercaptopropionic acid as a stabilizer; the CdTe quantum dot prepared by a microwave radiation heating method is used as a fluorescent probe; and the method for detecting the content of the phenylethanolamine A is established based on a fluorescent intensity enhancing effect on the CdTe quantum dot by the phenylethanolamine A. The method comprises the following steps: uniformly mixing the CdTe quantum dot with the phenylethanolamine A of a substance to be detected in a phosphate buffering solution; standing for 15 minutes; and detecting the fluorescent intensity of a system by adopting a molecular fluorescence photometer so as to realize trace detection of the phenylethanolamine A. The method has the advantages of high detection sensitivity, simplicity and convenience for operation, short detection time, low analysis cost, relatively low detection limit and relatively high standard recovery rate.

Description

A kind of method of the content utilizing CdTe quantum detection phenylethanolamine A
Technical field
The invention belongs to analytical chemistry field, a kind of method being specifically related to content utilizing CdTe quantum detection phenylethanolamine A.
Background technology
Phenylethanolamine A belongs to beta-receptor agonist, the nutritional labeling in animal body can be made to be shifted to muscle by fat, show repartitioning function effect, and then the substance metabolism of regulation and control animal body, strengthen steatolysis, promote protein synthesis, significantly improve carcass lean meat percentage and the price of deed.But, beta-receptor agonist is easily in animal tissue, and particularly accumulation residual in internal organs, it can cause the symptoms such as muscular tremor, arrhythmia, headache after entering human body by food chain, and severe patient is likely to threat to life.For these reasons, the beta-receptor agonist such as phenylethanolamine A, Clenbuterol, phenylethanolamine A amine were classified as, in 1997, the medicine forbidding using in feedstuff and cultivation domestic animal drinking water by China.But, still have culturist illegal to be used in animal husbandry by it at present, cause drug residue, thus consumer health is caused serious harm.
Chinese patent literature CN104792762A discloses a kind of method utilizing CdTe quantum detection by quantitative albuterol, by the CdTe quantum of the TGA by finishing with test substance albuterol after phosphate buffer is mixed homogeneously, adopt molecular fluorescence photometer that the fluorescence intensity of system is detected, the trace detection to albuterol can be realized.But, due to the difference of albuterol and phenylethanolamine A structure, different from the mechanism of CdTe quantum effect, said method can not be used for detecting the content of phenylethanolamine A.
Therefore, a kind of method studying content utilizing CdTe quantum detection phenylethanolamine A is significant.
Summary of the invention
For this, the present invention proposes a kind of method of content utilizing CdTe quantum detection phenylethanolamine A.
For solving above-mentioned technical problem, the present invention is achieved through the following technical solutions:
The preparation method that the present invention provides a kind of CdTe quantum for phenylethanolamine A detection, comprises the steps:
(1) weigh 0.12-0.13g tellurium powder and 0.11-0.13g sodium borohydride respectively, and add 1-4mL high purity water, be stirred reaction 4h when ice-water bath, obtain NaHTe solution;
(2) 0.060-0.080gCdCl is weighed2·2.5H2O is dissolved in 180-200mL high purity water, adds 80-100 μ L mercaptopropionic acid, obtains suspension;
(3) pH with the 0.1mol/LNaOH solution described suspension of adjustment is 10-12, under nitrogen protection, adds NaHTe solution described in 200-500 μ L, controls Cd2+、HTe-, mercaptopropionic acid mol ratio be 0.8~1.0:0.6~0.8:2.5~3.0, obtain CdTe quantum precursor solution;
(4) described CdTe quantum precursor solution is transferred in microwave dissolver, 100-160 DEG C of heating 5-20min, cooled, washing, centrifugal, obtain described CdTe quantum.
The present invention also provides for the application in the content detection of phenylethanolamine A of CdTe quantum that above-mentioned preparation method prepares.
The present invention also provides for a kind of method of content utilizing CdTe quantum detection phenylethanolamine A, and described CdTe quantum is the CdTe quantum utilizing above-mentioned preparation method to prepare, and comprises the steps:
A () makes fluorescence sensitivity standard curve:
Preparing the phenylethanolamine A standard solution of a series of variable concentrations, and it moved in the color comparison tube of 5mL respectively, all adding 1.0mL concentration in each described color comparison tube is 7.25 × 10-4The CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, after shaking up, room temperature places 15min, detects the fluorescence intensity F of above-mentioned each individual system with molecular fluorescence photometer;Meanwhile, take in the color comparison tube that the CdTe solution that 1.0mL concentration is 7.25 × 10-4mol/L joins 5mL, with the phosphate buffered solution constant volume of pH=7.4, shake up rear room temperature and place 15min, with the fluorescence intensity F of molecular fluorescence photometer detection system0
With phenylethanolamine A concentration for abscissa, with F/F0For vertical coordinate, obtain the phenylethanolamine A equation of linear regression to CdTe quantum fluorescence sensitivity;
B () takes 1.0mL7.25 × 10 respectively-4The CdTe solution of mol/L and the sample liquid containing phenylethanolamine A join in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shake up and make it fully react, room temperature places 15min, the fluorescence intensity of system is obtained with the detection of molecular fluorescence photometer, with described phenylethanolamine A, the equation of linear regression of CdTe quantum fluorescence sensitivity is compareed, obtain the content of phenylethanolamine A in described sample liquid.
Preferably, in the method for the above-mentioned content utilizing CdTe quantum detection phenylethanolamine A of the present invention, in described step (a) and described step (b), the testing conditions of described fluorescence intensity is: excitation wavelength is 365nm, excites and launches slit width and is 5nm.
It is further preferred that in the method for the above-mentioned content utilizing CdTe quantum detection phenylethanolamine A of the present invention, the concentration of described phenylethanolamine A standard solution 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.
Further preferably, in the method for the above-mentioned content utilizing CdTe quantum detection phenylethanolamine A of the present invention, when the concentration range of described phenylethanolamine A standard solution is 8 μ g/L-120 μ g/L, the described phenylethanolamine A equation of linear regression F/F to CdTe quantum fluorescence sensitivity0=0.0019C+1.0321, linearly dependent coefficient is 0.996.
It is further preferred that in the method for the above-mentioned content utilizing CdTe quantum detection phenylethanolamine A of the present invention, the described sample liquid containing phenylethanolamine A is pig urine.
It is further preferred that in the method for the above-mentioned content utilizing CdTe quantum detection phenylethanolamine A of the present invention, described pig urinates through following pretreatment:
Taking pig urine samples liquid, regulating pH by NaOH solution is 7.0, filters and will collect filtrate, to obtain final product.
The technique scheme of the present invention has the advantage that compared to existing technology
(1) method of the content utilizing CdTe quantum detection phenylethanolamine A of the present invention, by the CdTe quantum by finishing mercaptopropionic acid, mix homogeneously at phosphate buffer with test substance phenylethanolamine A, room temperature places 15min, adopt molecular fluorescence photometer that the fluorescence intensity of system is detected, the trace detection to phenylethanolamine A can be realized, this is owing to the CdTe quantum surface of preparation has carboxyl, by covalency coupling, chain phenylethanolamine A, the surface defect making CdTe quantum reduces, closely fluorescence intensity enhancing, utilize the change of CdTe quantum fluorescence intensity, realize the detection by quantitative to phenylethanolamine A;Result shows, phenylethanolamine A in the scope of 8-120 μ g/L, the concentration of phenylethanolamine A and the fluorescence intensity F/F of system0All present good linear relationship, linearly dependent coefficient 0.996, illustrate that the fluorescence sensitivity of CdTe quantum is had higher sensitivity and the wider range of linearity by phenylethanolamine A;
(2) method of the content utilizing CdTe quantum detection phenylethanolamine A of the present invention, detection sensitivity is high, easy and simple to handle, and the 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 utilizing CdTe quantum detection phenylethanolamine A of the present invention, carries out pretreatment to described pig urine, effectively to remove the interference of metal ion in pig urine samples.
Accompanying drawing explanation
In order to make present disclosure be more likely to be clearly understood, below according to specific embodiments of the invention and in conjunction with accompanying drawing, the present invention is further detailed explanation, wherein:
Fig. 1 is the TEM figure of the CdTe quantum of the embodiment of the present invention 1 preparation;
Fig. 2 is the CdTe quantum of the embodiment of the present invention 1 preparation fluorescence photo under UV illumination is penetrated;
Fig. 3 is the fluorescence spectrum figure of the CdTe quantum of the embodiment of the present invention 1 preparation;
Fig. 4 is the CdTe quantum of the embodiment of the present invention 1 preparation cancellation spectrum change figure to variable concentrations phenylethanolamine A;
Fig. 5 is the phenylethanolamine A equation of linear regression to CdTe quantum fluorescence sensitivity in experimental example 1 of the present invention.
Detailed description of the invention
Below in conjunction with accompanying drawing, technical scheme is clearly and completely described, it is clear that described embodiment is a part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under not making creative work premise, broadly fall into the scope of protection of the invention.
In following example of the present invention and experimental example, molecular fluorescence photometer (model: F7000, Hitachi, Ltd offer);Phenylethanolamine A standard substance are purchased from sigma.
Embodiment 1
The preparation method of a kind of CdTe quantum of the present embodiment, comprises the steps:
(1) weigh 0.1276g tellurium powder and 0.1100g sodium borohydride respectively, and add 1mL high purity water, seal with ParafilmTM rapidly, it is inserted simultaneously into injection needle to communicate with the external world, it is stirred reaction 4h when ice-water bath, stands 10min, obtain 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 water, adds 80 μ L mercaptopropionic acids, forms suspension system;
(3) first regulating the pH of described suspension system with 0.1mol/LNaOH solution is 11, and logical high pure nitrogen 30min under nitrogen protection, adds NaHTe solution described in 200 μ L, controls Cd in solution2+、HTe-, mercaptopropionic acid mol ratio be 1.0:1.0:3.0, obtain CdTe quantum presoma;
(4) described CdTe quantum presoma is transferred in microwave dissolver, power setting 800w, 100 DEG C of heating 10min, cooled, washing, centrifugal, obtain described CdTe quantum.
The method of a kind of content utilizing CdTe quantum detection phenylethanolamine A of the present embodiment, detection sample is the negative pig urine samples liquid (it can be used as blind sample for detecting) without phenylethanolamine A, comprises the steps:
A () makes fluorescence sensitivity standard curve:
Preparing the phenylethanolamine A standard solution of a series of variable concentrations, and it moved in the color comparison tube of 5mL respectively, all adding 1.0mL concentration in each described color comparison tube is 7.25 × 10-4The CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, after shaking up, room temperature places 15min, detects the fluorescence intensity F of above-mentioned each individual system with molecular fluorescence photometer;Meanwhile, taking 1.0mL concentration is 7.25 × 10- 4The CdTe solution of mol/L joins in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection system0
With phenylethanolamine A concentration for abscissa, with F/F0For vertical coordinate, obtain the phenylethanolamine A equation of linear regression to CdTe quantum fluorescence sensitivity;
B () takes pig urine samples liquid, regulating pH by NaOH solution is 7.0, filters and will collect filtrate, obtaining analyte sample fluid;
Respectively to CdTe quantum solution described in 1.0mL, described analyte sample fluid is joined in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shake up standing 15min, detecting, with molecular fluorescence photometer, the fluorescence intensity F obtaining system after making it fully react is 998.0, testing conditions is: excitation wavelength is 365nm, excites and launches slit width and is 5nm, and scanning speed is 1200nm/min;
With described phenylethanolamine A, the equation of linear regression of CdTe quantum fluorescence sensitivity being compareed, can draw the content without phenylethanolamine A in described negative pig urine samples liquid, testing result is consistent with the fact that in described negative pig urine samples liquid without phenylethanolamine A.
The TEM of CdTe quantum prepared by the present embodiment schemes as shown in Figure 1.As shown in Figure 1, the pattern of CdTe quantum is spherical, good dispersion, and particle diameter is 4.5nm and is distributed homogeneous.
CdTe quantum prepared by the present embodiment fluorescence photo under UV illumination is penetrated is as shown in Figure 2.As shown in Figure 2, CdTe quantum sends the fluorescence of Chinese red under UV illumination is penetrated.
The fluorescence spectrum figure of CdTe quantum prepared by the present embodiment is as shown in Figure 3.From the figure 3, it may be seen that the fluorescence property of CdTe quantum is better, when selecting 365nm to excite, the maximum wavelength of its fluorescent emission is positioned at 650nm, and peak shape symmetry is good, and its fluorescence intensity is up to 2901.
CdTe quantum prepared by the present embodiment is to the cancellation spectrum change figure of variable concentrations phenylethanolamine A as shown in Figure 4.Wherein, the concentration of curve corresponding phenylethanolamine A from the bottom to top increases successively, it may be assumed that the concentration of nethermost curve correspondence phenylethanolamine A is minimum is 0, and the concentration of uppermost curve correspondence phenylethanolamine A is 2.0 × 10 to the maximum-6mol/L.As shown in Figure 4, along with phenylethanolamine A concentration increases to 2.0 × 10 from 0-6Mol/L, the fluorescence intensity of system progressively increases to the 24.9% of initial value.
Embodiment 2
The preparation method of a kind of CdTe quantum of the present embodiment, comprises the steps:
(1) weigh 0.12g tellurium powder and 0.1200g sodium borohydride respectively, and add 2mL high purity water, seal with ParafilmTM rapidly, be inserted simultaneously into injection needle and communicate with the external world, be stirred reaction 4h when ice-water bath, stand 10min, obtain NaHTe solution;
(2) 0.08gCdCl is weighed2·2.5H2O is dissolved in 180mL high purity water, adds 100 μ L mercaptopropionic acids, forms suspension system;
(3) first regulating the pH of described suspension system with 0.1mol/LNaOH solution is 10, and logical high pure nitrogen 30min under nitrogen protection, adds NaHTe solution described in 500 μ L, controls Cd in solution2+、HTe-, mercaptopropionic acid mol ratio be 0.9:0.7:2.8, obtain CdTe quantum presoma;
(4) described CdTe quantum presoma is transferred in teflon-lined micro-wave diminishing pot, power setting 400w, 120 DEG C of heating 20min, cooled, washing, centrifugal, obtain described CdTe quantum.
The method of a kind of content utilizing CdTe quantum detection phenylethanolamine A of the present embodiment, detection sample is positive pig urine samples liquid (it can be used as blind sample for detecting), comprises the steps:
A () makes fluorescence sensitivity standard curve:
Preparing the phenylethanolamine A standard solution of a series of variable concentrations, and it moved in the color comparison tube of 5mL respectively, all adding 1.0mL concentration in each described color comparison tube is 7.25 × 10-4The CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, after shaking up, room temperature places 15min, detects the fluorescence intensity F of above-mentioned each individual system with molecular fluorescence photometer;Meanwhile, taking 1.0mL concentration is 7.25 × 10- 4The CdTe solution of mol/L joins in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection system0
B () takes pig urine samples liquid, regulating pH by NaOH solution is 7.0, filters and will collect filtrate, obtaining analyte sample fluid;
(2) respectively to CdTe quantum solution described in 1.0mL, described analyte sample fluid is joined in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shake up standing 15min, detecting, with molecular fluorescence photometer, the fluorescence intensity F obtaining system after making it fully react is 999.0, testing conditions is: excitation wavelength is 365nm, excites and launches slit width and is 5nm, and scanning speed is 1200nm/min;
Compare with the equation of linear regression of fluorescence sensitivity curve, can show that in described pig urine samples liquid, the content of phenylethanolamine A is < 10 μ g/L.
Embodiment 3
The preparation method of a kind of CdTe quantum of the present embodiment, comprises the steps:
(1) weigh 0.13g tellurium powder and 0.1300g sodium borohydride respectively, and add 4mL high purity water, seal with ParafilmTM rapidly, be inserted simultaneously into injection needle and communicate with the external world, be stirred reaction 4h when ice-water bath, stand 10min, obtain NaHTe solution;
(2) 0.06gCdCl is weighed2·2.5H2O is dissolved in 200mL high purity water, adds mercaptopropionic acid, forms suspension system;
(3) first regulating the pH of described suspension system with 0.1mol/LNaOH solution is 12, and logical high pure nitrogen 30min under nitrogen protection, adds NaHTe solution described in 400 μ L, controls Cd in solution2+、HTe-, mercaptopropionic acid mol ratio be 0.8:0.6:2.5, obtain CdTe quantum presoma;
(4) described CdTe quantum presoma is transferred in microwave dissolver, power setting 1200w, 160 DEG C of heating 5min, cooled, washing, centrifugal, obtain described CdTe quantum.
The method of a kind of content utilizing CdTe quantum detection phenylethanolamine A of the present embodiment, detection sample is positive pig urine samples liquid (it can be used as blind sample for detecting), comprises the steps:
A () makes fluorescence sensitivity standard curve:
Preparing the phenylethanolamine A standard solution of a series of variable concentrations, and it moved in the color comparison tube of 5mL respectively, all adding 1.0mL concentration in each described color comparison tube is 7.25 × 10-4The CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, after shaking up, room temperature places 15min, detects the fluorescence intensity F of above-mentioned each individual system with molecular fluorescence photometer;Meanwhile, taking 1.0mL concentration is 7.25 × 10- 4The CdTe solution of mol/L joins in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection system0
B () takes pig urine samples liquid, regulating pH by NaOH solution is 7.0, filters and will collect filtrate, obtaining analyte sample fluid;
Respectively to CdTe quantum solution described in 1.0mL, described analyte sample fluid is joined in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shake up standing 15min, detecting, with molecular fluorescence photometer, the fluorescence intensity F obtaining system after making it fully react is 1128, testing conditions is: excitation wavelength is 365nm, excites and launches slit width and is 5nm, and scanning speed is 1200nm/min;
Compare with the equation of linear regression of fluorescence sensitivity curve, can show that in described positive pig urine samples liquid, the content of phenylethanolamine A is 51.7 μ g/L.
Experimental example 1Detection limit is tested
This experimental example carries out detection limit experiment according to following steps:
(1) standard solution of phenylethanolamine A is taken, with the phosphate buffered solution of pH=7.4 for solvent, stepwise dilution obtains the standard solution of a series of phenylethanolamine A, the concentration of phenylethanolamine A respectively 8,16,32,40,60,80,120 μ g/L in described standard solution.
(2) being moved to respectively by the phenylethanolamine A standard solution of above-mentioned series concentration in the color comparison tube of 5mL, all adding 1.0mL concentration in each described color comparison tube is 7.25 × 10-4The CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, shake up rear room temperature and place 15min, detect fluorescence intensity respectively F1=1041, F2=1060, F3=1093, F4=1112, F5=1152, F6=1189, F7=1250 of above-mentioned each individual system with molecular fluorescence photometer;Testing conditions is: excitation wavelength is 365nm, excites and launches slit width and is 5nm;
The color comparison tube 1.0mL concentration additionally taking a 5mL is 7.25 × 10-4The CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, detects the fluorescence intensity F of above-mentioned blank sample system (without phenylethanolamine A) with molecular fluorescence photometer after shaking up0Being 998.2, testing conditions is: excitation wavelength is 365nm, excites and launches slit width and is 5nm;
For the phenylethanolamine A standard solution of above-mentioned series concentration, the relative intensity of fluorescence respectively F1/F that detection obtains0=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) with phenylethanolamine A concentration for abscissa, relative intensity of fluorescence is vertical coordinate, obtains the described phenylethanolamine A equation of linear regression (as shown in Figure 5) to CdTe quantum fluorescence sensitivity.
As shown in Figure 5, when the concentration range of described phenylethanolamine A is 8-120 μ g/L, the equation of linear regression of described fluorescence sensitivity curve is F/F0=0.0019C+1.0321, linearly dependent coefficient is 0.996.This shows, the fluorescence sensitivity of CdTe quantum is had higher sensitivity and the wider range of linearity by phenylethanolamine A.
Continuous for blank sample system 11 times are carried out the Parallel testing of fluorescence intensity.Result shows, the standard deviation of continuous 11 Parallel testings is 0.0015, and according to 3 times of standard deviation calculation go out this method detection phenylethanolamine A detection be limited to 2.37 μ g/L, detection limit is relatively low.
Experimental example 2Recovery of standard addition is tested
This experimental example carries out recovery of standard addition experiment according to following steps: joined by the standard solution of phenylethanolamine A in blank pig urine samples liquid (i.e. the negative sample liquid of pig urine), control spiked levels respectively 10,50,100 μ g/L, the content of phenylethanolamine A in method detection pig urine samples liquid described in embodiment 1, carry out 6 horizontal surveies under each spiked levels, average.
According to the actual scalar sum testing result that adds, calculate the recovery of standard addition of phenylethanolamine A in pig urine samples liquid.Specific experiment result is as shown in table 1.
Table 1 recovery of standard addition experimental result
Add scalar (μ g/L) 10 50 100
Practical measurement meansigma methods 10±2.7 50±6.4 100±20.8
The response rate (%) 73.0~127.0 87.2~112.0 79.2~120.8
As shown in Table 1, in pig urine samples liquid, the recovery of standard addition of phenylethanolamine A is 86.6%-95.8%, and recovery of standard addition is higher.
Experimental example 3Degree of accuracy is tested
This experimental example carries out degree of accuracy experiment according to following steps: adopting the content of phenylethanolamine A in pig urine samples liquid described in using high performance liquid chromatography tandem mass spectrum technical measurement embodiment 3, testing result is 51.0 μ g/L.
This shows, adopts the content of phenylethanolamine A in method detection pig urine samples liquid described in embodiment 3 consistent with the result adopting using high performance liquid chromatography tandem mass spectrum technical measurement, and the method degree of accuracy is higher, and accuracy is higher.
Obviously, above-described embodiment is only for clearly demonstrating example, and is not the restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also cannot all of embodiment be given exhaustive.And the apparent change thus extended out or variation are still among the protection domain of the invention.

Claims (8)

1. the preparation method for the CdTe quantum of phenylethanolamine A detection, it is characterised in that comprise the steps:
(1) weigh 0.12-0.13g tellurium powder and 0.11-0.13g sodium borohydride respectively, and add 1-4mL high purity water, be stirred reaction 4h when ice-water bath, obtain NaHTe solution;
(2) 0.060-0.080gCdCl is weighed2·2.5H2O is dissolved in 180-200mL high purity water, adds 80-100 μ L mercaptopropionic acid, obtains suspension;
(3) pH with the 0.1mol/LNaOH solution described suspension of adjustment is 10-12, under nitrogen protection, adds NaHTe solution described in 200-500 μ L, controls Cd2+、HTe-, mercaptopropionic acid mol ratio be 0.8~1.0:0.6~0.8:2.5~3.0, obtain CdTe quantum precursor solution;
(4) described CdTe quantum precursor solution is transferred in microwave dissolver, 100-160 DEG C of heating 5-20min, cooled, washing, centrifugal, obtain described CdTe quantum.
2. the CdTe quantum that the preparation method described in claim 1 prepares application in the content detection of phenylethanolamine A.
3. the method utilizing the content of CdTe quantum detection phenylethanolamine A, described CdTe quantum is the CdTe quantum utilizing the preparation method described in claim 1 to prepare, it is characterised in that comprise the steps:
A () makes fluorescence sensitivity standard curve:
Preparing the phenylethanolamine A standard solution of a series of variable concentrations, and it moved in the color comparison tube of 5mL respectively, all adding 1.0mL concentration in each described color comparison tube is 7.25 × 10-4The CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, after shaking up, room temperature places 15min, detects the fluorescence intensity F of above-mentioned each individual system with molecular fluorescence photometer;Meanwhile, taking 1.0mL concentration is 7.25 × 10- 4The CdTe solution of mol/L joins in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shakes up rear room temperature and places 15min, with the fluorescence intensity F of molecular fluorescence photometer detection system0
With phenylethanolamine A concentration for abscissa, with F/F0For vertical coordinate, obtain the phenylethanolamine A equation of linear regression to CdTe quantum fluorescence sensitivity;
B () takes 1.0mL7.25 × 10 respectively-4The CdTe solution of mol/L and the sample liquid containing phenylethanolamine A join in the color comparison tube of 5mL, with the phosphate buffered solution constant volume of pH=7.4, shake up and make it fully react, room temperature places 15min, the fluorescence intensity of system is obtained with the detection of molecular fluorescence photometer, with described phenylethanolamine A, the equation of linear regression of CdTe quantum fluorescence sensitivity is compareed, obtain the content of phenylethanolamine A in described sample liquid.
4. the method for the content utilizing CdTe quantum detection phenylethanolamine A according to claim 3, it is characterized in that, in described step (a) and described step (b), the testing conditions of described fluorescence intensity is: excitation wavelength is 365nm, excites and launches slit width and is 5nm.
5. the method for the content utilizing CdTe quantum detection phenylethanolamine A according to claim 3 or 4, it is characterized in that, the concentration of described phenylethanolamine A standard solution 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.
6. the method for the content utilizing CdTe quantum detection phenylethanolamine A according to any one of claim 3-5, it is characterized in that, when the concentration range of described phenylethanolamine A standard solution is 8 μ g/L-120 μ g/L, the described phenylethanolamine A equation of linear regression F/F to CdTe quantum fluorescence sensitivity0=0.0019C+1.0321, linearly dependent coefficient is 0.996.
7. the method for the content utilizing CdTe quantum detection phenylethanolamine A according to any one of claim 3-6, it is characterised in that the described sample liquid containing phenylethanolamine A is pig urine.
8. the method for the content utilizing CdTe quantum detection by quantitative phenylethanolamine A according to claim 7, it is characterised in that described pig urinates through following pretreatment:
Taking pig urine samples liquid, regulating pH by NaOH solution is 7.0, filters and will collect filtrate, to obtain final product.
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