CN104792762A - Method for quantitatively detecting salbutamol by using CdTe quantum dots - Google Patents
Method for quantitatively detecting salbutamol by using CdTe quantum dots Download PDFInfo
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Abstract
The invention provides a method for quantitatively detecting salbutamol by using CdTe quantum dots. The method comprises the following steps: uniformly mixing the CdTe quantum dots with surfaces modified by mercaptoacetic acid with a substance to be detected, namely salbutamol, in a phosphate buffer solution, and then detecting fluorescent strength of a system by adopting a molecular fluorometer to realize trace detection of salbutamol because that in a weakly alkaline solution system, the CdTe quantum dots with the surfaces modified with carboxyl groups having negative charges and target molecules having positive charges, namely salbutamol, form a new compound system through electrostatic interaction so as to cause fluorescence quenching. Detection results show that salbutamol has relatively high sensitivity and a relatively wide linear range against the fluorescence quenching of the CeTe quantum dots, so that the changes in the fluorescent strength of the CdTe quantum dots are used for realizing the quantitative detection of salbutamol; and furthermore, the method for quantitatively detecting salbutamol by using the CdTe quantum dots, provided by the invention, is very simple in experimental operation, the detection time is short and the analysis cost is low.
Description
Technical field
The present invention relates to a kind of method utilizing CdTe quantum quantitatively to detect salbutamol, belong to the detection field of salbutamol.
Background technology
Salbutamol belongs to beta-receptor activator, the nutritional labeling in animal body can be made to be shifted to muscle by fat, show repartitioning function effect, and then the metabolism of regulation and control animal body, strengthen lipolysis, promote protein synthesis, significantly improve carcass lean meat percentage and the price of deed.But beta-receptor activator is easily in animal tissue, and particularly in internal organ, accumulation is residual, and it can cause the symptoms such as muscular tremor, arrhythmia cordis, headache after entering human body by food chain, and severe patient may threat to life.In view of above reason, the beta-receptor activators such as salbutamol, Clenbuterol, Ractopamine were classified as in 1997 the medicine forbidding using in feed and cultivation domestic animal potable water by China.But, still have culturist to be illegally used in animal husbandry by it at present, cause medicament residue, thus consumer health is caused serious harm.
Chinese patent CN104251898 discloses a kind of film dialysis-Liquid Chromatography-Tandem Mass Spectrometry and measures the method that in livestock products, multiple beta-receptor activator is residual, concrete steps are as follows: (1) sample pre-treatments: accurately take the sample that 5g crushes, add 20ml0.02mol/L ammonium acetate buffer (with acetic acid furnishing pH4-5), mixing, ultrasonic 20 minutes, 8000 leave the heart 5 minutes, supernatant moves in bag filter, being immersed by bag filter fills in the brown beaker of 400-500ml0.02mol/L ammonium acetate buffer (pH4-5), put into rotor, beaker is placed on magnetic stirring apparatus and dialyses, speed of agitator drives bag filter to rotate to form vortex in cup, bag filter does not sink to being as the criterion, opaque sack on cup outer cover, time is 6h.To dialyse rear taking-up bag filter, dislysate in beaker is adjusted to pH to 9-10, move in the pyriform shunting funnel of 1L, add 40ml solvent (cyclohexane: ethyl acetate=4:1), extract 2 times, combining extraction liquid carries out revolving steaming, becomes 1.0ml, for HPLC-MS/MS determination and analysis with 0.1% aqueous formic acid (v/v) constant volume; (2) HPLC-MS/MS measures: the content adopting external standard method beta-receptor activator, liquid-phase chromatographic column adopts Thermo Hypersil Gold (2.1mm × 100mm, 3 μm), filler is selected from Octadecylsilane bonded phase silica gel, mobile phase is 0.1% aqueous formic acid A-acetonitrile B, and flow velocity is 0.2ml/min, and condition of gradient elution is: t=0min, 96%A, 4%B; T=2min, 96%A, 4%B; T=5min, 77%A, 23%B; T=12min, 5%A, 95%B; T=28min, 44%A, 56%B; T=24min, 5%A, 95%B; T=24.1min, 96%A, 4%B; T=32min, 96%A, 4%B; Mass Spectrometry Conditions is: electron spray ionisation source positive ion scanning ESI
+, multiple-reaction monitoring pattern MRM; Electron spray voltage: 5.5kV; Ion source temperature: 550 DEG C, atomization gas pressure GSI:40psi; Assisted gas flow velocity GS2:60psi, gas curtain atmospheric pressure CUR:40psi; Collision cell entrance potential EP:10V; Collision cell exit potential CXP:13V, the ion pair of monitoring analysis thing carries out medicament residue confirmatory analysis.
Said method first adopts film dialysis to carry out sample pre-treatments, Liquid Chromatography-Tandem Mass Spectrometry is adopted to measure multiple beta-receptor activator in livestock products afterwards again, but, there is sample pre-treatments complexity in above-mentioned detection method, testing process is loaded down with trivial details, analysis cost is high, sense cycle is long, expensive equipment, be difficult to the problems such as operation, be difficult to carry out execute-in-place, be restricted in actual applications.
Summary of the invention
When technical matters to be solved by this invention is to adopt Liquid Chromatography-Tandem Mass Spectrometry to detect beta-receptor activator in livestock products in prior art, there is sample pre-treatments complexity, testing process be loaded down with trivial details, analysis cost is high, sense cycle is long, expensive equipment, be difficult to the problems such as operation, thus propose a kind of simple to operate, cost is low and CdTe fluorescent optical sensor that can realize Fast Measurement salbutamol and its preparation method and application.
For solving the problems of the technologies described above, technical scheme of the present invention is as follows:
For a preparation method for the CdTe quantum that salbutamol detects, comprise the steps:
(1) take 0.12g-0.13g tellurium powder and 0.07g-0.09g sodium borohydride respectively, and add 1-2ml high purity water, under ice-water bath condition, carry out stirring reaction, obtain transparent NaHTe solution;
(2) 0.1-0.2gCdCl is taken
22.5H
2o is dissolved in 200ml high purity water, then adds 100 μ L mercaptoacetic acid, forms milky suspension system;
(3) first 0.1molL is used
-1naOH solution regulates the pH of described suspension system to be 10-12, pre-inflated with nitrogen 30min, then adds the NaHTe solution described in step (1) under nitrogen protection, control Cd
2+, HTe
-, mercaptoacetic acid mol ratio be 0.8-1.0:0.4-0.5:1.5-2.5, obtain the CdTe quantum presoma of brown;
(4) described CdTe quantum presoma is transferred in reactor, at 140-160 DEG C of heating 5-60min, through cooling, washing, centrifugally namely obtains described CdTe quantum.
Utilize described CdTe quantum quantitatively to detect a method for salbutamol, it comprises the steps:
A () makes the equation of linear regression of Stern-Volmer curve:
Prepare the salbutamol standard working solution of a series of variable concentrations, and it moved to respectively in the color comparison tube of 5ml, in each described color comparison tube, all add 1.5ml concentration is 1.45 × 10
-3the CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, shakes up the fluorescence intensity F that rear molecular fluorescence photometer detects above-mentioned each individual system; Meanwhile, getting 1.5ml concentration is 1.45 × 10
-3the 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 the fluorescence intensity F of rear molecular fluorescence photometer detection system
0;
With salbutamol concentration for horizontal ordinate, with F
0/ F is ordinate, obtains the equation of linear regression of salbutamol to the Stern-Volmer curve of CdTe quantum fluorescent quenching;
B () is got the CdTe solution described in 1.5ml respectively and is joined in the color comparison tube of 5ml containing the sample liquid of salbutamol, with the phosphate buffered solution constant volume of pH=7.4, shake up and make it fully react rear molecular fluorescence photometer to detect and obtain the fluorescence intensity of system, contrast with the equation of linear regression of Stern-Volmer curve, obtain the content of salbutamol in described sample liquid.
Step (a) is with in step (b), and the testing conditions of described fluorescence intensity is: excitation wavelength is 365nm, excites and launch slit width to be 5nm.
The concentration of the standard working solution of described salbutamol is respectively 0.042 × 10
-6, 0.084 × 10
-6, 0.126 × 10
-6, 0.168 × 10
-6, 0.210 × 10
-6, 0.252 × 10
-6, 0.420 × 10
-6, 0.630 × 10
-6, 0.84 × 10
-6, 1.26 × 10
-6, 1.68 × 10
-6, 2.10 × 10
-6mol/L.
The equation of linear regression of described Stern-Volmer curve is divided into two parts, and the concentration range of described salbutamol is 0.042 × 10
-6-0.420 × 10
-6time, the equation of linear regression of described Stern-Volmer curve is 0.8428 × 10
6c+1.0434, linearly dependent coefficient is 0.976;
The concentration range of described salbutamol is 0.420 × 10
-6-2.10 × 10
-6during mol/L, the equation of linear regression of Stern-Volmer curve is F
0/ F=0.1491 × 10
6c+1.3078, linearly dependent coefficient is 0.999.
The described sample liquid containing salbutamol is pig urine.
Described pig urine is through following pre-service:
Get pig urine samples liquid, regulate pH to be 7.0 by NaOH solution, filter and will filtrate be collected, obtaining analyte sample fluid.
Technique scheme of the present invention has the following advantages compared to existing technology:
(1) method utilizing CdTe quantum quantitatively to detect salbutamol of the present invention, by the CdTe quantum of finishing mercaptoacetic acid is mixed at phosphate buffer with test substance salbutamol, molecular fluorescence photometer is adopted to detect the fluorescence intensity of system afterwards, the trace detection to salbutamol can be realized, this is due in weakly alkaline solution system, CdTe quantum and the positively charged target molecule salbutamol of the electronegative carboxyl of finishing form new compound system by electrostatic interaction, cause fluorescent quenching, thus utilize the change of CdTe quantum fluorescence intensity, realize the quantitative detection to salbutamol, result shows, salbutamol is 0.042 × 10
-6-0.420 × 10
-6with 0.420 × 10 in the scope of mol/L
-6-2.09 × 10
-6in the scope of mol/L, the concentration of salbutamol and relative intensity of fluorescence F
0/ F all presents good linear relationship, linearly dependent coefficient is respectively up to 0.976 and 0.999, thus illustrate that the fluorescent quenching of salbutamol to CdTe quantum has higher sensitivity and the wider range of linearity, the method utilizing CdTe quantum quantitatively to detect salbutamol of the present invention, experimental implementation is very simple, detection time is short, and analysis cost is low, and detection limit is lower is 2 × 10
-8mol/L, recovery of standard addition is higher is 86.6%-95.8%, when can effectively avoid adopting in prior art Liquid Chromatography-Tandem Mass Spectrometry to detect beta-receptor activator in livestock products, there is sample pre-treatments complexity, testing process is loaded down with trivial details, analysis cost is high, sense cycle is long, expensive equipment, be difficult to the problems such as operation.
(2) CdTe quantum of the present invention quantitatively detects the method for salbutamol in pig urine, also carries out pre-service, effectively to remove the interference of metallic ion in pig urine samples to described pig urine.
Accompanying drawing explanation
In order to make content of the present invention be more likely to be clearly understood, below according to a particular embodiment of the invention and by reference to the accompanying drawings, the present invention is further detailed explanation, wherein
Fig. 1 is the TEM figure of CdTe quantum of the present invention;
Fig. 2 is the XRD figure of CdTe quantum of the present invention;
Fig. 3 is the fluorescence spectrum figure of CdTe quantum of the present invention;
Fig. 4 is the cancellation spectrum change figure of CdTe quantum of the present invention to variable concentrations salbutamol;
Fig. 5 is the Stern-Volmer curve of salbutamol to CdTe quantum fluorescent quenching.
Embodiment
Technical characterstic of the present invention is set forth further below in conjunction with specific embodiment.
1, instrument and reagent
Molecular fluorescence photometer (model: F7000, is provided by Hitachi, Ltd);
Salbutamol standard items are purchased from sigma.
2, Stern-Volmer curve and detection limit
(1) get the standard solution of salbutamol, with the phosphate buffered solution of pH=7.4 for solvent, stepwise dilution obtains the standard working solution of a series of salbutamol, and in described standard working solution, the concentration of salbutamol is respectively 0.042 × 10
-6, 0.084 × 10
-6, 0.126 × 10
-6, 0.168 × 10
-6, 0.210 × 10
-6, 0.252 × 10
-6, 0.420 × 10
-6, 0.630 × 10
-6, 0.84 × 10
-6, 1.26 × 10
-6, 1.68 × 10
-6, 2.10 × 10
-6mol/L;
(2) moved to respectively in the color comparison tube of 5ml by the salbutamol standard working solution of above-mentioned series concentration, in each described color comparison tube, all add 1.5ml concentration is 1.45 × 10
-3the CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, the fluorescence intensity shaking up the above-mentioned each individual system of rear molecular fluorescence photometer detection is respectively F1=1040, F2=1015, F3=995.1, F4=963.3, F5=931.3, F6=846.7, F7=813.2, F8=764.8, F9=735.5, F10=695, F11=619.4, F12=569.3; Testing conditions is: excitation wavelength is 365nm, excites and launch slit width to be 5nm;
Get the color comparison tube of a 5ml in addition and to add 1.5ml concentration be 1.45 × 10
-3the CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, shakes up the fluorescence intensity F that rear molecular fluorescence photometer detects above-mentioned blank sample system (not containing salbutamol)
0be 1141, testing conditions is: excitation wavelength is 365nm, excites and launch slit width to be 5nm;
For the salbutamol standard working solution of above-mentioned series concentration, detect the relative intensity of fluorescence obtained and be respectively F
0-F1=99, F
0-F2=126, F
0-F3=146, F
0-F4=177.7, F
0-F5=209.7, F
0-F6=293.4, F
0-F7=327.8, F
0-F8=376.2, F
0-F9=405.5, F
0-F10=445.5, F
0-F11=521.6, F
0-F12=571.7;
C (), with salbutamol concentration for horizontal ordinate, relative intensity of fluorescence is ordinate, obtain the Stern-Volmer curve of described salbutamol to CdTe quantum fluorescent quenching, as shown in Figure 5;
The equation of linear regression of described Stern-Volmer curve is divided into two parts, and the concentration range of described salbutamol is 0.042 × 10
-6-0.420 × 10
-6during mol/L, the equation of linear regression of described Stern-Volmer curve is F
0/ F=0.8428 × 10
6c+1.0434, linearly dependent coefficient is 0.976; The concentration range of described salbutamol is 0.420 × 10
-6-2.10 × 10
-6during mol/L, the equation of linear regression of described Stern-Volmer curve is F
0/ F=0.1491 × 10
6c+1.3078, linearly dependent coefficient is 0.999, thus illustrates that the fluorescent quenching of salbutamol to CdTe quantum has higher sensitivity and the wider range of linearity;
Continuous for blank sample system 11 times are carried out the Parallel testing of fluorescence intensity, result show, the standard deviation of measurement is 0.0021, and according to 3 times of standard deviation calculation go out this method detect detecting of salbutamol be limited to 2 × 10
-8mol/L.
3, sample tests
Embodiment 1
The present embodiment provides a kind of method utilizing CdTe quantum quantitatively to detect salbutamol in pig urine samples liquid, described pig urine samples liquid is negative sample, not containing salbutamol in known described negative pig urine samples liquid, it can be used as blind sample for detecting, detection method comprises the steps:
The preparation of (a) described CdTe quantum, specific as follows:
(1) 0.1276g tellurium powder and 0.0800g sodium borohydride is taken respectively, and add 1ml high purity water, rapid ParafilmTM seals, insert injection needle to communicate with the external world simultaneously, reaction 4h is carried out under ice-water bath and strong magnetic agitation condition, leave standstill 10min, obtain the NaHTe solution that pinkish is transparent;
Reaction equation is as follows:
4NaBH
4+2Te+7H
2O＝2NaHTe+Na
2B
4O
7+14H
2↑
(2) 0.12gCdCl is taken
22.5H
2o is dissolved in 200ml high purity water, then adds 100 μ L mercaptoacetic acid, forms milky suspension system;
(3) first 0.1molL is used
-1naOH solution regulates the pH of described suspension system to be 12, and logical high pure nitrogen 30min, then adds the described NaHTe solution that 210 μ L steps (1) prepare under nitrogen protection, controls Cd in solution
2+, HTe
-, mercaptoacetic acid mol ratio be 1.0:0.42:2.0, obtain the CdTe quantum presoma of brown;
(4) described CdTe quantum presoma is transferred in teflon-lined hydrothermal synthesis reaction still, is placed in 160 DEG C of baking ovens and heats 50min, through cooling, washing, centrifugally namely obtain described CdTe quantum;
B the CdTe quantum described in () utilization quantitatively detects salbutamol, specific as follows:
Get pig urine samples liquid, regulate pH to be 7.0 by NaOH solution, filter and will filtrate be collected, obtaining analyte sample fluid;
Get CdTe solution described in 1.5ml respectively and described analyte sample fluid joins in the color comparison tube of 5ml, with the phosphate buffered solution constant volume of pH=7.4, shake up make it fully react rear molecular fluorescence photometer to detect the fluorescence intensity F obtaining system be 1141, testing conditions is: excitation wavelength is 365nm, excite and launch slit width and be 5nm, sweep velocity is 1200nm/min;
Contrast with the equation of linear regression of Stern-Volmer curve, can show that testing result is consistent with the fact not containing salbutamol in described negative pig urine samples liquid not containing salbutamol in described negative pig urine samples liquid.
Figure 1 shows that the TEM figure of described CdTe quantum, as can be seen from the figure, the pattern of described CdTe quantum is spherical, good dispersion, and particle diameter is 4.5nm and distributes homogeneous.
Figure 2 shows that the XRD figure of described CdTe quantum, as can be seen from the figure, diffraction peak is respectively: 25.76,42.16 and 48.36, corresponding to (111) of CdTe cubic system, (220), (311) three crystal faces, in order to contrast, body schalenblende CdTe (solid line) and CdS (dotted line) has been marked below XRD spectra, find that these three values are between CdTe and CdS, but be partial to CdTe crystal, thus illustrate that described CdTe quantum belongs to sphalerite cube crystalline phase.
Figure 3 shows that the fluorescence spectrum figure of CdTe quantum described in the present embodiment, as can be seen from the figure, the fluorescence property of described CdTe quantum is better, when selecting 365nm to excite, the maximum wavelength of its fluorescent emission is positioned at 550nm, and peak shape symmetry is good, and its fluorescence intensity is up to 7624.
Be illustrated in figure 4 the cancellation spectrum change figure of described CdTe quantum to variable concentrations salbutamol, in figure, the concentration of curve from top to bottom corresponding salbutamol increases successively, namely in figure, the concentration of the corresponding salbutamol of uppermost curve is minimum is 0, and the concentration of the corresponding salbutamol of nethermost curve is 2.10 × 10 to the maximum
-6mol/L, therefore, as seen from Figure 4, along with salbutamol concentration is increased to 2.10 × 10 from 0
-6mol/L, the fluorescence intensity of system drops to 50.10% of initial value gradually.
Embodiment 2
The present embodiment provides a kind of method utilizing CdTe quantum quantitatively to detect salbutamol in pig urine samples liquid, and detection method comprises the steps:
The preparation of (a) CdTe quantum, specific as follows:
(1) 0.12g tellurium powder and 0.0900g sodium borohydride is taken respectively, and add 2ml high purity water, rapid ParafilmTM seals, insert injection needle to communicate with the external world simultaneously, reaction 4h is carried out under ice-water bath and strong magnetic agitation condition, leave standstill 10min, obtain the NaHTe solution that pinkish is transparent;
(2) 0.1gCdCl is taken
22.5H
2o is dissolved in 200ml high purity water, then adds 100 μ L mercaptoacetic acid, forms milky suspension system;
(3) first 0.1molL is used
-1naOH solution regulates the pH of described suspension system to be 10, and logical high pure nitrogen 30min, then adds the described NaHTe solution that 210 μ L steps (1) prepare under nitrogen protection, controls Cd in solution
2+, HTe
-, mercaptoacetic acid mol ratio be 0.8:0.4:1.5, obtain the CdTe quantum presoma of brown;
(4) described CdTe quantum presoma is transferred in teflon-lined hydrothermal synthesis reaction still, is placed in 140 DEG C of baking ovens and heats 30min, through cooling, washing, centrifugally namely obtain described CdTe quantum.
B the CdTe quantum described in () utilization quantitatively detects salbutamol, specific as follows:
Get pig urine samples liquid, regulate pH to be 7.0 by NaOH solution, filter and will filtrate be collected, obtaining analyte sample fluid;
(2) the CdTe solution described in 1.5ml is got respectively and the analyte sample fluid described in step (1) joins in the color comparison tube of 5ml, with the phosphate buffered solution constant volume of pH=7.4, shake up make it fully react rear molecular fluorescence photometer to detect the fluorescence intensity F obtaining system be 1140, testing conditions is: excitation wavelength is 365nm, excite and launch slit width and be 5nm, sweep velocity is 1200nm/min;
Contrast with the equation of linear regression of Stern-Volmer curve, can show that the content of salbutamol in described pig urine samples liquid is < 0.042 × 10
-6mol/L.
Embodiment 3
The present embodiment provides a kind of method utilizing CdTe quantum quantitatively to detect salbutamol in pig urine samples liquid, and detection method comprises the steps:
The preparation of (a) CdTe quantum, specific as follows:
(1) 0.13g tellurium powder and 0.0700g sodium borohydride is taken respectively, and add 1.5ml high purity water, rapid ParafilmTM seals, insert injection needle to communicate with the external world simultaneously, reaction 4h is carried out under ice-water bath and strong magnetic agitation condition, leave standstill 10min, obtain the NaHTe solution that pinkish is transparent;
(2) 0.2gCdCl is taken
22.5H
2o is dissolved in 200ml high purity water, then adds 100 μ L mercaptoacetic acid, forms milky suspension system;
(3) first 0.1molL is used
-1naOH solution regulates the pH of described suspension system to be 11, and logical high pure nitrogen 30min, then adds the described NaHTe solution that 210 μ L steps (1) prepare under nitrogen protection, controls Cd in solution
2+, HTe
-, mercaptoacetic acid mol ratio be 1.0:0.5:2.5, obtain the CdTe quantum presoma of brown;
(4) described CdTe quantum presoma is transferred in teflon-lined hydrothermal synthesis reaction still, is placed in 150 DEG C of baking ovens and heats 10min, through cooling, washing, centrifugally namely obtain described CdTe quantum.
B the CdTe quantum described in () utilization quantitatively detects salbutamol, specific as follows:
Get pig urine samples liquid, regulate pH to be 7.0 by NaOH solution, filter and will filtrate be collected, obtaining analyte sample fluid;
(2) the CdTe solution described in 1.5ml is got respectively and the analyte sample fluid described in step (1) joins in the color comparison tube of 5ml, with the phosphate buffered solution constant volume of pH=7.4, shake up make it fully react rear molecular fluorescence photometer to detect the fluorescence intensity F obtaining system be 862.2, testing conditions is: excitation wavelength is 365nm, excite and launch slit width and be 5nm, sweep velocity is 1200nm/min;
Contrast with the equation of linear regression of Stern-Volmer curve, can show that the content of salbutamol in described positive pig urine samples liquid is 1.04 × 10
-7mol/L.
In order to verify degree of accuracy and the accuracy of detection method, adopt the using high performance liquid chromatography tandem mass spectrum technology of comparative maturity in prior art to measure the content of salbutamol in pig urine samples liquid, testing result is 1.04 × 10
-7mol/L, thus it is consistent with the result adopting using high performance liquid chromatography tandem mass spectrum technology to measure to show to adopt the content of salbutamol in the method for the invention detection pig urine samples liquid.
4, recovery of standard addition
The standard solution of salbutamol is joined in blank pig urine samples liquid (i.e. the negative sample liquid of pig urine), control spiked levels and be respectively 0.75 × 10
-7, 1.5 × 10
-7, 1.8 × 10
-7mol/L, test according to the method utilizing CdTe quantum quantitatively to detect salbutamol in pig urine samples liquid described in the embodiment of the present invention, 6 horizontal surveies are carried out under each spiked levels, average, scalar sum testing result is added according to actual, the recovery of standard addition calculating pig urine samples liquid is as shown in table 1, and the recovery of standard addition of sample liquid is 86.6%-95.8%.
The horizontal survey of table 1-mark-on sample liquid
| Add scalar (× 10 -7mol/L) | 0.75 | 1.5 | 1.8 |
| Practical measurement mean value | 0.65±0.08 | 1.34±0.18 | 1.72±0.22 |
| The recovery (%) | 86.7±0.06 | 89.3±0.27 | 95.9±0.12 |
Obviously, above-described embodiment is only for clearly example being described, and the restriction not to embodiment.For those of ordinary skill in the field, also can make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of extending out or variation be still among the protection domain of the invention.
Claims (8)
1., for a preparation method for the CdTe quantum of salbutamol detection, comprise the steps:
(1) take 0.12g-0.13g tellurium powder and 0.07g-0.09g sodium borohydride respectively, and add 1-2ml high purity water, under ice-water bath condition, carry out stirring reaction, obtain transparent NaHTe solution;
(2) 0.1-0.2gCdCl is taken
22.5H
2o is dissolved in 200ml high purity water, then adds 100 μ L mercaptoacetic acid, forms milky suspension system;
(3) first 0.1molL is used
-1naOH solution regulates the pH of described suspension system to be 10-12, pre-inflated with nitrogen 30min, then adds the NaHTe solution described in step (1) under nitrogen protection, control Cd
2+, HTe
-, mercaptoacetic acid mol ratio be 0.8-1.0:0.4-0.5:1.5-2.5, obtain the CdTe quantum presoma of brown;
(4) described CdTe quantum presoma is transferred in reactor, at 140-160 DEG C of heating 5-60min, through cooling, washing, centrifugally namely obtains described CdTe quantum.
2. utilize the CdTe quantum described in claim 1 quantitatively to detect a method for salbutamol, it comprises the steps:
A () makes Stern-Volmer curve:
Prepare the salbutamol standard working solution of a series of variable concentrations, and it moved to respectively in the color comparison tube of 5ml, in each described color comparison tube, all add 1.5ml concentration is 1.45 × 10
-3the CdTe solution of mol/L, with the phosphate buffered solution constant volume of pH=7.4, shakes up the fluorescence intensity F that rear molecular fluorescence photometer detects above-mentioned each individual system; Meanwhile, getting 1.5ml concentration is 1.45 × 10
-3the 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 the fluorescence intensity F of rear molecular fluorescence photometer detection system
0;
With salbutamol concentration for horizontal ordinate, with F
0/ F is ordinate, obtains the equation of linear regression of salbutamol to the Stern-Volmer curve of CdTe quantum fluorescent quenching;
B () is got the CdTe solution described in 1.5ml respectively and is joined in the color comparison tube of 5ml containing the sample liquid of salbutamol, with the phosphate buffered solution constant volume of pH=7.4, shake up and make it fully react rear molecular fluorescence photometer to detect and obtain the fluorescence intensity of system, contrast with the equation of linear regression of described Stern-Volmer curve, obtain the content of salbutamol in described sample liquid.
3. CdTe quantum according to claim 2 quantitatively detects the method for salbutamol, it is characterized in that, step (a) is with in step (b), and the testing conditions of described fluorescence intensity is: excitation wavelength is 365nm, excites and launch slit width to be 5nm.
4. the CdTe quantum according to Claims 2 or 3 quantitatively detects the method for salbutamol, it is characterized in that, the concentration of the standard working solution of described salbutamol is respectively 0.042 × 10
-6, 0.084 × 10
-6, 0.126 × 10
-6, 0.168 × 10
-6, 0.210 × 10
-6, 0.252 × 10
-6, 0.420 × 10
-6, 0.630 × 10
-6, 0.84 × 10
-6, 1.26 × 10
-6, 1.68 × 10
-6, 2.10 × 10
-6mol/L.
5. the CdTe quantum according to any one of claim 2-4 quantitatively detects the method for salbutamol, it is characterized in that, the equation of linear regression of described Stern-Volmer curve is divided into two parts, and the concentration range of described salbutamol is 0.042 × 10
-6-0.420 × 10
-6during mol/L, the equation of linear regression of described Stern-Volmer curve is F
0/ F=0.8428 × 10
6c+1.0434, linearly dependent coefficient is 0.976;
The concentration range of described salbutamol is 0.420 × 10
-6-2.10 × 10
-6during mol/L, the equation of linear regression of described Stern-Volmer curve is F
0/ F=0.1491 × 10
6c+1.3078, linearly dependent coefficient is 0.999.
6. the CdTe quantum according to any one of claim 2-5 quantitatively detects the method for salbutamol, it is characterized in that, the described sample liquid containing salbutamol is pig urine.
7. CdTe quantum according to claim 6 quantitatively detects the method for salbutamol, it is characterized in that, described pig urine is through following pre-service:
Get pig urine samples liquid, regulate pH to be 7.0 by NaOH solution, filter and will filtrate be collected, obtaining analyte sample fluid.
8. the application of CdTe quantum in salbutamol quantitatively detects that prepare of method according to claim 1.
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| CN106525800A (en) * | 2016-11-22 | 2017-03-22 | 无锡艾科瑞思产品设计与研究有限公司 | Quantitative detection method of salbutamol |
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| CN108152257A (en) * | 2017-12-12 | 2018-06-12 | 江西省农业科学院农产品质量安全与标准研究所 | A kind of method that Zilpaterol is measured using CdTe quantum |
| CN108037105B (en) * | 2017-12-12 | 2020-08-04 | 江西省农业科学院农产品质量安全与标准研究所 | Method for measuring zilpaterol by utilizing CdTe quantum dots |
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