A kind of nano fluorescent probe and its preparation method for rapid detection of hydrogen sulfide
A nano-fluorescent probe, fluorescent probe technology, applied in chemical instruments and methods, fluorescence/phosphorescence, color-changing fluorescent materials, etc., can solve the problem of not yet retrieved fluorescent nano-probes, and achieve high sensitivity, broad application prospects, good selective effect
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Embodiment 1
[0045] Preparation of fluorescent probes
[0046] 1. The preparation steps are as follows:
[0047] (1) Synthesis of metal chlorides: add thulium oxide (Tm 2 o 3 , 168 mg), distilled water (3 mL) and hydrochloric acid (3 mL) and heated until the powder was completely dissolved. After refluxing for 30 minutes, the mixture was cooled to room temperature. The solution was then transferred to a 10 mL volumetric flask and made up to 10 mL with distilled water. Thulium chloride solution was used in the next step.
[0048] Similarly, solutions of yttrium chloride, erbium chloride, and ytterbium chloride were prepared according to the protocol for thulium chloride.
[0049] (2)NaYF 4 : Yb, Tm @NaYF 4 : Synthesis of Yb, Er: synthesized by thermal decomposition; RECl containing Y, Yb and Tm 3 (1 mmol / L) (ratio=75%:25%:0.3%) was added to the four-necked flask, and then 1-octadecene (15 mL) and oleic acid (6 mL) were added to the above mixture. After nitrogen evacuation at room t...
Embodiment 2
[0057] Probe PAAO-UCNPs-EM1 and H 2 High resolution mass spectrum of the solution after S response
[0058] The preparation steps of the PAAO-UCNPs-EM1 probe solution and NaHS solution involved in this example are the same as in Example 1, and other specific steps are as follows: Add NaHS solution (100 μmol / L, 10 μL) to the probe solution prepared in Example 1 After reacting for 30 seconds, the reacted solution was diluted with distilled water, and its mass spectrum peak was measured with an ABI Mariner ESI-TOF spectrometer.
[0059] as attached figure 2 As shown, the peak (684.41224) of EM2 appears in the solution after the reaction, and this result shows that the probe solution and H 2 The mechanism of S response is that EM1 connected to the probe interacts with it and generates EM2.
Embodiment 3
[0061] The preparation steps of the PAAO-UCNPs-EM1 probe solution and NaHS solution involved in this embodiment are the same as in Example 1, and other specific steps are as follows: NaHS solutions (0-10 μmol / L) After reacting for 30 seconds, the reacted solution was irradiated with a 980nm laser (100mw) externally connected to the F97pro fluorescence spectrophotometer, and its fluorescence emission spectrum was obtained.
[0062] as attached image 3 As shown, we can see that with H 2 With the increase of S concentration, the fluorescence emission intensity of the reacted probe solution at 540nm and 660nm is increasing, and it is known from the calculation that the probe PAAO-UCNPs-EM1 has an effect on H 2 The detection limit of S is low, and the detection range can reach 0.01-0.13 μmol / L, which shows that the detection effect of the probe is good and the sensitivity is high.
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