CN106770124B - It is a kind of for detecting the fluorescent optical sensor and preparation method of zinc ion - Google Patents
It is a kind of for detecting the fluorescent optical sensor and preparation method of zinc ion Download PDFInfo
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- CN106770124B CN106770124B CN201710006224.7A CN201710006224A CN106770124B CN 106770124 B CN106770124 B CN 106770124B CN 201710006224 A CN201710006224 A CN 201710006224A CN 106770124 B CN106770124 B CN 106770124B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
Abstract
The present invention relates to a kind of fluorescent optical sensors and preparation method thereof for detecting zinc ion, belong to the fluorescence chemical sensor technical field of nanostructure.Nano silica is put into ethyl alcohol by the present invention, and 3- r-chloropropyl trimethoxyl silane is then added, and back flow reaction obtains product A；Product A is put into acetonitrile, indoles -3- acetaldehyde is added, back flow reaction obtains product B under nitrogen protection；Product B is put into methanol, sodium hydroxide and 2- hydroxy acetophenone is then added, back flow reaction obtains product C；Product C is put into methanol, sodium hydroxide and hydrogenperoxide steam generator is then added, reacts, be centrifugated up to target product under ice bath.The advantages of fluorescent optical sensor prepared by the present invention has preferable selectivity to zinc ion, and has detection limit low, fast response time.
Description
Technical field
The present invention relates to a kind of for detecting the fluorescent optical sensor and preparation method of zinc ion, belongs to field of sensing technologies.
Background technique
Zinc is one of main vital activity element, is played regulatory role to the immune function of human body, and for human body
Metabolism have a very important role.Human life activity be unable to do without zinc, but excessive zinc has human life activity
Tremendous influence.The main pollution source of zinc is the waste discharge of the departments such as plating, metallurgy, pigment and chemical industry.Therefore, zinc ion
Analysis detection be particularly important.The detection method of zinc mainly has atomic absorption spectrography (AAS), inductively coupled plasma atom hair
Penetrate spectroscopic methodology, fluorescent spectrometry etc..But these methods have, and pretreatment process is cumbersome, analysis time is long, instrument and cost of drugs are high
The deficiencies of.Therefore, it establishes simple, quick and high sensitivity zinc ion detection method and is increasingly becoming research emphasis.
Fluorescence analysis because have high sensitivity, the unique advantages such as easy to operate and have been a great concern.It is glimmering
Optical analysis has the characteristics that high sensitivity, selectivity is good, apparatus structure is relatively easy, cheap.Research in recent years
Show to construct sensor using nano material as substrate, can effectively improve the sensitivity and selectivity of sensor.Nanometer
Silica due to specific surface area stable, higher with property, nontoxic, high mechanical strength, it is cheap and easy to get, be easy to surface modification
The advantages that, it has been widely used in and has constructed fluorescent optical sensor, and shown good detection performance.
There is presently no the modified manometer silicon dioxide base fluorescence chemical sensors for being directed to zinc ion.
Summary of the invention
The present invention is directed to the deficiency of existing zinc ion detection technique, provides a kind of for detecting the fluorescent optical sensor of zinc ion
And preparation method thereof, which is used to detect the zinc ion in aqueous solution, has fast response time, detection limit
It is low, it is easy to operate, the characteristics of strong antijamming capability.
It is a kind of for detecting the fluorescent optical sensor of zinc ion, chemical structural formula are as follows:
。
Another object of the present invention is to provide the preparation methods of the fluorescent optical sensor for being used to detect zinc ion, specifically
Steps are as follows:
(1) nano silica is put into ethyl alcohol, 3- r-chloropropyl trimethoxyl silane is then added, in temperature 70 ~ 90
Back flow reaction 16 under the conditions of DEG C ~ for 24 hours, product A is obtained, CPTMS-SiO is labeled as2；
(2) the product A(CPTMS-SiO for obtaining step (1)2) be put into acetonitrile, indoles -3- acetaldehyde is added, in nitrogen
Protection, back flow reaction 16 under conditions of 50 ~ 70 DEG C of temperature ~ for 24 hours, obtain product B, are labeled as IA-SiO2；
(3) the product B(IA-SiO for obtaining step (2)2) be put into methanol, sodium hydroxide and 2- hydroxy benzenes is then added
Ethyl ketone, 8 ~ 12h of back flow reaction, obtains product C at room temperature, is labeled as HA-SiO2；
(4) the product C(HA-SiO for obtaining step (3)2) be put into methanol, sodium hydroxide and hydrogen peroxide is then added
Solution reacts 8 ~ 12h under condition of ice bath, is centrifugated up to target product HC-SiO2。
The partial size of nano silica is 10 ~ 20nm in the step (1)；
The liquid-solid ratio of 3- r-chloropropyl trimethoxyl silane and silica is 1:1 ~ 3:1, ethyl alcohol and two in the step (1)
The liquid-solid ratio of silica is 10:1 ~ 20:1；
2- indoles -3- acetaldehyde and CPTMS-SiO in the step (2)2Mass ratio be 2:1 ~ 4:1, acetonitrile and CPTMS-
SiO2Liquid-solid ratio be 10:1 ~ 20:1；
Sodium hydroxide and IA-SiO in the step (3)2Mass ratio be 2:1 ~ 4:1,2- hydroxy acetophenone and IA-SiO2
Mass ratio be 2:1 ~ 4:1, methanol and IA-SiO2Liquid-solid ratio be 10:1 ~ 20:1；
The preparation method of the fluorescence chemical sensor, sodium hydroxide and HA-SiO in step (4)2Mass ratio be 3:
1 ~ 5:1, the mass percent concentration of hydrogen peroxide is 25 ~ 35% in hydrogenperoxide steam generator, hydrogenperoxide steam generator and HA-SiO2's
Liquid-solid ratio is 8:1 ~ 12:1, methanol and HA-SiO2Liquid-solid ratio be 10:1 ~ 20:1.
The beneficial effects of the present invention are:
(1) present invention has the fluorescence chemical sensor HC-SiO of selective fluorescence response for zinc ion2, can be used as
The characteristics of detection contains aluminum ions new material, has fast response time, and detection limit is low, strong antijamming capability；
(2) method of the present invention preparation for detecting the fluorescent optical sensor of zinc ion, process is simple and easy, and yield is high；
(3) fluorescent optical sensor application method of the invention is easy to operate, low in cost.
Detailed description of the invention
Fig. 1 is the infrared spectroscopy of fluorescent optical sensor prepared by embodiment 1；
The fluorescent optical sensor and the fluorescent emission figure after various concentration zinc ion action that Fig. 2 is embodiment 1.
Specific embodiment
Invention is further described in detail With reference to embodiment, but protection scope of the present invention and unlimited
In the content.
Embodiment 1: a kind of for detecting the preparation method of the fluorescent optical sensor of zinc ion, the specific steps are as follows:
(1) nano silica (partial size of nano silica is 10nm) is put into ethyl alcohol, wherein ethyl alcohol and dioxy
The liquid-solid ratio mL:mg of SiClx is 10:1；Then 3- r-chloropropyl trimethoxyl silane is added, wherein 3- r-chloropropyl trimethoxyl silane
Liquid-solid ratio mL:mg with silica is 1:1, and the product A that back flow reaction 16h is obtained under the conditions of temperature 70 C is labeled as
CPTMS-SiO2；
(2) the product A(CPTMS-SiO for obtaining step (1)2) be put into acetonitrile, wherein acetonitrile and CPTMS-SiO2Liquid
Gu being 10:1 than mL:mg；Indoles -3- acetaldehyde is added, wherein 2- indoles -3- acetaldehyde and product A(CPTMS-SiO2) mass ratio
For 2:1, the product B that back flow reaction 16h is obtained under conditions of temperature 70 C, nitrogen protection is labeled as IA-SiO2；
(3) the product B(IA-SiO for obtaining step (2)2) be put into methanol, wherein methanol and product B(IA-SiO2)
Liquid-solid ratio mL:mg is 20:1；Then sodium hydroxide and 2- hydroxy acetophenone is added, wherein sodium hydroxide and product B(IA-SiO2)
Mass ratio be 2:1,2- hydroxy acetophenone and product B(IA-SiO2) mass ratio be 2:1, at room temperature back flow reaction
The product C that 8h is obtained is labeled as HA-SiO2；
(4) the product C(HA-SiO for obtaining step (3)2) be put into methanol, wherein methanol and product C(HA-SiO2)
Liquid-solid ratio mL:mg is 20:1；Then sodium hydroxide (sodium hydroxide and product C(HA-SiO is added2) mass ratio be 3:1) and mistake
Hydrogen peroxide solution, wherein the mass percent concentration of hydrogen peroxide is 25% in hydrogenperoxide steam generator, hydrogenperoxide steam generator and product
C(HA-SiO2) liquid-solid ratio mL:mg be 12:1, react 8h under condition of ice bath, be centrifugated up to fluorescent optical sensor (HC-
SiO2), the yield of fluorescent optical sensor is 94%.
The infrared spectroscopy for the fluorescent optical sensor that the present embodiment is prepared is shown in Fig. 1, sees from Fig. 1, and sample is 1110
cm-1The peak at place corresponds to the absorption peak of Si-O-Si, 1441cm-1The peak at place corresponds to the absorption peak of-NH, 1542cm-1The peak at place
The absorption peak of corresponding C=C, 1734cm-1The peak at place corresponds to the absorption peak of C=O, in 3430 cm-1The broad peak at place is corresponding to-O-H's
Absorption peak, to demonstrate the successful synthesis of fluorescence chemical sensor.
To the test experience of zinc ion: by the fluorescent optical sensor HC-SiO of preparation2It is dissolved in acetonitrile solvent, is configured to dense
Degree is the HC-SiO of 0.3g/L2Acetonitrile solution, then compound concentration is 2 × 10 respectively-5The aluminium of mol/L, calcium, chromium, manganese, cobalt,
Copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion, respectively by the HC-SiO of 1.5mL2Acetonitrile it is molten
The aluminium of liquid and 1.5mL, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion add
Enter into sample bottle, irradiated in the UV lamp after shaking up, wherein aluminium, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, cobalt
Or the acetonitrile solion of lead ion does not have color change, and the acetonitrile solion containing zinc ion becomes blue from colourless,
The sensor and zinc ion can reach within 2 minutes in conjunction with balance, have quick binding kinetics.
In addition various concentration (1 × 10 is prepared-9~1×10-5M zinc ion acetonitrile solution) analyzes HC-SiO2To different dense
The fluorescence spectrum of the zinc ion of degree, the results showed that the sensor fluorescence intensity enhances, detection limit with the increase of zinc ion concentration
About 1 × 10-9M；Fig. 2 is by the change curve for the fluorescence spectrum surveyed when the zinc ion action of fluorescent optical sensor and various concentration.
Embodiment 2: a kind of for detecting the preparation method of the fluorescent optical sensor of zinc ion, the specific steps are as follows:
(1) nano silica (partial size of nano silica is 12nm) is put into ethyl alcohol, wherein ethyl alcohol and dioxy
The liquid-solid ratio mL:mg of SiClx is 15:1；Then 3- r-chloropropyl trimethoxyl silane is added, wherein 3- r-chloropropyl trimethoxyl silane
Liquid-solid ratio mL:mg with silica is 2:1, and the product A that back flow reaction 18h is obtained under the conditions of 80 DEG C of temperature is labeled as
CPTMS-SiO2；
(2) the product A(CPTMS-SiO for obtaining step (1)2) be put into acetonitrile, wherein acetonitrile and CPTMS-SiO2Liquid
Gu being 15:1 than mL:mg；Indoles -3- acetaldehyde is added, wherein 2- indoles -3- acetaldehyde and product A(CPTMS-SiO2) mass ratio
For 3:1, the product B that back flow reaction 18h is obtained under conditions of 65 DEG C of temperature, nitrogen protection is labeled as IA-SiO2；
(3) the product B(IA-SiO for obtaining step (2)2) be put into methanol, wherein methanol and product B(IA-SiO2)
Liquid-solid ratio mL:mg is 15:1；Then sodium hydroxide and 2- hydroxy acetophenone is added, wherein sodium hydroxide and product B(IA-SiO2)
Mass ratio be 3:1,2- hydroxy acetophenone and product B(IA-SiO2) mass ratio be 3:1, at room temperature back flow reaction
The product C that 9h is obtained is labeled as HA-SiO2；
(4) the product C(HA-SiO for obtaining step (3)2) be put into methanol, wherein methanol and product C(HA-SiO2)
Liquid-solid ratio mL:mg is 15:1；Then sodium hydroxide (sodium hydroxide and product C(HA-SiO is added2) mass ratio be 4:1) and mistake
Hydrogen peroxide solution, wherein the mass percent concentration of hydrogen peroxide is 30% in hydrogenperoxide steam generator, hydrogenperoxide steam generator and product
C(HA-SiO2) liquid-solid ratio mL:mg be 10:1, react 9h under condition of ice bath, be centrifugated up to fluorescent optical sensor (HC-
SiO2), the yield of fluorescent optical sensor is 95%.
To the test experience of zinc ion: by the fluorescent optical sensor HC-SiO of preparation2It is dissolved in acetonitrile solvent, is configured to dense
Degree is the HC-SiO of 0.3g/L2Acetonitrile solution, then compound concentration is 2 × 10 respectively-5The aluminium of mol/L, calcium, chromium, manganese, cobalt,
Copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion, respectively by the HC-SiO of 1.5mL2Acetonitrile it is molten
The aluminium of liquid and 1.5mL, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion add
Enter into sample bottle, irradiated in the UV lamp after shaking up, wherein aluminium, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, cobalt
Or the acetonitrile solion of lead ion does not have color change, and the acetonitrile solion containing zinc ion becomes blue from colourless,
The sensor and zinc ion can reach within 2 minutes in conjunction with balance, have quick binding kinetics.
In addition various concentration (1 × 10 is prepared-9~1×10-5Mol/L zinc ion acetonitrile solution) analyzes HC-SiO2To not
With the fluorescence spectrum of the zinc ion of concentration, the results showed that the sensor fluorescence intensity enhances with the increase of zinc ion concentration, inspection
Rising limit is about 1 × 10-9 mol/。
Embodiment 3: a kind of for detecting the preparation method of the fluorescent optical sensor of zinc ion, the specific steps are as follows:
(1) nano silica (partial size of nano silica is 16nm) is put into ethyl alcohol, wherein ethyl alcohol and dioxy
The liquid-solid ratio mL:mg of SiClx is 20:1；Then 3- r-chloropropyl trimethoxyl silane is added, wherein 3- r-chloropropyl trimethoxyl silane
Liquid-solid ratio mL:mg with silica is 3:1, and the product A that back flow reaction 22h is obtained under the conditions of 85 DEG C of temperature is labeled as
CPTMS-SiO2；
(2) the product A(CPTMS-SiO for obtaining step (1)2) be put into acetonitrile, wherein acetonitrile and CPTMS-SiO2Liquid
Gu being 18:1 than mL:mg；Indoles -3- acetaldehyde is added, wherein 2- indoles -3- acetaldehyde and product A(CPTMS-SiO2) mass ratio
For 3:1, the product B that back flow reaction 22h is obtained under conditions of temperature 60 C, nitrogen protection is labeled as IA-SiO2；
(3) the product B(IA-SiO for obtaining step (2)2) be put into methanol, wherein methanol and product B(IA-SiO2)
Liquid-solid ratio mL:mg is 17:1；Then sodium hydroxide and 2- hydroxy acetophenone is added, wherein sodium hydroxide and product B(IA-SiO2)
Mass ratio be 3:1,2- hydroxy acetophenone and product B(IA-SiO2) mass ratio be 4:1, at room temperature back flow reaction
The product C that 11h is obtained is labeled as HA-SiO2；
(4) the product C(HA-SiO for obtaining step (3)2) be put into methanol, wherein methanol and product C(HA-SiO2)
Liquid-solid ratio mL:mg is 12:1；Then sodium hydroxide (sodium hydroxide and product C(HA-SiO is added2) mass ratio be 5:1) and mistake
Hydrogen peroxide solution, wherein the mass percent concentration of hydrogen peroxide is 28% in hydrogenperoxide steam generator, hydrogenperoxide steam generator and product
C(HA-SiO2) liquid-solid ratio mL:mg be 11:1, react 11h under condition of ice bath, be centrifugated up to fluorescent optical sensor (HC-
SiO2).The yield of fluorescent optical sensor is 96%.
To the test experience of zinc ion: by the fluorescent optical sensor HC-SiO of preparation2It is dissolved in acetonitrile solvent, is configured to dense
Degree is the HC-SiO of 0.3g/L2Acetonitrile solution, then compound concentration is 2 × 10 respectively-5The aluminium of mol/, calcium, chromium, manganese, cobalt,
Copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion, respectively by the HC-SiO of 1.5mL2Acetonitrile it is molten
The aluminium of liquid and 1.5mL, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion add
Enter into sample bottle, irradiated in the UV lamp after shaking up, wherein aluminium, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, cobalt
Or the acetonitrile solion of lead ion does not have color change, and the acetonitrile solion containing zinc ion becomes blue from colourless；
The sensor and zinc ion can reach within 2 minutes in conjunction with balance, have quick binding kinetics.
In addition various concentration (1 × 10 is prepared-9~1×10-5Mol/L zinc ion acetonitrile solution) analyzes HC-SiO2To not
With the fluorescence spectrum of the zinc ion of concentration, the results showed that the sensor fluorescence intensity enhances with the increase of zinc ion concentration, inspection
Rising limit is about 1 × 10-9 mol/L。
Embodiment 4: a kind of for detecting the preparation method of the fluorescent optical sensor of zinc ion, the specific steps are as follows:
(1) nano silica (partial size of nano silica is 20nm) is put into ethyl alcohol, wherein ethyl alcohol and dioxy
The liquid-solid ratio mL:mg of SiClx is 20:1；Then 3- r-chloropropyl trimethoxyl silane is added, wherein 3- r-chloropropyl trimethoxyl silane
Liquid-solid ratio mL:mg with silica is 3:1, and the product A that back flow reaction obtains for 24 hours under the conditions of 90 DEG C of temperature is labeled as
CPTMS-SiO2；
(2) the product A(CPTMS-SiO for obtaining step (1)2) be put into acetonitrile, wherein acetonitrile and CPTMS-SiO2Liquid
Gu being 20:1 than mL:mg；Indoles -3- acetaldehyde is added, wherein 2- indoles -3- acetaldehyde and product A(CPTMS-SiO2) mass ratio
For 4:1, the product B that back flow reaction obtains for 24 hours under conditions of temperature 50 C, nitrogen protection is labeled as IA-SiO2；
(3) the product B(IA-SiO for obtaining step (2)2) be put into methanol, wherein methanol and product B(IA-SiO2)
Liquid-solid ratio mL:mg is 20:1；Then sodium hydroxide and 2- hydroxy acetophenone is added, wherein sodium hydroxide and product B(IA-SiO2)
Mass ratio be 4:1,2- hydroxy acetophenone and product B(IA-SiO2) mass ratio be 4:1, at room temperature back flow reaction
The product C that 12h is obtained is labeled as HA-SiO2；
(4) the product C(HA-SiO for obtaining step (3)2) be put into methanol, wherein methanol and product C(HA-SiO2)
Liquid-solid ratio mL:mg is 10:1；Then sodium hydroxide (sodium hydroxide and product C(HA-SiO is added2) mass ratio be 5:1) and mistake
Hydrogen peroxide solution, wherein the mass percent concentration of hydrogen peroxide is 35% in hydrogenperoxide steam generator, hydrogenperoxide steam generator and product
C(HA-SiO2) liquid-solid ratio mL:mg be 8:1, react 12h under condition of ice bath, be centrifugated up to fluorescent optical sensor (HC-
SiO2), the yield of fluorescent optical sensor is 95%.
To the test experience of zinc ion: by the fluorescent optical sensor HC-SiO of preparation2It is dissolved in acetonitrile solvent, is configured to dense
Degree is the HC-SiO of 0.3g/L2Acetonitrile solution, then compound concentration is 2 × 10 respectively-5The aluminium of mol/L, calcium, chromium, manganese, cobalt,
Copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion, respectively by the HC-SiO of 1.5mL2Acetonitrile it is molten
The aluminium of liquid and 1.5mL, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, zinc, cobalt or lead ion acetonitrile solion add
Enter into sample bottle, irradiated in the UV lamp after shaking up, wherein aluminium, calcium, chromium, manganese, cobalt, copper, aluminium, iron, nickel, magnesium, manganese, sodium, cobalt
Or the acetonitrile solion of lead ion does not have color change, and the acetonitrile solion containing zinc ion becomes blue from colourless,
The sensor and zinc ion can reach within 2 minutes in conjunction with balance, have quick binding kinetics.
In addition various concentration (1 × 10 is prepared-9~1×10-5Mol/L zinc ion acetonitrile solution) analyzes HC-SiO2To not
With the fluorescence spectrum of the zinc ion of concentration, the results showed that the sensor fluorescence intensity enhances with the increase of zinc ion concentration, inspection
Rising limit is about 1 × 10-9 mol/L。
Claims (14)
1. a kind of for detecting the fluorescent optical sensor of zinc ion, which is characterized in that its chemical structural formula are as follows:
。
2. for detecting the preparation method of the fluorescent optical sensor of zinc ion described in claim 1, which is characterized in that specific steps are such as
Under:
(1) nano silica is put into ethyl alcohol, 3- r-chloropropyl trimethoxyl silane is then added, in 70 ~ 90 DEG C of items of temperature
Back flow reaction 16 under part ~ for 24 hours, obtain product A；
(2) the product A that step (1) obtains is put into acetonitrile, indoles -3- acetaldehyde is added, at 50 ~ 70 DEG C of nitrogen protection, temperature
Under conditions of back flow reaction 16 ~ for 24 hours, obtain product B；
(3) the product B that step (2) obtains is put into methanol, sodium hydroxide and 2- hydroxy acetophenone is then added, in room temperature item
8 ~ 12h of back flow reaction under part obtains product C；
(4) the product C that step (3) obtains is put into methanol, sodium hydroxide and hydrogenperoxide steam generator is then added, in ice bath item
8 ~ 12h is reacted under part, is centrifugated up to target product.
3. according to claim 2 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(1) partial size of nano silica is 10 ~ 20nm in.
4. according to claim 2 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(1) the liquid-solid ratio mL:mg of ethyl alcohol and nano silica is 10:1 ~ 20:1 in.
5. according to claim 4 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(1) 3- r-chloropropyl trimethoxyl silane and the liquid-solid ratio mL:mg of nano silica are 1:1 ~ 3:1 in.
6. according to claim 2 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(2) the liquid-solid ratio mL:mg of acetonitrile and product A are 10:1 ~ 20:1 in.
7. according to claim 6 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(2) mass ratio of indoles -3- acetaldehyde and product A are 2:1 ~ 4:1 in.
8. according to claim 2 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(3) the liquid-solid ratio mL:mg of methanol and product B are 10:1 ~ 20:1 in.
9. according to claim 8 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(3) mass ratio of sodium hydroxide and product B are 2:1 ~ 4:1 in.
10. according to claim 9 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(3) mass ratio of 2- hydroxy acetophenone and product B are 2:1 ~ 4:1 in.
11. according to claim 2 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(4) the liquid-solid ratio mL:mg of methanol and product C are 10:1 ~ 20:1 in.
12. according to claim 11 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(4) mass ratio of sodium hydroxide and product C are 3:1 ~ 5:1 in.
13. according to claim 2 for detecting the preparation method of the fluorescent optical sensor of zinc ion, it is characterised in that: step
(4) the mass percent concentration of hydrogen peroxide is 25 ~ 35% in hydrogenperoxide steam generator in.
14. 3 is described for detecting the preparation method of the fluorescent optical sensor of zinc ion according to claim 1, it is characterised in that: step
(4) liquid-solid ratio of hydrogenperoxide steam generator and product C are 8:1 ~ 12:1 in.
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|---|---|---|---|---|
| CN102735662A (en) * | 2012-07-19 | 2012-10-17 | 贵州大学 | High sensitivity and high selectivity fluorescence emission spectrum analysis method for zinc ions |
| CN103487416A (en) * | 2013-03-06 | 2014-01-01 | 中北大学 | Fluorescent sensor for detecting zinc ions based on asymmetrical porphyrin fluorescence ratio |
| CN104004513A (en) * | 2014-06-03 | 2014-08-27 | 兰州大学 | Fluorescence molecular probe for detecting zinc ions and preparation method thereof |
| CN104059386A (en) * | 2014-06-18 | 2014-09-24 | 东华大学 | Functional active dye complexing with zinc ions and preparation method and application thereof |
| CN104237188A (en) * | 2014-09-26 | 2014-12-24 | 东北师范大学 | Fluorescent probe for simply and quickly detecting zinc ions |
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2017
- 2017-01-05 CN CN201710006224.7A patent/CN106770124B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102735662A (en) * | 2012-07-19 | 2012-10-17 | 贵州大学 | High sensitivity and high selectivity fluorescence emission spectrum analysis method for zinc ions |
| CN103487416A (en) * | 2013-03-06 | 2014-01-01 | 中北大学 | Fluorescent sensor for detecting zinc ions based on asymmetrical porphyrin fluorescence ratio |
| CN104004513A (en) * | 2014-06-03 | 2014-08-27 | 兰州大学 | Fluorescence molecular probe for detecting zinc ions and preparation method thereof |
| CN104059386A (en) * | 2014-06-18 | 2014-09-24 | 东华大学 | Functional active dye complexing with zinc ions and preparation method and application thereof |
| CN104237188A (en) * | 2014-09-26 | 2014-12-24 | 东北师范大学 | Fluorescent probe for simply and quickly detecting zinc ions |
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