阅读说明：本技术 基于荧光分析选择性测定地表水样中2,4-二硝基酚的方法 (The method for selectively measuring 2,4- dinitrophenol dinitrophenolate in earth's surface water sample based on fluorescence analysis ) 是由 叶存玲 王远飞 孔欠欠 王全坤 王治科 范顺利 于 2019-08-26 设计创作，主要内容包括：本发明公开了一种基于荧光分析选择性测定地表水样中2,4-二硝基酚的方法,具体步骤为：取0.3mL AgNCs@CAZ和0.8mL、pH=9的BR缓冲溶液,加入待测地表水样,定容至4mL,在室温条件下充分混匀后反应50min,在激发波长368nm处测定混合体系的荧光强度,然后根据测得的荧光强度并结合线性方程计算得到待测地表水样中2,4-二硝基酚的浓度。本发明首先通过简单、快速的方法合成荧光强度高且稳定性好的AgNCs@CAZ,该AgNCs@CAZ能够对2,4-二硝基酚进行特异性响应,本发明建立的荧光分析法能快速高效、高选择性、高灵敏测定地表水样中的2,4-二硝基酚,具有潜在的应用前景。(The invention discloses one kind to be selectively measured 2 in earth's surface water sample based on fluorescence analysis, the method of 4- dinitrophenol dinitrophenolate, specific steps are as follows: take the BR buffer solution of 0.3mL AgNCs CAZ and 0.8mL, pH=9, earth's surface water sample to be measured is added, it is settled to 4mL, 50min is reacted after mixing well at room temperature, the fluorescence intensity of mixed system is measured at excitation wavelength 368nm, then the concentration of 2,4- dinitrophenol dinitrophenolate in earth's surface water sample to be measured is obtained according to the fluorescence intensity measured and in conjunction with linear equation calculation.The present invention synthesizes the AgNCs@CAZ that fluorescence intensity is high and stability is good by simple, quick method first, the AgNCs@CAZ can be to 2,4- dinitrophenol dinitrophenolate carries out specificly-response, the fluorescence analysis that the present invention establishes can rapidly and efficiently, it is highly selective, in Sensitive Determination earth's surface water sample 2,4- dinitrophenol dinitrophenolate has potential application prospect.)

1. the method for selectively measuring 2,4- dinitrophenol dinitrophenolate in earth's surface water sample based on fluorescence analysis, it is characterised in that specific steps Are as follows: the BR buffer solution for taking 0.3mL AgNCs CAZ and 0.8mL, pH=9 is added earth's surface water sample to be measured, 4mL is settled to, in room 50min is reacted after mixing well under the conditions of temperature, the fluorescence intensity of mixed system is measured at excitation wavelength 368nm, then basis The fluorescence intensity and the linear equation calculation of combination measured obtains the concentration of 2,4- dinitrophenol dinitrophenolate in earth's surface water sample to be measured；2,4- dinitro Base phenol linear concentration range is 0.05-15 μ g/mL, and linear equation is (F₀-F)/F=0.1378C_2,4-DNP- 0.0028, wherein F₀、F Respectively the fluorescent value before and after 2,4- dinitrophenol dinitrophenolate, coefficient R is added in mixed system at 368nm²=0.9959, repeat 12 It is 0.9% that secondary experiment measurement, which obtains RSD, and detection limit LOD is 0.027 μ g/mL；

The specific preparation process of the [email protected] is；Take 0.5mL, 10mM AgNO₃Solution is acutely stirring in collet beaker The lower cefotaxime CAZ solution that 4mL, 5mM is added is mixed, 10mL is settled to, 4h is persistently stirred to react under the conditions of being protected from light for 85 DEG C, is used Miniature syringe filter filtering, finally AgNCs CAZ obtained is kept in dark place in 4 DEG C spare.

2. the method according to claim 1 that 2,4- dinitrophenol dinitrophenolate in earth's surface water sample is selectively measured based on fluorescence analysis, It is characterized by: the [email protected] being capable of 2,4- in the presence of common phenolic compound in specificly-response aqueous solution Dinitrophenol dinitrophenolate, wherein common phenolic compound be 2- nitrophenols, 3- nitrophenols, para-aminophenol, m-aminophenol, to acetyl ammonia Base phenol, o-aminophenol, catechol or/and benzoic acid.

Technical field

The invention belongs to fluorescence analysis fields, and in particular to one kind selectively measures earth's surface water sample based on fluorescence analysis The method of middle 2,4- dinitrophenol dinitrophenolate.

Background technique

Metalfluorescent nano-cluster is ideal fluorescent nano material, and wherein silver nanoclusters are due to excellent fluorescence The features such as performance, preferable water-soluble, stability and biocompatibility, using relatively broad in numerous metal nanometre clusters.So And there is also the deficiencies more sensitive to environment for silver nanoclusters, deposit as cannot be stablized under high ionic strength and illumination condition To limit its further applying in fields such as environment measurings.

Summary of the invention

The technical problem to be solved by the present invention is to provide one kind rapidly and efficiently, selective high and high sensitivity based on fluorescence The method that analysis selectively measures 2,4- dinitrophenol dinitrophenolate in earth's surface water sample.

The present invention adopts the following technical scheme that one kind selectively measures ground based on fluorescence analysis to solve above-mentioned technical problem The method of 2,4- dinitrophenol dinitrophenolate in table water sample, it is characterised in that specific steps are as follows: take 0.3mL AgNCs CAZ and 0.8mL, pH=9 BR buffer solution, earth's surface water sample to be measured is added, is settled to 4mL, reacts 50min after mixing well at room temperature, swash The fluorescence intensity that mixed system is measured at wavelength 368nm is sent out, then according to the fluorescence intensity measured and in conjunction with linear equation calculation Obtain the concentration of 2,4- dinitrophenol dinitrophenolate in earth's surface water sample to be measured；2,4- dinitrophenol dinitrophenolate linear concentration ranges are 0.05-15 μ g/mL, Linear equation is (F₀-F)/F=0.1378C_2,4-DNP- 0.0028, wherein F₀, F be respectively that 2,4- is added in mixed system at 368nm Fluorescent value before and after dinitrophenol dinitrophenolate, coefficient R²=0.9959, being repeated 12 times experiment measurement and obtaining RSD is 0.9%, detection limit LOD is 0.027 μ g/mL；

The specific preparation process of the [email protected] is；Take 0.5mL, 10mM AgNO₃Solution is acutely stirring in collet beaker The lower cefotaxime CAZ solution that 4mL, 5mM is added is mixed, 10mL is settled to, 4h is persistently stirred to react under the conditions of being protected from light for 85 DEG C, is used Miniature syringe filter filtering, finally AgNCs CAZ obtained is kept in dark place in 4 DEG C spare.

Preferably, the [email protected] can be in the presence of common phenolic compound in specificly-response aqueous solution 2,4- dinitrophenol dinitrophenolates, wherein common phenolic compound be 2- nitrophenols, 3- nitrophenols, para-aminophenol, m-aminophenol, to second Acylamino- phenol, o-aminophenol, catechol or/and benzoic acid.

The present invention synthesizes the [email protected] that fluorescence intensity is high and stability is good by simple, quick method first, should [email protected] can carry out specificly-response to 2,4- dinitrophenol dinitrophenolate, the fluorescence analysis that the present invention establishes can rapidly and efficiently, it is high 2,4- dinitrophenol dinitrophenolate in selectivity, Sensitive Determination earth's surface water sample has potential application prospect.

Detailed description of the invention

Fig. 1 is influence of the pH to [email protected] fluorescence property.

Fig. 2 is influence of the sodium chloride concentration to [email protected] fluorescence property.

Fig. 3 is influence of the uv-exposure time to [email protected] fluorescence property.

Fig. 4 is the excitation and emission spectra of [email protected]

Fig. 5 is emission spectrum of the [email protected] under different excitation wavelengths.

Fig. 6 is [email protected] and cefotaxime (CAZ) infrared spectroscopy.

Fig. 7 is the selectivity and interference free performance of 2,4-DNP fluorescence analysis.

Specific embodiment

Above content of the invention is described in further details by the following examples, but this should not be interpreted as to this The range for inventing above-mentioned theme is only limitted to embodiment below, and all technologies realized based on above content of the present invention belong to this hair Bright range.