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Detection method of bisphenol-a in water environment based on diazo coupling reaction

A technology of coupling reaction and detection method, which is applied in the field of fluorescence and spectroscopic methods, can solve the problems of weak detection sensitivity of bisphenol A fluorescence signal intensity, bisphenol A synchronous fluorescence spectrum band narrowing, etc., to achieve convenient and fast reaction , detection sensitivity improvement, the effect of improving sensitivity

Active Publication Date: 2019-03-01
CHANGZHOU INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Compared with the conventional fluorescence analysis method, the simultaneous fluorescence spectrum band of bisphenol A is narrowed, and the interference of phenol and the like is avoided, but the detection sensitivity of this method is still limited by the weak fluorescence signal intensity of bisphenol A itself

Method used

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  • Detection method of bisphenol-a in water environment based on diazo coupling reaction
  • Detection method of bisphenol-a in water environment based on diazo coupling reaction

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] ① Accurately weigh 10.0 mg of bisphenol A, then add 0.5 mL of absolute ethanol to dissolve, add water to make up volume in a 100.0 mL brown volumetric flask, and prepare a 0.1 mg / mL bisphenol A stock solution. Dilute gradually with this stock solution to prepare a series of standard solutions of bisphenol A with different concentrations.

[0034] ② Use the coupling product λ em 305nm fluorescence signal optimization experimental conditions: discuss the influence of the amount of sodium nitrite, diazotization reaction time, acidity of coupling reaction, amount of coupling agent, coupling reaction time and coupling reaction temperature. The best experimental conditions for the fluorescence method are: acidity 0.01mol / L, diazotization time 5min, diazotization temperature 0°C, clenbuterol hydrochloride concentration 3.0mg / L, sodium nitrite 4.0mg / L , the concentration of ammonia water is 160.0mg / L.

[0035] ③Under the optimized experimental conditions, the linear range of ...

Embodiment 2

[0037] ① Accurately weigh 10.0mg sample processing: cut the plastic bottle of beverage or bottled water to 0.5cm*0.5cm fragments, weigh 1.000g of the fragments into an iodine bottle, add 50ml of secondary purified water, and put it in a water bath at 70°C Heating at constant temperature for 90min, cooling to room temperature, taking a certain amount of solution for measurement.

[0038] ② same as embodiment one ②.

[0039] ③ For ①, three parallel samples were made respectively, and the parallel measurement was performed three times, and the standard addition method was used for determination. The recovery rate is between 94.5% and 103.6%, meeting the requirements.

Embodiment 3

[0041] ① same as embodiment one ①.

[0042] ②Using the visible absorption of the coupling product at 410nm to optimize the experimental conditions: discuss the effects of the amount of sodium nitrite, the reaction time of diazotization, the acidity of the coupling reaction, the amount of coupling agent, the time of the coupling reaction and the temperature of the coupling reaction. The optimum experimental condition of spectrophotometry is, acidity, diazotization time, diazotization temperature are identical with embodiment one, and the concentration of clenbuterol hydrochloride is 16mg / L, and the concentration of sodium nitrite is 12mg / L, ammoniacal liquor The concentration is 200mg / L.

[0043] ③The linear range of bisphenol A determined by photometric method is 0.24mg / L~8.4mg / L, and the correlation coefficient is 0.9955. The relative standard deviation of 11 parallel determinations was 0.22%, and the reproducibility was good. The results were satisfactory, and there was no...

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Abstract

The invention discloses a method for detecting bisphenol A in a water environment on the basis of an azo coupling reaction. The method comprises the following steps: 1, clenbuterol hydrochloride is added to a sodium nitrite solution under an acidic condition for diazotization; 2, bisphenol A with different concentrations is added, dilute ammonia water is added, and secondary water is added for dilution; 3, the reaction liquid in the step 2 has a visible absorption peak at 410 nm; bisphenol A is detected with a spectrophotometric method; 4, the reaction liquid in the step 2 has strong fluorescence emission at 305 nm, and the fluorescence signals are enhanced 3.2 times than those of bisphenol A with the same concentration. With adoption of the method, the absorbance and the fluorescence signals are enhanced multiple times than those of bisphenol A with the same concentration, and the sensitivity of a fluorescence method and the spectrophotometric method for detecting bisphenol A is improved; the method is simple, fast and good in selectivity, can be used for detecting bisphenol A in the water environment and avoids use of an organic solvent.

Description

technical field [0001] The invention relates to a method for detecting bisphenol A, an environmental endocrine disrupting substance, in particular to the application of fluorescence and spectroscopic methods, and belongs to the technical field of analysis and detection. Background technique [0002] In recent years, epidemiological studies have found that the incidence of hormonal diseases (such as: breast cancer, ovarian cancer, prostate cancer and testicular cancer) has increased significantly. Scientists have confirmed that the occurrence of reproductive endocrine-related tumors may be related to the presence of endocrine disruptors in the external environment. Environmental endocrine disrupting substances refer to any exogenous substances that can cause endocrine dysfunction in organisms or their offspring. Such substances widely exist in rivers, soil, atmosphere and agricultural products. They can enter the body through food, water, air, etc., and directly or indirect...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/33G01N21/64
CPCG01N21/33G01N21/643G01N2021/1734
Inventor 壮亚峰刘宝亮陈建欣
Owner CHANGZHOU INST OF TECH
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