Efficient liquid phase chromatographic fluorescence detection method for measuring concentration of perfluorooctanoic acid in landfill leachate

A technology of high-performance liquid chromatography and landfill leachate, which is applied in the field of high-performance liquid chromatography fluorescence detection method for determining the concentration of perfluorooctanoic acid in landfill leachate, can solve the problems of expensive equipment, high measurement cost, and low detection limit, and achieve The effect of improving detection sensitivity, long retention time, and increasing accuracy

Active Publication Date: 2018-12-14
CHONGQING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Commonly used PFOA detection methods have disadvantages such as high detection limit, expensive equipment, high measurement cost or cumbersome operation steps.
High-performance liquid chromatography / fluorescence detector (HPLC-FLD) method has high sensitivity and low detection limit, but PFOA does not have fluorescence activity. At present, there are few researches on HPLC-FLD methods related to PFOA at home and abroad, and there are existing fluorescence derivatives. The agent preparation process is complicated and the cost is high

Method used

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  • Efficient liquid phase chromatographic fluorescence detection method for measuring concentration of perfluorooctanoic acid in landfill leachate
  • Efficient liquid phase chromatographic fluorescence detection method for measuring concentration of perfluorooctanoic acid in landfill leachate
  • Efficient liquid phase chromatographic fluorescence detection method for measuring concentration of perfluorooctanoic acid in landfill leachate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Preparation of standard solution

[0037] Accurately weigh 10 mg of PFOA standard substance, dissolve it in 100 mL of acetonitrile, prepare a standard solution with a concentration of 100 mg / L, put it in a polyethylene bottle, and store it in a refrigerator below 4 °C.

[0038] Preparation of working curve samples: Take an appropriate amount of 100mg / L standard solution and dilute it with acetonitrile solution to 0.001, 0.002, 0.004, 0.006, 0.008, 0.01, 0.02, 0.04, 0.06, 0.08, 0.1, 0.2, 0.4, 0.6, 0.8, 1mg / LPFOA acetonitrile solution, mix 10mL with 1mL, 5mg / mL 3-bromoacetylcoumarin acetone solution, add 50mg tetrabutylammonium bromide, react in a constant temperature water bath at 70°C for 150min, and store in a container below 4°C The refrigerator is waiting to be tested on the machine.

[0039] (2) Setting of detection conditions

[0040] The chromatographic column Zorbax Eclipse Plus C18 is used, the specification is 4.6mmx150mm, 3.5μm; the detection wavelength...

Embodiment 2

[0071] Limit of detection and limit of quantitation experiments

[0072] Under the optimal chromatographic conditions and derivation conditions in Example 1, the standard solution of 0.01 mg / L was taken in parallel for 6 times of concentration to carry out derivation reaction, and the reaction fluorescent derivative was measured, and the experimental results were as shown in Table 3. The standard deviation (Sb) of the peak area, multiplied by 3 times the signal-to-noise ratio, and then divided by the slope (S) of the corresponding working curve, the minimum detection concentration (Limitofdetection, LOD) of the method is 0.007mg / L. The formula for calculating the detection limit of the method is shown in the following formula.

[0073]

[0074] In the formula: Pi—the peak area value of the PFOA-derived solution in a single test; P—the average value of the peak area, n: the number of tests; S—the slope of the working curve; 3—the signal-to-noise ratio.

[0075] Take 10 time...

Embodiment 3

[0079] Precision and recovery experiments

[0080] Under the optimal chromatographic conditions and derivatization conditions in Example 1, 0.05mg / L and 0.5mg / L PFOA acetonitrile solutions were reacted with 1mL and 5mg / mL3-BrAC acetone solutions in parallel for 6 times, and the derivatization solution after reaction was taken Measure, when the PFOA concentration is 0.05mg / L, the recovery rate is 86%~94%, the result relative standard deviation is 3.4%, when the PFOA concentration is 0.5mg / L, the recovery rate is 92.2%~95.8%, the result The relative standard deviation is 1.64%. The experimental results are shown in Table 4.

[0081] Table 4 Test method precision and recovery test

[0082]

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Abstract

The invention discloses an efficient liquid phase chromatographic fluorescence detection method for measuring concentration of perfluorooctanoic acid in a landfill leachate. The method comprises the following steps of (1) carrying out pretreatment on a leachate sample with a certain volume to obtain a solution A; (2) performing constant volume of 10mL of the solution A obtained in the step (1), then adding 1mL and 5mg / mL of derivating agent acetone solution, and next, carrying out a catalytic reaction for 150min in a constant-temperature water bath at the temperature of 70 DEG C to obtain a fluorescent derivative solution; and (3) taking 1 mL of the fluorescent derivative solution, taking Zorbax Eclicpse Plus C18 as a chromatographic column, and taking acetonitrile-water as a flowing phase, performing machine measuring, recording the peak area, obtaining the concentration of perfluorooctanoic acid in the step (2) according to a calculation formula, and next, indirectly calculating theconcentration of perfluorooctanoic acid in the landfill leachate. The method has the advantages of being high in sensitivity, low in detection limit, relatively low in derivatization agent cost, simple in method and the like.

Description

technical field [0001] The invention relates to a detection method for perfluorooctanoic acid, in particular to a high performance liquid chromatography fluorescence detection method for determining the concentration of perfluorooctanoic acid in landfill leachate Background technique [0002] Perfluorooctanoic acid (PFOA) is a new type of organic pollutant, which is difficult to degrade from the environment. It can be absorbed by the human body through ingestion, inhalation, skin contact, etc., causing the proliferation of peroxisomes in the human body to affect energy transfer and damage cell membranes. Induce cancer, hepatomegaly and other diseases. Therefore, it brings great potential risks to environmental ecology and human health, and has attracted widespread attention in recent years. Due to the low concentration of PFOA in environmental samples (by ng / L or μg / L) and the ultraviolet activity of PFOA The detection method of PFOA has been one of the research hotspots al...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02
Inventor 曾晓岚黄永周丁文川刘杰孙现红杨占强马志伟
Owner CHONGQING UNIV
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