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A kind of method for detecting phenolic compounds in water

A technology for phenolic compounds and water samples, which is applied in the field of water pollution detection, can solve the problems of complex derivation operations, harsh reaction conditions, and low detection limits, and achieve the effects of improved analysis rate, simple method, and high accuracy

Active Publication Date: 2022-08-02
宁波市产品食品质量检验研究院(宁波市纤维检验所)
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, the research on phenolic compounds in water mostly focuses on the detection of a single type (such as phenol, chlorophenols, nitrophenols, etc.) or a small amount of multiple types of phenolic compounds. A common phenolic compound; Li Xiaoqing established a new method for the simultaneous detection of 6 phenolic compounds in water; Joaquindeng et al. used HPLC to detect 5 synthetic phenolic antioxidants in wastewater; Luo et al. used HPLC Combined with the fluorescence method to detect 12 kinds of phenolic compounds in water, although these methods have simple pretreatment, low detection limit and high sensitivity, they can only detect a small number of phenolic compounds at the same time
There are few reports on the detection of alkylphenols and bromophenols in water in current research, and most of the current detection methods for phenolic compounds require derivatization, but the derivation operation is more complicated, the reaction conditions are harsh, and the by-products of the reaction and excessive derivatization reagents may be derivatized. Separation and detection of interfering target compounds, etc.

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  • A kind of method for detecting phenolic compounds in water
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  • A kind of method for detecting phenolic compounds in water

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of standard solution

[0028] Using methanol as a solvent, the standard samples of alkylphenol, bromophenol and 10 kinds of nitrophenols were prepared into 10mL of 1g / L stock solution, and then the 1g / L stock solution was diluted with methanol to 100mg / L intermediate solution; Draw the intermediate solution at a ratio of 1:10 to prepare a mixed standard solution with the concentrations of the first type phenols and the second type phenols at 1 and 10 mg / L, respectively. The above stock solutions and intermediate solutions are stored at -10 °C. ,spare.

[0029] Accurately draw an appropriate amount of the 18 mixed standard solutions, and dilute them with methanol to obtain the concentration of the first type phenols are 0.50, 1.00, 5.00, 10.00, 20.00 μg / L, and the second type phenols are 5.00, 10.00, 50.00, 100.00 , 200.00μg / L mixed standard solution.

[0030] Wherein, the first type of phenolic substances are: Nonylphenol (Nonylphenol, NP), Bisphenol A...

Embodiment 2

[0042] Embodiment 2: a kind of method for detecting phenolic compounds in water

[0043] (1) Sample pretreatment: enrichment of phenolic compounds

[0044] Use hydrochloric acid to adjust the pH of the water sample to be tested to 3.0, activate the solid-phase extraction cartridge (OasisPRiME HLB 3cc) with 6 mL of methanol and 6 mL of ultrapure water, then add the water sample to be tested into the cartridge, adjust the solid-phase extractor to ensure that the water The sample flows through the column at a rate of 1 mL / min. Before the end of the sample loading, make sure that the small column does not dry during the whole process. After the sampling is completed, continue the negative pressure suction filtration for about 15 minutes, and finally add 10 mL of ethyl acetate to the column in turn, soak it. After 2min, rely on gravity elution, collect the eluate into a test tube, blow nitrogen to about 0.8mL, dilute to 1mL, pass through an organic membrane, and wait for testing. ...

Embodiment 3

[0048] Example 3: Optimization of Solid Phase Extraction Conditions

[0049] (1) Solid phase extraction cartridge selection

[0050] Select C18 column, SLH column, PSD column and HLB column respectively, and carry out pretreatment according to the corresponding experimental steps. The results obtained after measurement are shown in Table 2, figure 2 . Depend on figure 2 It can be seen that the recovery rate of phenolic compounds is the highest when the HLB column is used for solid phase extraction, so the HLB solid phase extraction column is selected.

[0051] Table 2 Effects of different cartridges on the recovery of phenolic compounds (n=3)

[0052]

[0053] (2) Selection of initial pH value

[0054] Adjust the pH of 3 parallel samples to 7, 6, 5, 4, 3, and 2 with hydrochloric acid respectively, and carry out pretreatment according to the corresponding experimental steps. The results obtained after the measurement are shown in Table 3, image 3 . Depend on image...

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Abstract

The invention discloses a method for detecting phenolic compounds in water, and belongs to the technical field of water pollution detection. The method is as follows: firstly, the pH of the water sample is adjusted to 2.5-3.5, and the solid phase extraction method is used for enrichment; then the phenolic compounds are quantitatively detected by gas chromatography tandem mass spectrometry; and the solid phase extraction conditions are: using HLB solid phase extraction method. The phase extraction cartridge uses ethyl acetate as the eluent; the phenolic compounds include alkylphenolic compounds, bromophenolic compounds and nitrophenolic compounds. The method established by the invention does not need derivatization, simplifies the pretreatment method, is simple in operation, has high accuracy and good repeatability, can simultaneously detect 18 kinds of phenolic compounds in complex water bodies, and the average recovery rate is 77.3-100.6%, which is relatively standard. The deviation was 3.1-7.4%, and the detection limit was 0.04-0.5 μg / L.

Description

technical field [0001] The invention relates to a method for detecting phenolic compounds in water, and belongs to the technical field of water pollution detection. Background technique [0002] With the rapid development of coking, oil refining, metallurgy, gas and other industries, the discharge of various phenol-containing wastewaters has increased accordingly, and phenolic compounds have begun to enter the public eye. The "Sodium Pentachlorophenate Poisoning" incident in Liangzi Lake of Hubei Province and the "Phenol Polluted Water Source" incident in Jiangsu Province, phenolic compounds are more and more popular among scholars due to their high toxicity, long-term accumulation, persistence, and potential carcinogenicity. wide attention. Phenol pollution in the environment mainly refers to the pollution of water bodies by phenolic compounds. As one of the most harmful and polluting industrial wastewaters in the world, phenol-containing wastewater is an important source...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/86
CPCG01N30/02G01N30/06G01N30/8675
Inventor 邢家溧毛玲燕李杨张书芬郑睿行应璐承海
Owner 宁波市产品食品质量检验研究院(宁波市纤维检验所)
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