Analysis method for simultaneous determination of 6 kinds of trace phenol environmental endocrine disrupting chemicals in solid environmental sample

A technology for endocrine disruptors and environmental samples, which is applied in the analysis field of simultaneous determination of 6 trace amounts of phenolic environmental endocrine disruptors in solid environmental samples, can solve the problem of not forming phenolic EDCs, etc., and achieves improved chromatographic peak type, precision Good accuracy and good reproducibility

Inactive Publication Date: 2015-11-25
SOUTHWEAT UNIV OF SCI & TECH
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  • Abstract
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Problems solved by technology

[0003] In the existing research, there is no uniform standard analysis method for phenolic EDCs in solid environmental samples, especially the simultaneous determination of six typical trace phenolic EDCs (octylphenol, cumenylphenol, The analysis method of nonylphenol, bisphenol A, nonylphenol dioxyethylene ether and nonylphenol monooxyethylene ether) is still blank

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  • Analysis method for simultaneous determination of 6 kinds of trace phenol environmental endocrine disrupting chemicals in solid environmental sample
  • Analysis method for simultaneous determination of 6 kinds of trace phenol environmental endocrine disrupting chemicals in solid environmental sample

Examples

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Embodiment 1

[0066] The collected river silt was dried in a vacuum freeze dryer at -55°C for 4 days, then taken out and returned to normal temperature for use. Weigh 4g of freeze-dried sludge and place it in a 100mL microwave extraction tank, add 10mL of BPA-d 16 After stirring the solution with a glass rod, put it in a cool and dry place and let it stand for 48 hours. Add 25mL of methanol, microwave extraction at 110°C for 20min, then cool to room temperature naturally in a ventilated place, and open the extraction tank. Rinse the extraction tank with methanol 3 times × 5mL / time, and the extract was filtered through absorbent cotton and collected into a 250mL flat-bottomed flask. The extract was concentrated to about 1 mL by a rotary evaporator, gently blown to near dryness with high-purity nitrogen, and then rinsed with 3 mL of cyclohexane / ethyl acetate mixed solvent (1:1, v / v) for three times to rinse the flat-bottomed flask. The solution was transferred to a gel permeation chromatogr...

Embodiment 2

[0068] Weigh the freeze-dried crucian carp sample, peel off the fish muscle, take 4g and put it in a 100mL extraction tank (crush the coarse particles with a mortar), and add 10mL of recovery indicator BPA-d 16 After stirring the solution with a glass rod, put it in a cool and dry place and let it stand for 48 hours. Add 25mL of methanol, microwave extraction at 110°C for 20min, then cool to room temperature naturally in a ventilated place, and open the extraction tank. Rinse the extraction tank with methanol 3 times × 5mL / time, and the extract was filtered through absorbent cotton and collected into a 250mL flat-bottomed flask. The extract was concentrated to about 0.5 mL by a rotary evaporator, blown gently with high-purity nitrogen until nearly dry, and then rinsed the flat-bottomed flask with 3 mL of cyclohexane / ethyl acetate mixed solvent (1:1, v / v) for three times. The washing solution was transferred to a sample tube purified by gel permeation chromatography, and the v...

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Abstract

The invention discloses an analysis method for simultaneous determination of 6 kinds of trace phenol environmental endocrine disrupting chemicals (EDCs) in a solid environmental sample. The method comprises the steps: carrying out microwave-assisted extraction and gel permeation chromatography purification and the like, after solid-phase extraction, concentrating with a rotary evaporimeter, then blowing to dry with moderate nitrogen, adding BSTFA and pyridine, carrying out trimethyl silylation treatment on hydroxyls of the phenol EDCs, and finally analyzing by using GC-MS. Through sample concentration, purification, derivatization and other processes, a chromatographic peak pattern is improved, the detection limit and the impurity interference are reduced, the purification effect is improved, and the instrument analysis accuracy and sensitivity are increased. The method simplifies the operations, has the advantages of high efficiency, energy saving, short phase separation time, not easy emulsification in the extraction process, no pollution, simple operations and the like, and can well suitable for analysis determination of 6 kinds of typical trace phenol EDCs in the solid environmental sample.

Description

technical field [0001] The invention relates to the field of environmental analytical chemistry, in particular to an analytical method for simultaneously determining six kinds of trace phenolic environmental endocrine disruptors in solid environmental samples. Background technique [0002] Phenolic EDCs mainly come from domestic sewage and industrial wastewater. After entering the water body, they are adsorbed by sediment or suspended particles, and the part dissolved in water can enter other systems with the flow of water body. Phenolic EDCs are widely distributed and may cause potential harm to the ecological environment and even human beings. [0003] In the existing research, there is no unified standard analysis method for phenolic EDCs in solid environmental samples, especially the simultaneous determination of six typical trace phenolic EDCs (octylphenol, cumenylphenol, The analytical methods for nonylphenol, bisphenol A, nonylphenol dioxyethylene ether and nonylphen...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06
Inventor 王彬王有志董发勤宗美荣黎明陈梦君谌书傅开彬罗毅
Owner SOUTHWEAT UNIV OF SCI & TECH
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