Method for detecting estrogen, nonyl phenol, octyl phenol and bisphenol A in water body sediment together

A sediment and estrogen technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of the existence of traces of estrogen and the difficulty of pretreatment technology, and achieve high sensitivity and accuracy, fast extraction speed, and purification good effect

Inactive Publication Date: 2011-09-14
BEIJING NORMAL UNIVERSITY
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Problems solved by technology

[0006] The purpose of the present invention is to solve the problems such as the complex matrix of sediment samples, the existence of trace amounts of estrogen in sediments, and the difficulty of pretreatment technology. It is proposed to develop a high recovery, high sensitivity, accurate and fast analysis technology to realize Quantitative determination of estrogen, nonylphenol, octylphenol and bisphenol A in biological samples

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  • Method for detecting estrogen, nonyl phenol, octyl phenol and bisphenol A in water body sediment together
  • Method for detecting estrogen, nonyl phenol, octyl phenol and bisphenol A in water body sediment together
  • Method for detecting estrogen, nonyl phenol, octyl phenol and bisphenol A in water body sediment together

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[0032] The technical solutions of the present invention will be further described below in conjunction with examples and accompanying drawings.

[0033] (1) Sediment sample pretreatment

[0034]The collected sediment samples were first freeze-dried. Take 5g of the freeze-dried sample and perform fast solvent extraction with 60ml of acetone. For the fast solvent extraction method adopted, the selected temperature is 60°C, the pressure is 1500pis, and the static extraction is performed twice, 8 minutes each. Concentrate the extract to about 1ml with a rotary evaporator, transfer it to a 50ml centrifuge tube and dry it with nitrogen in a water bath at 37°C. Use 15ml of 1mol / L NaOH solution to ultrasonically dissolve the residue three times, then centrifuge and transfer the supernatant to a 50ml centrifuge tube, adjust its pH to 2 with 4mol / L hydrochloric acid, divide it with 30ml ethyl acetate three times at 300r / min The liquid-liquid extraction was carried out under shaking c...

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Abstract

The invention discloses a method for detecting estrogen, nonyl phenol, octyl phenol and bisphenol A in water body sediment based on an accelerated solvent extraction (ASE), liquid-liquid extraction (LLE) and liquid chromatography / tandem mass spectrum (LC / MS / MS) technology. The method comprises the following steps of: performing accelerated solvent extraction by using acetone as an extracting agent to extract the estrogen, the nonyl phenol, the octyl phenol and the bisphenol A in the water body sediment; dissolving residues generated after extract is blown by nitrogen by using 1mol / L sodium hydroxide solution, performing centrifugal collection on the supernate, and performing liquid-liquid extraction by using ethyl acetate under the condition that the pH is equal to 2; and performing concentration detection by using a 3200QTRAP type liquid chromatography / tandem mass spectrometer and an Agilent 1100 high performance liquid chromatography system of American Applied Biosystem Company and an automatic sample injector of American Agilent Company. The recovery rate is 59 to 94 percent, and the detection limit is 0.04ng / g.

Description

technical field [0001] The invention relates to the technical field of detecting organic pollutants in water body sediments by using fast solvent extraction-liquid-liquid extraction-liquid chromatography / tandem mass spectrometry (ASE-LLE-LC / MS / MS), in particular to Co-detection method of trace estrogen and its nonylphenol, octylphenol and bisphenol A in drugs. Background technique [0002] The natural estrogens estrone (Estrone, E1), 17β-estradiol (17β-Estradiol, E2) and estriol (Estriol, E3) secreted by human and animal ovaries, as well as synthetic estradiol as the main component of oral contraceptives The hormone 17α-ethinyl estradiol (17α-Ethinyl Estradiol, EE2) will enter the sewage treatment system or farmland soil along with the excrement and urine. The discharge of estrogen is inevitable, and estrogen, as a typical endocrine disruptor, has received extensive attention in the past decade. The survey results of estrogen concentration and removal efficiency of many se...

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/72G01N30/06
Inventor 史江红陈庆彩吴唯郭慧媛薄婷
Owner BEIJING NORMAL UNIVERSITY
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