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Preprocessing method suitable for analyzing estrogen and bisphenol A in complex matrix solid sample

A complex matrix, estrogen technology, applied in the direction of analysis materials, material separation, measurement devices, etc., can solve the problem of difficult processing technology

Inactive Publication Date: 2012-10-24
BEIJING NORMAL UNIVERSITY
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to solve the problems of difficult pretreatment technology for sludge and sediment samples with complex substrates, and to develop a purification technology with high recovery rate, high sensitivity, accuracy and speed, especially to achieve better removal Mixed effect, weaken matrix interference, and realize the co-detection and quantitative analysis technology of estrogen and bisphenol A in complex matrix samples

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  • Preprocessing method suitable for analyzing estrogen and bisphenol A in complex matrix solid sample
  • Preprocessing method suitable for analyzing estrogen and bisphenol A in complex matrix solid sample
  • Preprocessing method suitable for analyzing estrogen and bisphenol A in complex matrix solid sample

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Embodiment Construction

[0037] The following combination of examples and attached figure 2 The technical solution of the present invention is further described.

[0038] (1) Sample extraction

[0039] The collected solid samples were freeze-dried and ground. After accurately weighing the sample, use 60ml of acetone / methanol=1:1 (v / v) as the extractant, and extract the estrogen and bisphenol A in the sample with a fast solvent; then it is concentrated to about 1ml by rotary evaporation and blown with nitrogen. dry.

[0040] (2) Extraction solution purification

[0041] The sample extract is first purified by liquid-liquid extraction (LLE). After re-dissolving the residue with 10ml of acetonitrile, add 10ml of n-hexane and vortex for 10 minutes to extract non-polar substances such as grease in the extract. Repeat twice to discard the n-hexane phase, and dry the acetonitrile phase with nitrogen. Then proceed to the second step of Florisil (6cc, 500mg) purification: re-dissolve the LLE purification residue w...

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Abstract

The invention discloses a preprocessing method suitable for analyzing estrogen and bisphenol A in a complex matrix solid sample, which is a method for detecting the estrogen and the bisphenol A based on accelerated solvent extraction-liquid-liquid extraction-Florisil column purification-alkaline solution extraction-HLB (Hydrophile Lipophile Balance) column enrichment purification-liquid chromatogram / tandem mass spectrometry (ASE-LLE-Florisil-AS-HLB-LC / MS / MS). The method comprises the following steps of: taking acetone and methanol in a volume ratio of 1 : 1 (v / v) as extracting agents for the accelerated solvent extraction of the estrogen and the bisphenol A in sludge and deposit; taking acetonitrile-normal hexane system for the liquid-liquid extraction to remove non-polar impurities such as grease and polycyclic aromatic hydrocarbon and the like; taking the Florisil column for purifying most of pigments; extracting the estrogen and the bisphenol A from residue by using 0.1mol / L of sodium hydroxide; filtering by a filter membrane of 0.22 um[m]; and enriching and purifying by using an HLB column. According to the method, the recovery rate of the estrogen and the bisphenol A is 75-100%, the detection limit is lower than 0.4ng / g, the purification effect is good and the detection requirement for the estrogen in the complex matrix solid sample is satisfied. According to the research result, the estrogens and the bisphenol A in the sludge, the deposit and the livestock and poultry manure sample can be quickly and effectively separated and purified, the accuracy and stability of the method can be favorably improved and the damage of the complex sample on the instrument also can be reduced.

Description

Technical field [0001] The invention relates to the technical field of detection of organic pollutants in complex matrix solid samples, in particular to a sample purification method for analyzing the content of estrogen and bisphenol A in activated sludge, sediment or livestock and poultry manure. Background technique [0002] In recent years, natural and synthetic estrogen estrone (Estrone, E1), 17β-estradiol (17β-Estradiol, E2), 17α-ethinyl estradiol (17α-Ethinyl Estradiol, EE2), and estrogen-like activity The substance Bisphenol A (BPA), as a typical endocrine disruptor in the environment, has attracted widespread attention in the academic community. Research findings show that estrogen at a concentration of ng / L is detected in rivers or lakes in most countries, and this concentration range can lead to feminization of rainbow trout. Although, the ultimate source of estrogen production is humans and mammals. But in fact, the centralized treatment and discharge of domestic sew...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/14
Inventor 史江红陈庆彩吴唯刘晓薇张晖
Owner BEIJING NORMAL UNIVERSITY
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