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

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 manure. Background technique [0002] In recent years, natural and synthetic estrogens estrone (Estrone, E1), 17β-estradiol (17β-Estradiol, E2), 17α-ethinyl estradiol (17α-Ethinyl Estradiol, EE2), and estrogen-like activity The substance bisphenol A (Bisphenol A, BPA) as a typical endocrine disruptor in the environment has attracted widespread attention in the academic circles. The findings of the research show that estrogens at ng / L concentration levels have been detected in rivers or lakes in most countries, and this concentration range can lead to the feminization of rainbow trout. Although, the ultimate source of estrogen production is humans and mammals. But in fact, centralized treatment and d...

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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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