An improved method for simultaneous analysis of steroid and phenolic endocrine disrupting chemicals in biological samples

作者：Liu, Jingliang; Pan, Xuejun^*; Huang, Bin; Fang, Kai; Wang, Yu; Gao, Jianpei

来源：International Journal of Environmental Analytical Chemistry, 2012, 92(10): 1135-1149.

DOI：10.1080/03067319.2010.510604

• endocrine disrupting chemicals
• biological samples
• microwave-assisted extraction
• gel permeation chromatography
• solid phase extraction
• gas chromatography-mass spectrometry

An improved method was developed for the simultaneous determination of eight steroid and phenolic endocrine disrupting chemicals, such as oestrone (E1), 17 beta-oestradiol (E2), oestriol (E3), 17 alpha-ethynylestradoil (EE2), 4-nonylphenol (4-NP), bisphenol A (BPA), 4-tert-octylphenol (4-t-OP) and 4-cumylphenol (4-CP), in biological samples. The optimal extraction and clean-up procedures were investigated using microwave-assisted extraction (MAE), automated gel permeation chromatography (GPC) and solid phase extraction (SPE). As a consequence, the most efficient extraction was achieved by using MAE with methanol as solvent at an extraction temperature of 110 degrees C for 20 min. The clean-up of extracts was carried out by GPC on a Biobeads S-X3 column with cyclohexane/ethyl acetate (1:1, v/v) as mobile phase. Target compounds were eluted in the fraction from 7-14 min retention time. Moreover, the cleanest extracts were obtained by solid phase extraction with C-18 cartridges after the elution with 15mL ethyl acetate. The final sample extracts were derivatised using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) (1% trimethylchlorosilane, TMCS) as derivatisation reagent with pyridine as the solvent. Quantification was performed by gas chromatography-mass spectrometry (GC-MS) with electron ionisation (EI) and selected ion monitoring (SIM) mode. The method was validated by spiked samples which showed good recovery and reproducibility. The overall recoveries ranged between 55.1% and 100.6%, with relative standard deviations (RSD) of 2.3-12.7% for the entire procedure. Method detection limits (MDL) ranged from 0.3 to 0.7 ng g(-1) dry weight (dw). Performance of the method was demonstrated by its application on tissues from fish exposed to high concentration of EDCs in the laboratory. The developed method is a promising approach for the analysis of steroid and phenolic endocrine disrupting chemicals in various biological samples.

• 出版日期2012
• 单位昆明理工大学