Citation: SONG Wenwen, LUO Xialin, LI Gongke, HU Yufei. Analysis of trace estrogens in toners by monolithic column online solid phase microextraction coupled with high performance liquid chromatography[J]. Chinese Journal of Chromatography, ;2017, 35(1): 20-26. doi: 10.3724/SP.J.1123.2016.08012 shu

Analysis of trace estrogens in toners by monolithic column online solid phase microextraction coupled with high performance liquid chromatography

School of Chemistry, Sun-Yat-Sen University, Guangzhou 510275, China

Received Date: 15 August 2016

Fund Project: National Natural Science Foundation of China (Nos. 21475153, 21575167)

A Poly(glycidyl methacrylate-co-ethyleneglycol dimethacrylate) (Poly(GMA-co-EDMA)) monolithic column was prepared in a capillary by in-situ polymerization. Glycidyl methacrylate (GMA) was chosen to be the monomer and ethyleneglycol dimethacrylate (EDMA) was utilized as crosslinking agent. The binary porogenic agents of methanol and n-hexane can develop the permeability of monolithic column and they were suitable to construct the online analysis apparatus. A series of experiments were carried out, and they demonstrated the monolithic column had good permeability with low column pressure (1.5×10⁶ Pa at the washing flow rate of 0.5 mL/min). The enrichment factors of the prepared monolithic column for estradiol, ethynyl estradiol, estrone and diethylstilbestrol were 86, 116, 77 and 86, respectively. It was proved that the monolithic column was suitable for the online microextraction system by using the interface unit. A method was established for the analysis of trace estradiol, ethynyl estradiol, estrone and diethylstilbestrol in toners by monolithic column online solid phase microextraction coupled with high performance liquid chromatography. The limits of detection (S/N=3) were 0.05-0.20 μg/L. The recoveries in toner samples varied from 69.3% to 111.3%, and relative standard deviations were less than 5.0%. The method is efficient, sensitive, accurate, reliable and applicable to analyze trace estrogens in toners.
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