Citation: WANG Xiaoyan, QI Weimei, ZHAO Xian'en, LÜ Tao, WANG Xiya, ZHENG Longfang, YAN Yehao, YOU Jinmao. Determination of four phenolic endocrine disruptors in environmental water samples by high performance liquid chromatography-fluorescence detection using dispersive liquid-liquid microextraction coupled with derivatization[J]. Chinese Journal of Chromatography, ;2014, 32(6): 623-628. doi: 10.3724/SP.J.1123.2014.02012 shu

Determination of four phenolic endocrine disruptors in environmental water samples by high performance liquid chromatography-fluorescence detection using dispersive liquid-liquid microextraction coupled with derivatization

WANG Xiaoyan ¹ ,
QI Weimei ² ,
ZHAO Xian'en ^1,, ,
LÜ Tao ¹ ,
WANG Xiya ¹ ,
ZHENG Longfang ¹ ,
YAN Yehao ¹ ,
YOU Jinmao ^1,3,,

1.
1. Shandong Provincial Key Laboratory of Life-Organic Analysis, College of Chemistry and Chemical Engineering, Qufu Normal University, Qufu 273165, China;

Corresponding author: ZHAO Xian'en, YOU Jinmao,
Received Date: 17 February 2014
Available Online: 10 April 2014
Fund Project: 国家自然科学基金项目(81303179) (81303179)曲阜师范大学科研启动基金项目(BSQD2012019). (BSQD2012019)

To achieve accurate, fast and sensitive detection of phenolic endocrine disruptors in small volume of environmental water samples, a method of dispersive liquid-liquid microextraction (DLLME) coupled with fluorescent derivatization was developed for the determination of bisphenol A, nonylphenol, octylphenol and 4-tert-octylphenol in environmental water samples by high performance liquid chromatography-fluorescence detection (HPLC-FLD). The DLLME and derivatization conditions were investigated, and the optimized DLLME conditions for small volume of environmental water samples (pH 4.0) at room temperature were as follows: 70 μL chloroform as extraction solvent, 400 μL acetonitrile as dispersing solvent, vortex mixing for 3 min, and then high-speed centrifugation for 2 min. Using 2-[2-(7H-dibenzo[a,g]carbazol-7-yl)-ethoxy] ethyl chloroformate (DBCEC-Cl) as precolumn derivatization reagent, the stable derivatives of the four phenolic endocrine disruptors were obtained in pH 10.5 Na₂CO₃-NaHCO₃ buffer/acetonitrile at 50 ℃ for 3 min, and then separated within 10 min by HPLC-FLD. The limits of detection (LODs) were in the range of 0.9-1.6 ng/L, and the limits of quantification (LOQs) were in the range of 3.8-7.1 ng/L. This method had perfect linearity, precision and recovery results, and showed obvious advantages and practicality comparing to the previously reported methods. It is a convenient and validated method for the routine analysis of phenolic endocrine disruptors in waste water of paper mill, lake water, domestic wastewater, tap water, etc.
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