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通过分子印迹固相萃取与高效液相色谱联用分离和测定痕量环境雌激素。

Separation and determination of trace environmental estrogen through molecularly imprinted solid phase extraction coupled to high performance liquid chromatography.

机构信息

College of Food Science and Engineering, Shandong Agricultural University, Tai'an, China.

出版信息

J Environ Sci Health A Tox Hazard Subst Environ Eng. 2012;47(12):1889-96. doi: 10.1080/03601234.2012.676438.

Abstract

In recent years, there has been an increasing demand on the determination of trace environmental estrogen. In this study, a new 17β-estradiol molecularly imprinted polymer was successfully synthesized on the surface of activated silica gel. This prepared molecularly imprinted polymer was characterized, and found to exhibit good recognition, high selectivity, and a rapid adsorption-desorption dynamic toward 17β-estradiol. Using the molecularly imprinted polymer as a sorbent, an effective method of solid phase extraction coupled to high performance liquid chromatography for the separation and determination of 17β-estradiol was developed. Under optimal conditions, the detection limit (S/N = 3) of 17β-estradiol was 12.0 ng L(-1). The enrichment factor was 198, and the linear range of the calibration graph was 0.05-300 mg L(-1). Blank water samples spiked with 17β-estradiol at three different levels were analyzed by the developed method to afford recoveries ranging from 82.7% to 103.0%. Moreover, this presented method was applied to the quantitative detection of 17β-estradiol in a polluted water sample with a level of 0.024 mg L(-1).

摘要

近年来,痕量环境雌激素的测定需求日益增加。本研究成功地在活化硅胶表面合成了一种新型的 17β-雌二醇分子印迹聚合物。对所制备的分子印迹聚合物进行了表征,发现其对 17β-雌二醇具有良好的识别性、高选择性和快速的吸附-解吸动力学。将分子印迹聚合物作为吸附剂,结合高效液相色谱法,建立了一种有效的固相萃取分离测定 17β-雌二醇的方法。在最佳条件下,17β-雌二醇的检测限(S/N = 3)为 12.0 ng L(-1)。富集因子为 198,校准曲线的线性范围为 0.05-300 mg L(-1)。用所建立的方法对空白水样进行加标实验,在三个不同浓度水平下,17β-雌二醇的回收率在 82.7%至 103.0%之间。此外,该方法还应用于实际受污染水样中 17β-雌二醇的定量检测,结果为 0.024 mg L(-1)。

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