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固相萃取与超高效液相色谱-紫外检测联用分析水中雌激素降解的改进方法。

Improved method for analyzing the degradation of estrogens in water by solid-phase extraction coupled with ultra performance liquid chromatography-ultraviolet detection.

机构信息

The First Institute of Oceanography, Qingdao 266101, China.

出版信息

J Environ Sci (China). 2011;23(4):693-8. doi: 10.1016/s1001-0742(10)60439-1.

DOI:10.1016/s1001-0742(10)60439-1
PMID:21793415
Abstract

We established an improved method for the determination of four estrogens including estriol (E3), 17beta-estradiol (E2), 17alpha-ethynylestrodiol (EE2) and estrone (El) in water. The method consisted of solid-phase extraction (0.5 L water) and subsequent analysis of analytes by ultra-performance liquid chromatography (UPLC) with an ultraviolet detector (UVD). Base-line separation was achieved for all studied estrogens using a column (50 mm x 2.1 mm) packed with 1.7 microm particle size stationary phase. Recovery was higher than 88% and detection limits ranged between 12.5-23.7 ng/L for the four estrogens, with the RSD ranging from 7% to 11%. The method was successfully applied to determine E2 and EE2 in simulated natural water, which found that about 70% of E2 was degraded (with a half-life of about 30 hr) within 48 hr and about 55% of EE2 was degraded (with a half-life of about 36 hr). Low levels of E1 were found, however E3 was undetectable during the process.

摘要

我们建立了一种改进的方法,用于测定水中的四种雌激素,包括雌三醇(E3)、17β-雌二醇(E2)、17α-乙炔基雌二醇(EE2)和雌酮(E1)。该方法包括固相萃取(0.5 L 水)和随后通过超高效液相色谱(UPLC)与紫外检测器(UVD)分析分析物。使用填充有 1.7 微米粒径固定相的柱(50mm×2.1mm)实现了所有研究的雌激素的基线分离。对于四种雌激素,回收率高于 88%,检测限在 12.5-23.7ng/L 之间,RSD 在 7%-11%之间。该方法成功应用于模拟天然水中的 E2 和 EE2 的测定,发现约 70%的 E2 在 48 小时内降解(半衰期约为 30 小时),约 55%的 EE2 降解(半衰期约为 36 小时)。在此过程中发现雌酮的水平较低,但无法检测到雌三醇。

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