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首页> 外文期刊>Environmental toxicology and chemistry >ANALYSIS OF ESTROGENS IN SEDIMENT FROM A SEWAGE-IMPACTED URBAN ESTUARY USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/TIME-OF-FLIGHT MASS SPECTROMETRY
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ANALYSIS OF ESTROGENS IN SEDIMENT FROM A SEWAGE-IMPACTED URBAN ESTUARY USING HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY/TIME-OF-FLIGHT MASS SPECTROMETRY

机译：高效液相色谱/飞行时间质谱法分析污水渗入的城市河口中的雌激素

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摘要

We describe a highly selective and sensitive method for determination of estrone (El) and β-estradiol (E2) in sediments, using high-performance liquid chromatography/time-of-flight (HPLC-ToF) mass spectrometry. The method involved sequential cleanup of sediment extracts over solid phase extraction cartridges, normal phase HPLC, and immunoaffinity extraction, which combine to remove coeluting matrix interferences. Resulting method detection limits (0.03 and 0.04ng/g for El and E2, respectively) are sufficient to determine El and E2 in estuarine sediments collected from sewage-impacted Jamaica Bay (New York, NY, USA). The ToF analyzer has a higher resolution (>6,000) than quadrupole mass analyzers and can provide accurate mass estimation to within 2 mDa, which helped in distinguishing steroids from isobaric matrix interferences. The El and E2 were internally mass calibrated with respect to their coeluting surrogate standards, and the mass measurement error was between 1.1 and 1.4 mDa. The levels of El and E2 ranged between 0.07 to 2.52 and 0.05 to 0.53 ng/g, respectively. The measured concentrations of steroids in sediments correlated closely with other wastewater tracers. Despite the low concentrations of sediment-associated estrogens, their predicted estrogenic potency exceeds that of other measured estrogenic contaminants.
机译：我们描述了一种使用高效液相色谱/飞行时间（HPLC-ToF）质谱法测定沉积物中雌酮（El）和β-雌二醇（E2）的高度选择性和灵敏的方法。该方法包括在固相萃取柱上依次纯化沉淀物，正相HPLC和免疫亲和萃取，两者结合以消除共洗脱基质干扰。所得到的方法检出限（分别为El和E2的0.03和0.04ng / g）足以确定从受污水影响的牙买加湾（纽约，纽约，美国）收集的河口沉积物中的El和E2。与四极杆质量分析仪相比，ToF分析仪具有更高的分辨率（> 6,000），并且可以提供精确的质量估计值，误差范围在2 mDa之内，这有助于区分类固醇与等压基质干扰。 E1和E2就其共洗脱替代标准品进行了内部质量校准，质量测量误差在1.1至1.4 mDa之间。 E1和E2的水平分别在0.07至2.52和0.05至0.53ng / g之间。沉积物中类固醇的测量浓度与其他废水示踪剂密切相关。尽管与沉积物相关的雌激素浓度较低，但它们的预测雌激素效价超过其他测得的雌激素污染物。

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