Mulabagal Vanisree, Wilson Caleb, Hayworth Joel S
Department of Civil Engineering, Auburn University, Auburn, AL, 36849, USA.
Rapid Commun Mass Spectrom. 2017 Mar 15;31(5):419-429. doi: 10.1002/rcm.7807.
Estuaries are dynamic ecosystems, providing vital habitat for unique organisms of great ecological and commercial importance. The influx of natural and synthetic steroid hormones into estuaries poses risks to these organisms and to broader ecosystem health. However, detecting these trace level pollutants in estuarine water and sediment requires improved analytical techniques.
We describe an optimized ultrahigh-performance chromatography/tandem mass spectrometry (UHPLC/MS/MS) method for simultaneous quantitation of four classes of steroid hormones (estrogens, glucocorticoids, androgens and progestins) in sediment samples collected from an Alabama estuary. Sediment samples were homogenized using Hydromatrix (HM) sorbent and extracted with methanol and water (70%, v/v). Centrifuged extracts were purified using an Agilent Bond Elut QuEChERS dispersive-SPE kit to eliminate interfering substances that could negatively influence the ionization process. Chromatographic separation was achieved on a Poroshell 120 Phenyl-Hexyl column using an Agilent 1290 Infinity II UHPLC pump. Quantitation was carried out using an Agilent triple quadrupole mass spectrometer equipped with a JetStream/ESI source in dual mode.
Chromatographic separation and better peak resolution were accomplished on an Agilent Poroshell 120 Phenyl-Hexyl column using a binary gradient method with a mobile phase consisting of 1 mM ammonium fluoride in water and a mixture of methanol/acetonitrile. A dynamic multiple reaction monitoring (MRM) method was developed by optimizing various MS parameters. The method was used to analyze target steroid hormones in estuarine sediments. A total of ten steroid hormones were detected at trace amounts in estuarine sediments.
The optimized analytical method described here involves reasonably simple sample preparation and simultaneous trace level quantitation of four classes (estrogens, glucocorticoids, androgens and progestins) of steroid hormones in a single experimental run. Copyright © 2016 John Wiley & Sons, Ltd.
河口是动态生态系统，为具有重大生态和商业价值的独特生物提供重要栖息地。天然和合成类固醇激素流入河口会对这些生物以及更广泛的生态系统健康构成风险。然而，要在河口水体和沉积物中检测这些痕量污染物，需要改进分析技术。
我们描述了一种优化的超高效液相色谱/串联质谱（UHPLC/MS/MS）方法，用于同时定量从阿拉巴马州一个河口采集的沉积物样品中的四类类固醇激素（雌激素、糖皮质激素、雄激素和孕激素）。沉积物样品使用Hydromatrix（HM）吸附剂进行匀浆，并用甲醇和水（70%，v/v）萃取。离心后的萃取物使用安捷伦Bond Elut QuEChERS分散固相萃取试剂盒进行净化，以消除可能对电离过程产生负面影响的干扰物质。使用安捷伦1290 Infinity II超高效液相色谱泵在Poroshell 120苯基己基柱上实现色谱分离。使用配备JetStream/ESI源的安捷伦三重四极杆质谱仪以双模进行定量。
使用由水中1 mM氟化铵以及甲醇/乙腈混合物组成的流动相，通过二元梯度法在安捷伦Poroshell 120苯基己基柱上实现了色谱分离和更好的峰分辨率。通过优化各种质谱参数开发了一种动态多反应监测（MRM）方法。该方法用于分析河口沉积物中的目标类固醇激素。在河口沉积物中总共检测到十种痕量类固醇激素。
本文所述的优化分析方法涉及相当简单的样品制备，并且能够在单次实验运行中同时对四类（雌激素、糖皮质激素、雄激素和孕激素）类固醇激素进行痕量定量。版权所有© 2016约翰威立父子有限公司。
