Determination of steroid sex hormones in water and urine matrices by stir bar sorptive extraction and liquid chromatography with diode array detection
Determination of steroid sex hormones in water and urine matrices by stir bar sorptive extraction and liquid chromatography with diode array detection
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DOI：
10.1016/j.jpba.2006.02.037
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发表时间：
2006-06-16
影响因子：
3.4
通讯作者：
Nogueira, J. M. F.
中科院分区：
文献类型：
--
作者：
Almeida, C.;Nogueira, J. M. F.
本研究采用搅拌棒吸附萃取、液体解吸、高效液相色谱与二极管阵列检测（SBSE-LD-HPLC/DAD）相结合，同时测定水中9种甾体性激素（雌酮、17α-雌二醇、17β-雌二醇、17α-乙炔雌二醇、己烯雌酚、美雌醇、黄体酮、19-炔诺酮和炔诺孕酮）的含量。和尿液基质。在方法开发过程中，已证明平衡时间、离子强度和反萃取溶剂是测定水基质中的九种激素时最重要的控制参数，其中使用了涂有 126 111 聚二甲基硅氧烷的搅拌棒。在优化的实验条件下，对 30 ml 水样中添加 10 μg/L 的浓度进行测定，回收率范围为 11.1 +/- 4.9%（17 β-雌二醇）至 100.2 +/- 10.4%（美雌醇），表明该方法通过后者的辛醇-水分配系数（K-PDMS/W 近似于 K-O/W）得到了很好的描述，而与观察其余激素的理论效率（KPDMS/W 0 KO/W）。通过校准研究，所有激素都获得了良好的分析性能，包括合适的精度 (2.1-17.1 %)、低检测限 (0.3-1.0 mu g/l) 和出色的线性动态范围 (1.25-50.0 mu g/l)。对环境水和尿液基质的分析表明，回收率与加标水平（10μg/l）非常一致，并且适合分析孕妇尿液样本中低μg/l水平的天然激素。本方法在痕量水平上简单、可靠且灵敏，仅需要少量样品，是环境和生物医学实验室常规质量控制的良好分析替代方案。 (c) 2006 Elsevier B.V. 保留所有权利。
In this study, stir bar sorptive extraction and liquid desorption followed by high performance liquid chromatography with diode array detection (SBSE-LD-HPLC/DAD) were combined for the simultaneous determination of nine steroid sex hormones (estrone, 17 alpha-estradiol, 17 beta-estradiol, 17 alpha-ethynylestradiol, diethylstilbestrol, mestranol, progesterone, 19-norethisterone and norgestrel) in water and urine matrices. During the method development, it has been demonstrated that equilibrium time, ionic strength and back extraction solvents are the most important parameters to control, for determining the nine-hormones in water matrices, in which stir bars coated with 126 111 of polydimethylsiloxane were used. Assays performed on 30 ml water samples spiked at 10 mu g/l levels under optimised experimental conditions, yielded recoveries ranging from 11.1 +/- 4.9% (17 beta-estradiol) to 100.2 +/- 10.4% (mestranol), showed that the methodology is well described by the octanol-water partition coefficients (K-PDMS/W approximate to K-O/W) for the latter, while pronounced deviations to the theoretical efficiency (KPDMS/W 0 KO/W) were observed for the remaining hormones. From calibration studies, a good analytical performance for all hormones was attained, including a suitable precision (2.1-17.1 %), low limits of detection (0.3-1.0 mu g/l) and an excellent linear dynamic range (1.25-50.0 mu g/l). Assays on environmental water and urine matrices showed recovery yields in worthy good agreement with the spiking level (10 mu g/l), and suitability for profiling low mu g/l levels of natural hormones in urine samples taken from pregnant women. The present methodology is easy, reliable and sensitive at the trace level, only requiring a low samplevolume, showing to be a good analytical alternative to routine quality control for environmental and biomedical laboratories. (c) 2006 Elsevier B.V. All rights reserved.