首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Using a novel sol-gel stir bar sorptive extraction method for the analysis of steroid hormones in water by laser diode thermal desorption/atmospheric chemical ionization tandem mass spectrometry
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Using a novel sol-gel stir bar sorptive extraction method for the analysis of steroid hormones in water by laser diode thermal desorption/atmospheric chemical ionization tandem mass spectrometry

机译:新型溶胶-凝胶搅拌棒吸附萃取法用于激光二极管热解吸/大气化学电离串联质谱分析水中的类固醇激素

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摘要

A new coating material was used for a stir bar sorptive extraction (SBSE) method coupled to a high throughput sample analysis technique. This allowed for a simple procedure for fast determinations of eight steroid hormones (estriol, estradiol, ethynylestradiol, estrone, progesterone, medroxyprogesterone, levonorgestrel, northindrone) in water. Sample pre-treatment was performed using an in-house SBSE method based on a polydimethylsiloxane/ phenyltrimethylsiloxane/β-cyclodextrin sol-gel material. The analytes were desorbed by liquid extraction prior to their analysis by laser diode thermal desorption/atmospheric pressure chemical ionization coupled to tandem mass spectrometry (LDTD-APCI-MS/MS). Several parameters, including ionic strength, volume and time of extraction as well as volume and time of desorption, were investigated to maximize extraction efficiency by SBSE in aqueous solutions. The in-house stir bar showed good reproducibility and could be used for at least 50 extractions without affecting analytical performance. The recoveries of the spiked steroid hormones ranged from 55% to 96% in all water matrices studied (HPLC grade water, tap water and raw wastewater). Only one compound showed poor recovery values (<2% for estriol) in all matrices. The method detection limits (MDLs) in real matrices were within the range of 0.1-0.3 μg L ~(-1) except for estriol at 48 μg L~(-1). The extraction performance of the in-house SBSE for the eight selected hormones was also compared with that of a commercially-available stir bar coated with polydimethylsiloxane (PDMS). This novel stir bar coating could prove to be useful method for the detection and quantification of trace levels of steroid hormones.
机译:一种新的涂料用于搅拌棒吸附萃取(SBSE)方法,并结合了高通量样品分析技术。这使得在水中可以快速测定八种类固醇激素(雌三醇,雌二醇,乙炔雌二醇,雌酮,孕酮,甲羟孕酮,左炔诺孕酮,北吲哚酮)的简单方法。使用基于聚二甲基硅氧烷/苯基三甲基硅氧烷/β-环糊精溶胶-凝胶材料的内部SBSE方法进行样品预处理。在通过激光二极管热脱附/大气压化学电离联用串联质谱法(LDTD-APCI-MS / MS)进行分析之前,先通过液体萃取对分析物进行解吸。研究了几个参数,包括离子强度,萃取体积和时间以及解吸体积和时间,以最大程度地提高SBSE在水溶液中的萃取效率。内部搅拌棒显示出良好的重现性,可用于至少50次提取,而不会影响分析性能。在所有研究的水基质(HPLC级水,自来水和原废水)中,加标的类固醇激素的回收率在55%至96%之间。在所有基质中,只有一种化合物的回收率较差(雌三醇<2%)。除了雌三醇在48μgL〜(-1)以外,实际基质中的方法检测限(MDL)在0.1-0.3μgL〜(-1)的范围内。内部SBSE对8种选定激素的提取性能也与涂有聚二甲基硅氧烷(PDMS)的市售搅拌棒的提取性能进行了比较。这种新颖的搅拌棒涂层可以证明是检测和定量痕量类固醇激素的有用方法。

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