In Situ Formed Organic Ion-Associate Liquid-Phase Microextraction without Centrifugation from Aqueous Solutions Using Thymol Blue and Estrogens

Sachiko Osada, Seira Takahashi, Kazuto Sazawa, H. Kuramitz, Nozomi Kohama, Takuya Okazaki, Shigeru Taguchi, N. Hata
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Abstract

In this study, we present a method for ion-associated liquid phase (IALP) separation and concentration of analytes from an aqueous matrix into an IALP formed in situ by the charge neutralization reaction of organic cations and anions, without centrifugation. The effects of various factors on the extraction efficiency and other parameters are investigated, whereas no instrumental stirring, such as vortexing or ultrasonics, is required because the solvent (IALP) is formed in situ. The organic cation and anion used are ethylhexyloxypropylammonium and dodecyl sulfate, respectively. The developed in situ IALP microextraction method for phase separation without centrifugation is tested using the thymol blue dye and several endocrine disruptors. The tested endocrine disruptors (bisphenol A, 17β-estradiol, 17α-ethinylestradiol, and estrone) are analyzed via high-performance liquid chromatography/fluorescence detection, with respective detection limits of 0.02, 0.02, 0.02, and 0.4 μg L−1, and the corresponding enrichment factor ranging from 47 to 71. This IALP microextraction method can be used to separate and concentrate environmental water samples of different matrices. The employed IALP is fast and easy to use, enables an approximately 100-fold analyte concentration, and has a high affinity for estrogens, thus holding promise for the separation, concentration, and quantitation of diverse trace analytes.
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使用百里酚蓝和雌激素从水溶液中不离心原位形成有机离子析出液相微萃取法
在本研究中,我们提出了一种无需离心的离子相关液相(IALP)分离和浓缩方法,将分析物从水性基质中分离到由有机阳离子和阴离子的电荷中和反应在原位形成的 IALP 中。研究了各种因素对萃取效率和其他参数的影响,由于溶剂(IALP)是在原位形成的,因此不需要涡旋或超声等仪器搅拌。使用的有机阳离子和阴离子分别是乙基己氧基丙基铵和十二烷基硫酸盐。使用百里酚蓝染料和几种内分泌干扰物测试了所开发的无需离心即可进行相分离的原位 IALP 微萃取方法。测试的内分泌干扰物(双酚 A、17β-雌二醇、17α-炔雌醇和雌酮)通过高效液相色谱/荧光检测法进行分析,检测限分别为 0.02、0.02、0.02 和 0.4 μg L-1,相应的富集因子范围为 47 至 71。这种 IALP 微萃取方法可用于分离和浓缩不同基质的环境水样。所采用的 IALP 快速简便,可使分析物浓度提高约 100 倍,并且对雌激素具有高亲和力,因此有望用于多种痕量分析物的分离、浓缩和定量。
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