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Hollow fiber-protected liquid-phase microextraction followed by high performance liquid chromatography for simultaneously screening multiple trace level β-blockers in environmental water samples

机译:中空纤维保护液相微萃取,然后用高效液相色谱法同时筛查环境水样中的多种痕量β受体阻滞剂

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A sensitive and reliable method using a two-phase hollow fiber liquid-phase microextraction (HF-LPME) pretreatment technique was developed for simultaneously screening multiple ?2-blockers in environmental samples. In this study, heptanol was chosen as the optimal extraction solvent, and six ?2-blockers with a wide range of polarities were extracted across the porous walls of hollow fibers and into the acceptor phase (AP). The fundamental parameters affecting the extraction efficiency (EE) of analytes including extraction time, temperature, pH of the donor phase (DP) and AP, stirring speed, volume of the sample solution, ionic strength and the type of hollow fiber membrane were studied and optimized. Under optimal conditions, extracts were analyzed by HPLC with ultraviolet detection (UV). Finally, satisfactory results were obtained, good linearity was observed for all ?2-blockers in the range of 0.16a€“200 ng mLa?’1, limits of detection (LODs) were between 0.08 and 0.5 ng mLa?’1, the intra- and inter-day precision values of the six ?2-blockers were 1.0a€“2.2% and 1.4a€“2.7%, respectively. The recovery with RSDs was less than 2.2% for the pretreatment method. The proposed technique was successfully applied for screening multiple ?2-blockers in complex aqueous samples with the best specificity and provided a simple and reliable new means for the self-checking of laboratories at the basic level.
机译:开发了一种灵敏且可靠的方法,该方法使用两相中空纤维液相微萃取(HF-LPME)预处理技术来同时筛选环境样品中的多种β2-阻滞剂。在这项研究中,选择庚醇作为最佳的萃取溶剂,并从中空纤维的多孔壁上将六种具有广泛极性的α2-阻滞剂萃取到受体相(AP)中。研究了影响分析物提取效率(EE)的基本参数,包括提取时间,温度,施主相(DP)和AP的pH,搅拌速度,样品溶液的体积,离子强度和中空纤维膜的类型,并优化。在最佳条件下,提取物通过HPLC和紫外检测(UV)进行分析。最后,获得了满意的结果,所有α2-阻滞剂在0.16a?200 ng mLa?1范围内均观察到良好的线性,检测限(LOD)在0.08至0.5 ng mLa?1之间。六个α2-阻滞剂的日内和日间精度值分别为1.0a€2.2%和1.4a€2.7%。预处理方法的RSD回收率低于2.2%。所提出的技术已成功应用于具有最佳特异性的复杂水性样品中多种α2-受体阻滞剂的筛选,并为基础实验室的自我检查提供了一种简单可靠的新方法。

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