Hollow Fiber Liquid-Phase Microextraction At-Line Coupled to Capillary Electrophoresis for Direct Analysis of Human Body Fluids.,Analytical Chemistry

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Hollow Fiber Liquid-Phase Microextraction At-Line Coupled to Capillary Electrophoresis for Direct Analysis of Human Body Fluids.
Analytical Chemistry ( IF 6.7 ) Pub Date : 2020-05-01 , DOI: 10.1021/acs.analchem.0c00697
Blanka Miková _{1,

2} , Miloš Dvořák ₁ , Lenka Ryšavá _{1,

3} , Pavel Kubáň ₁

Affiliation

A simple and cheap all-in-one concept for at-line coupling of hollow fiber liquid-phase microextraction (HF-LPME) to commercial capillary electrophoresis (CE) is demonstrated, which enables the direct analysis of complex samples. A disposable microextraction device compatible with injection systems of Agilent CE instruments is proposed, which consists of a short segment of a porous HF attached to a tapered polypropylene holder. The holder maintains a constant position of the HF in a CE vial during extraction and simultaneously guides the injection end of a separation capillary into the HF lumen for automated CE injection and analysis. In a typical analytical procedure, the HF is impregnated with a water-immiscible solvent, its lumen is filled with 5 μL of an aqueous acceptor solution, and the microextraction device is placed in a 2 mL glass CE vial containing 550 μL of a donor solution. The vial is agitated at 750 rpm for 10 min, and the resulting acceptor solution is injected directly from the HF lumen into the commercial CE. No additional manual handling is required, except for the transfer of the CE vial to the CE autosampler. Multiple complex samples can be simultaneously pretreated in a multiple-well plate format, thus significantly reducing the total analysis time. Suitability of the analytical method is demonstrated by the direct determination of model basic drugs (nortriptyline, haloperidol, loperamide, and papaverine) in physiological solutions, urine, and dried blood spot (DBS) samples. Repeatability of the method is better than 12.8% (%RSD), extraction recoveries range between 34 and 76%, and enrichment factors are 37-84. The method is linear in a range of 2 orders of magnitude (R2 ≥ 0.9977) with limits of detection of 0.7-1.55 μg/L. The method has a high potential for the direct analysis of DBS samples since DBS elution and HF-LPME are performed simultaneously during the 10 min agitation. The manual DBS handling is thus reduced to inserting the DBS punch into the CE vial only. Moreover, the universal character of the HF-LPME might extend the applicability of the method to a wide range of analytes/matrices, and combination with other commercial detectors might improve the selectivity/sensitivity of the CE analysis.

中文翻译：

中空纤维液相微萃取在线耦合至毛细管电泳，直接分析人体液体。

展示了一种简单且便宜的多合一概念，用于将中空纤维液相微萃取（HF-LPME）在线耦合到商用毛细管电泳（CE），可直接分析复杂的样品。提出了一种与安捷伦CE仪器的进样系统兼容的一次性微萃取设备，该设备由一小段多孔HF组成，该HF连接到锥形聚丙烯支架上。固定器在萃取过程中保持HF在CE小瓶中的恒定位置，并同时将分离毛细管的注射端导入HF内腔，以实现自动CE注射和分析。在典型的分析程序中，将HF浸入与水不混溶的溶剂中，其内腔充满5μL的受体水溶液，然后将微萃取装置放入装有550μL供体溶液的2 mL玻璃CE小瓶中。将小瓶以750 rpm的速度搅拌10分钟，然后将所得的受体溶液直接从HF管腔注入商用CE。除了将CE样品瓶转移到CE自动进样器之外，不需要其他手动操作。多个复杂样品可以以多孔板形式同时进行预处理，从而大大减少了总分析时间。通过直接测定生理溶液，尿液和干血斑（DBS）样品中的模型基本药物（去甲替林，氟哌啶醇，洛哌丁胺和罂粟碱）证明了该分析方法的适用性。该方法的重复性优于12.8％（％RSD），萃取回收率在34％至76％之间，富集因子为37-84。该方法在2个数量级范围内（R2≥0.9977）是线性的，检出限为0.7-1.55μg/ L。该方法具有直接分析DBS样品的巨大潜力，因为在10分钟的搅拌过程中，DBS洗脱和HF-LPME可以同时进行。因此，手动DBS处理减少为仅将DBS打孔器插入CE小瓶。此外，HF-LPME的通用特性可能将方法的适用性扩展到广泛的分析物/基质，并且与其他商用检测器组合使用可能会提高CE分析的选择性/灵敏度。该方法具有直接分析DBS样品的巨大潜力，因为在10分钟的搅拌过程中可同时进行DBS洗脱和HF-LPME。因此，手动DBS处理减少为仅将DBS打孔器插入CE小瓶。此外，HF-LPME的通用特性可能将方法的适用性扩展到广泛的分析物/基质，并且与其他商用检测器组合使用可能会提高CE分析的选择性/灵敏度。该方法具有直接分析DBS样品的巨大潜力，因为在10分钟的搅拌过程中可同时进行DBS洗脱和HF-LPME。因此，手动DBS处理减少为仅将DBS打孔器插入CE小瓶。此外，HF-LPME的通用特性可能将方法的适用性扩展到广泛的分析物/基质，并且与其他商用检测器组合使用可能会提高CE分析的选择性/灵敏度。

更新日期：2020-04-14

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