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自动化固相动态萃取——使用壁涂覆注射器针头萃取有机物。

Automated solid phase dynamic extraction--extraction of organics using a wall coated syringe needle.

作者信息

Lipinski J

机构信息

SOFIA GmbH, Rudower Chaussee 29, 12489 Berlin, Germany.

出版信息

Fresenius J Anal Chem. 2001 Jan 1;369(1):57-62. doi: 10.1007/s002160000618.

Abstract

Extractions of liquid samples were carried out using wall coated needles prepared from stainless steel capillary columns instead of syringe needles. This micro extraction technique was applied to the analysis of pesticides in water. Important parameters influencing the extraction such as sample velocity, extraction time and also the desorption parameters were investigated and optimized. Automation of this technique was realized using a conventional automatic sampler. Limits of detection were improved using the multiple extraction/desorption technique. Chromatographic data and limits of detection were compared with those obtained by solid phase micro extraction (SPME). Using a needle with a 7 microns film yielded limits of detection varying from 0.001-0.1 microgram/L and were in the same range as those resulting from the extraction using a 100 microns polydimethylsiloxane (PDMS) SPME fiber. The main advantages of the needle extraction technique were the significantly higher extraction speed and the practical aspects of a stable steel needle compared to those of a fragile fiber. The extraction speed using a needle with a 7 microns film was up to five times higher than the speed of SPME using a 100 microns PDMS fiber. The steel needle could be stressed mechanically in a higher extent than a SPME fiber. Sample volumes and aliquots of liquid media could be handled and moved from one bottle to another using the automatic sampler.

摘要

液体样品的萃取是使用由不锈钢毛细管柱制备的涂壁针而非注射器针来进行的。这种微萃取技术被应用于水中农药的分析。研究并优化了影响萃取的重要参数,如样品流速、萃取时间以及解吸参数。使用传统自动进样器实现了该技术的自动化。采用多次萃取/解吸技术提高了检测限。将色谱数据和检测限与固相微萃取(SPME)所获得的结果进行了比较。使用具有7微米薄膜的针,检测限在0.001 - 0.1微克/升之间变化,与使用100微米聚二甲基硅氧烷(PDMS)SPME纤维萃取所得到的检测限处于同一范围。针萃取技术的主要优点是与脆弱的纤维相比,萃取速度显著更高,且钢针具有实用性。使用具有7微米薄膜的针的萃取速度比使用100微米PDMS纤维的SPME速度高出多达五倍。钢针在机械应力方面比SPME纤维能承受更高的程度。使用自动进样器可以处理液体介质的样品体积和等分试样,并将其从一个瓶子转移到另一个瓶子。

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