Tehranirokh Masoomeh, Van den Bronk Marcel, Smith Peter, Dai Zach, Ragunathan Kannan, Muscalu Alina, Mills Simon, Breadmore Michael C, Shellie Robert A
ARC Training Centre for Portable Analytical Separation Technologies (ASTech), University of Tasmania, Private Bag 75 Hobart, 7001 Australia; Trajan Scientific and Medical, 7 Argent Place Ringwood, 3134 Australia.
Trajan Scientific and Medical, 7 Argent Place Ringwood, 3134 Australia.
J Chromatogr A. 2021 Apr 12;1642:462032. doi: 10.1016/j.chroma.2021.462032. Epub 2021 Mar 3.
Liquid-liquid extraction is one of the most widely used and simplest sample preparation techniques. However, consumption of large volumes of organic solvent and manual handling are two major drawbacks of this technique. A multifunction autosampler syringe is introduced which permits automated liquid-liquid extraction in an enclosed operating environment, with low consumption of organic solvents. The device described herein features a micromixer function in addition to common autosampler syringe features like accurate and precise aspirating and dispensing. To test the functionality of the micromixer syringe, manual extraction of caffeine from a tea infusion and semi-automated extraction of dichloroethane from water were carried out. Excellent recoveries of caffeine from a tea infusion (89% recovery with 1.3% RSD) and dichloroethane from water (107% recovery with 10% RSD) were obtained. Two automated workflows were tested using the micromixer syringe mounted in a laboratory autosampler. Standalone automated micro liquid-liquid extraction was performed for sample preparation of selected polychlorinated biphenyl (PCB) congeners prior to comprehensive two-dimensional gas chromatography - electron capture detection analysis. Extraction of PCBs using the described approach used substantially less solvent than a validated solid-phase extraction approach whilst delivering equivalent results for samples with high-level PCBs. Finally, fully automated extraction and GC-MS analysis of polynuclear aromatic hydrocarbons (PAHs) from water samples was performed. Mean recoveries of extraction for PCB and PAH analysis were > 70% using 4 min automated liquid-liquid extractions.
液-液萃取是应用最广泛且最简单的样品制备技术之一。然而，大量有机溶剂的消耗和人工操作是该技术的两个主要缺点。本文介绍了一种多功能自动进样器注射器，它能在封闭的操作环境中实现自动液-液萃取，且有机溶剂消耗低。本文所述的装置除了具备普通自动进样器注射器准确精确的吸取和分配功能外，还具有微混合器功能。为测试微混合器注射器的功能，进行了从茶浸液中手动萃取咖啡因以及从水中半自动萃取二氯乙烷的实验。从茶浸液中萃取咖啡因的回收率极佳（回收率89%，相对标准偏差1.3%），从水中萃取二氯乙烷的回收率也很好（回收率107%，相对标准偏差10%）。使用安装在实验室自动进样器中的微混合器注射器测试了两种自动化工作流程。在全二维气相色谱-电子捕获检测分析之前，对选定的多氯联苯（PCB）同系物进行样品制备时，采用了独立的自动微液-液萃取。使用所述方法萃取多氯联苯时，溶剂用量比经过验证的固相萃取方法少得多，同时对于高含量多氯联苯的样品能给出相当的结果。最后，对水样中的多环芳烃（PAH）进行了全自动萃取和气相色谱-质谱分析。使用4分钟的自动液-液萃取，多氯联苯和多环芳烃分析的萃取平均回收率>70%。
