自动化混合器辅助微型液-液萃取与全蒸发动态顶空萃取与美国环保署方法的比较，用于气相色谱-质谱分析氯苯。
Comparison of automated mixer-assisted mini-scale liquid-liquid extraction coupled with full evaporation dynamic headspace extraction with United States Environmental Protection Agency methods for the gas chromatography-mass spectrometric analysis of chlorinated benzenes.
机构信息
Integrative Sciences and Engineering Programme, NUS Graduate School, National University of Singapore, University Hall, Tan Chin Tuan Wing #04-02, 21 Lower Kent Ridge Road, Singapore 119077, Singapore; Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
Integrative Sciences and Engineering Programme, NUS Graduate School, National University of Singapore, University Hall, Tan Chin Tuan Wing #04-02, 21 Lower Kent Ridge Road, Singapore 119077, Singapore; Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore; National University of Singapore Environmental Research Institute, T-Lab Building #02-01, 5A Engineering Drive 1, Singapore 117411, Singapore.
出版信息
J Chromatogr A. 2021 Jun 21;1647:462131. doi: 10.1016/j.chroma.2021.462131. Epub 2021 Apr 8.
Three modes of facilitating mini-scale-liquid-liquid-extraction (msLLE) prior to automated integration with full evaporation dynamic headspace (FEDHS) extraction were evaluated in this work. For msLLE, 1.2 mL of dichloromethane (DCM) was added to a conical-bottomed vial containing 7 mL of aqueous sample. The solution was then subjected to three different mixing modes, namely vortex-assistance (where a "whirlpool" was created in the solution), agitation-assistance (where the vial was rotated in circular motion) and Mix-assistance (where the vial was shaken at a high speed). Vortex-assistance was performed manually while the other two modes were automated using a commercial autosampler. Following this, the DCM extract was transferred automatically to another vial and was then vaporized and sent through a Tenax TA sorbent tube in the FEDHS step. Due to the stronger π interaction between the sorbent and the analytes of interest, the analytes were selectively concentrated while the DCM vapor passed through unhampered. After FEDHS, the analytes were thoroughly desorbed into a gas chromatography-mass spectrometric system for analysis. The applicability of this procedure was validated in the extraction of six chlorinated benzenes (CBs) (1,2-dichlorobenzene, 1,3-dichlorobenzene, 1,4-dichlorobenzene, 1,2,4-trichlorobenzene, 1,2,4,5-tetrachlorobenzne and hexachlorobenzene) from aqueous samples. The Mix-assisted msLLE-FEDHS approach achieved good absolute extraction recoveries (between 74.2% and 88.7%), low limits of detection (between 0.0006 and 0.0116 µg/L), good linearity (r≥0.9920), good repeatability (between 1.9% and 8.4%, and good reproducibility (between 9.0% and 13.6%). It was found to be superior to the methods published by the United States Environmental Protection Agency. Five consecutive fully automated Mix-assisted-msLLE-FEDHS-GC-MS runs spanned only ca. 4 hr.
在本工作中，评估了三种在与全蒸发动态顶空（FEDHS）萃取自动集成之前促进微型液-液萃取（msLLE）的模式。对于 msLLE，将 1.2 mL 二氯甲烷（DCM）加入到含有 7 mL 水样品的锥形底小瓶中。然后，将溶液置于三种不同的混合模式下，即涡旋辅助（在溶液中产生“漩涡”）、搅拌辅助（小瓶以圆周运动旋转）和混合辅助（小瓶以高速振动）。涡旋辅助是手动进行的，而其他两种模式则使用商业自动进样器自动进行。此后，DCM 萃取物自动转移到另一个小瓶中，然后蒸发并通过 FEDHS 步骤中的 Tenax TA 吸附管输送。由于吸附剂和感兴趣的分析物之间较强的π相互作用，分析物被选择性地浓缩，而 DCM 蒸气则不受阻碍地通过。FEDHS 后，分析物被彻底解吸到气相色谱-质谱系统中进行分析。该程序的适用性通过从水样中提取六种氯苯（CBs）（1,2-二氯苯、1,3-二氯苯、1,4-二氯苯、1,2,4-三氯苯、1,2,4,5-四氯苯和六氯苯）得到了验证。混合辅助 msLLE-FEDHS 方法实现了良好的绝对萃取回收率（在 74.2%和 88.7%之间）、低检测限（在 0.0006 和 0.0116 µg/L 之间）、良好的线性（r≥0.9920）、良好的重复性（在 1.9%和 8.4%之间）和良好的重现性（在 9.0%和 13.6%之间）。它被发现优于美国环境保护署公布的方法。连续五次完全自动化的混合辅助-msLLE-FEDHS-GC-MS 运行仅耗时约 4 小时。
Zotero 插件