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.
Anal Chem. 2016 Sep 6;88(17):8409-14. doi: 10.1021/acs.analchem.6b01543. Epub 2016 Aug 15.
A fully automated headspace bubble-in-drop microextraction (automated HS-BID) method, coupled to gas chromatography/mass spectrometric (GC/MS) analysis, was developed for the analysis of nitro musks in environmental water samples. The entire procedure, including the extraction of the analytes by HS-BID and GC/MS analysis of the analyte-enriched solvent, was completely automated. In BID, a certain volume of air is introduced into the extraction solvent droplet, enlarging the surface area of the extraction solvent droplet in relation to the water sample without increasing its volume, significantly enhancing extraction efficiency. Compared to conventional single drop microextraction, the developed method has higher extraction efficiency due to the enlarged surface area of the extraction solvent droplet. Under the optimized conditions (1.0 mL of sample solution, using 1.0 μL of 1-octanol containing of 0.5 μL of air bubble, at 40 °C for extraction for 20 min), the automated HS-BID gave low limits of detections (between 0.012 and 0.042 μg/L), good linearity (from 0.1 to 20 μg/L and from 0.2 to 50 μg/L, with r(2) between 0.9909 and 0.9958, depending on analytes), and good repeatability of the extractions (relative standard deviations, below 4.7%, n = 5). The developed procedure was applied to determine nitro musks in environmental water samples and was demonstrated to be efficient, labor-free, economical, and environmentally benign.
一种全自动顶空气泡-液滴微萃取（automated HS-BID）方法，与气相色谱/质谱（GC/MS）分析相结合，被开发用于分析环境水样中的硝基麝香。整个过程，包括通过 HS-BID 萃取分析物和 GC/MS 分析富集溶剂中的分析物，都是完全自动化的。在 BID 中，将一定体积的空气引入萃取溶剂液滴中，在不增加其体积的情况下，使萃取溶剂液滴的表面积相对于水样增大，从而显著提高萃取效率。与传统的单滴微萃取相比，由于萃取溶剂液滴的表面积增大，所开发的方法具有更高的萃取效率。在优化条件下（1.0 mL 样品溶液，使用 1.0 μL 含有 0.5 μL 气泡的 1-辛醇，在 40°C 下萃取 20 min），自动化 HS-BID 给出了较低的检测限（在 0.012 和 0.042 μg/L 之间）、良好的线性（从 0.1 到 20 μg/L 和从 0.2 到 50 μg/L，取决于分析物，r² 在 0.9909 和 0.9958 之间），以及良好的萃取重复性（相对标准偏差低于 4.7%，n = 5）。所开发的程序被应用于测定环境水样中的硝基麝香，结果表明该方法高效、无人工操作、经济且环境友好。
