Abstract
DOI: 10.1002/elps.202100216 The cover picture shows three modes of headspace liquid phase microextraction (HS-LPME) in-line coupled with CE. Headspace single drop microextraction (HS-SDME)-CE: When a single drop of the acceptor phase (blue) is formed at the inlet of a separation capillary filled with a run buffer (pale pink), the analytes evaporated from the sample donor solution (green) into the HS are extracted into the drop leaving less- or non-volatile matrix components in the sample. After extraction, a portion of the drop containing enriched analytes is injected into the capillary for CE analysis. Due to the large volume ratio between the sample donor solution and the acceptor drop, and the large surface-to-volume ratio of the drop, the sample enrichment factors obtained with SDME are quite high for a given extraction time, compared with other conventional LPME techniques. However, it is critical to maintain the drop stably attached to the capillary during extraction and thus it is rather difficult to carry out SDME for a long time especially under harsh conditions such as elevated temperature. Headspace in-tube microextraction (HS-ITME)-CE: Using a liquid plug in the capillary inlet as an acceptor phase instead of a hanging drop, the shortcomings of the hanging drop can be resolved. In HS-ITME-CE, the capillary inlet containing the acceptor plug is simply placed in the HS above a sample solution. Since the acceptor phase is well protected by the capillary, a long extraction at a temperature as high as 90°C can be performed with ease. Furthermore, since the enriched acceptor plug is already inside the capillary, the whole extract can be utilized for the subsequent CE analysis without additional injection step. Single bubble in-tube microextraction (SB-ITME)-CE: For a short extraction time, the extraction efficiency of HS-SDME or HS-ITME was not maximized because it takes some time for the analytes to fill the HS and reach saturated concentrations, especially for compounds of low volatility. By using a single bubble as a micro-HS formed at the inlet of a separation capillary immersed in the sample donor solution, the HS extraction can be expedited without waiting for the HS equilibration. Since the surface-to-volume ratio of the submicroliter bubble is much higher than that of a conventional HS of a few milliliters or more, the analyte concentrations in the bubble can be replenished much more rapidly for short extraction times. SB-ITME demonstrated higher sample enrichments than HS-ITME for a short HS extraction of chlorophenols in water.
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