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Combined headspace single-drop microextraction and solid-phase microextraction for the determination of phenols as their methyl ethers by gas chromatography-mass spectrometry
Analytical Methods ( IF 2.7 ) Pub Date : 2017-10-30 00:00:00 , DOI: 10.1039/c7ay02275a Archana Jain 1, 2, 3, 4 , Soumitra Soni 1, 2, 3, 4 , Kishan Reddy-Noone 1, 2, 3, 4 , Aradhana K. K. V. Pillai 1, 2, 3, 4 , Krishna K. Verma 1, 2, 3, 4
Analytical Methods ( IF 2.7 ) Pub Date : 2017-10-30 00:00:00 , DOI: 10.1039/c7ay02275a Archana Jain 1, 2, 3, 4 , Soumitra Soni 1, 2, 3, 4 , Kishan Reddy-Noone 1, 2, 3, 4 , Aradhana K. K. V. Pillai 1, 2, 3, 4 , Krishna K. Verma 1, 2, 3, 4
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Combined SDME and SPME worked as an elegant strategy to inject a large sampled mass of analytes into a GC. After headspace SDME of methyl derivatives of phenol, chlorophenols, methylphenols and other substituted phenols into 10 μL of solvent drop (1-butanol), the extract was subjected to headspace SPME (DVB/CAR/PDMS, 30/50 μm, fiber) for convenient transfer of analytes to the fiber and then into the GC. This combination resulted in achieving a high sensitivity of detection for a small volume (0.5–2 mL) of sample. The chromatographic separation of thirteen model phenols (as their methyl ethers) was complete within 10 min. A rectilinear calibration graph was obtained using combined headspace SDME/SPME and GC-MS in the range of 0.001–5 mg L−1, with a correlation coefficient of 0.990–0.999 and an average limit of detection of 20 ng L−1 (range 8–45 ng L−1), which was far better than that obtained by headspace SDME, 90 ng L−1 (range 50–138 ng L−1), or headspace SPME, 55 ng L−1 (range 36–70 ng L−1), when used alone. In spiking experiments on environmental water samples, the RSD of the results was in the range of 4.6–9.4%.
中文翻译：
顶空单滴微萃取与固相微萃取相结合用于气相色谱-质谱法测定酚类作为甲基醚
将SDME和SPME结合使用是一种优雅的策略，可以将大量的分析物样品注入GC中。将苯酚，氯酚，甲基苯酚和其他取代的苯酚的甲基衍生物的顶空SDME加入10μL溶剂滴（1-丁醇）中后，将萃取液进行顶空SPME（DVB / CAR / PDMS，30/50μm，纤维）方便地将分析物转移到纤维上，然后转移到GC中。这种结合导致对少量（0.5–2 mL）样品的检测具有很高的灵敏度。在10分钟内完成了13种模型酚（作为其甲基醚）的色谱分离。使用顶空SDME / SPME和GC-MS的组合在0.001-5 mg L -1范围内获得直线校准图的相关系数为0.990–0.999，平均检出限为20 ng L -1（范围为8–45 ng L -1），远优于顶空SDME获得的90 ng L -1（范围） 50–138 ng L -1）或顶空SPME单独使用时为55 ng L -1（范围36–70 ng L -1）。在对环境水样品的加标实验中，结果的RSD在4.6–9.4％的范围内。
更新日期：2017-11-17
中文翻译：
顶空单滴微萃取与固相微萃取相结合用于气相色谱-质谱法测定酚类作为甲基醚
将SDME和SPME结合使用是一种优雅的策略，可以将大量的分析物样品注入GC中。将苯酚，氯酚，甲基苯酚和其他取代的苯酚的甲基衍生物的顶空SDME加入10μL溶剂滴（1-丁醇）中后，将萃取液进行顶空SPME（DVB / CAR / PDMS，30/50μm，纤维）方便地将分析物转移到纤维上，然后转移到GC中。这种结合导致对少量（0.5–2 mL）样品的检测具有很高的灵敏度。在10分钟内完成了13种模型酚（作为其甲基醚）的色谱分离。使用顶空SDME / SPME和GC-MS的组合在0.001-5 mg L -1范围内获得直线校准图的相关系数为0.990–0.999，平均检出限为20 ng L -1（范围为8–45 ng L -1），远优于顶空SDME获得的90 ng L -1（范围） 50–138 ng L -1）或顶空SPME单独使用时为55 ng L -1（范围36–70 ng L -1）。在对环境水样品的加标实验中，结果的RSD在4.6–9.4％的范围内。
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