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Desorption Temperature, Solid-Phase Microextraction (SPME), and Natural Product Analyses, how Low Can we Go?
Journal of Chemical Ecology ( IF 2.2 ) Pub Date : 2021-01-18 , DOI: 10.1007/s10886-021-01247-0
Alexander M. Gaffke , Hans T. Alborn

Solid phase microextraction (SPME) has become a common technique for volatile sampling due to its ease of use and limited technical requirements. The solvent-free nature of SPME is also exceptionally attractive for gas chromatography mass spectrometry (GC/MS) analysis. To ensure efficient transfer of the sample to the GC, the manufacturer recommend injector desorption temperatures in the range of 200 to 320 °C. A high desorption temperature can, however, have unwanted effects on analyses of plant and insect produced semiochemicals. By investigating the quantitative and qualitative chromatographic responses at varying inlet temperatures for a component blend of seven plant produced volatile compounds, we found the thermally labile plant-nematode signaling compound, pregeijerene to degrade to geijerene at all tested temperatures within the recommended range (200, 240, and 280 °C), but that it did not break down with an inlet temperature below 200 °C (100 °C and 150 °C). Degradation was also detected for the sesquiterpene germacrene D, but only at the highest inlet temperature tested (280 °C). Surprisingly, an inlet temperature of 200 °C gave the highest sample recovery, measured as total peak area while an inlet temperature of 100 °C as well as 280 °C gave the lowest total area values. An increase in desorption time from 3 to 5 min. Resulted in a recovery at 100 °C close to that obtained at 200 °C. Peak broadening was minimal, and only observed at the 100 °C inlet temperature. Based on these results, we highly recommend that SPME users include desorption temperature as one variable when developing sampling procedures for novel biological systems to ensure that potentially present thermally labile compounds are not degraded.



中文翻译:

解吸温度,固相微萃取(SPME)和天然产物分析,我们能降低多少?

固相微萃取(SPME)由于其易用性和有限的技术要求,已成为挥发性采样的常用技术。SPME的无溶剂性质对于气相色谱质谱(GC / MS)分析也具有极大的吸引力。为了确保将样品有效地转移到GC,制造商建议进样器的解吸温度为200至320°C。但是,较高的解吸温度可能会对植物和昆虫产生的化学信息素的分析产生不良影响。通过研究七种植物产生的挥发性化合物的组分混合物在不同入口温度下的定量和定性色谱响应,我们发现了热不稳定的植物-线虫信号传导化合物,在推荐范围(200、240和280°C)内的所有测试温度下,pregeijerene都会降解为geijerene,但在入口温度低于200°C(100°C和150°C)时,它不会分解。还可以检测到倍半萜烯germ烯D的降解,但仅在测试的最高进口温度(280°C)下才降解。出乎意料的是,以总峰面积衡量,入口温度为200°C时样品回收率最高,而入口温度为100°C和280°C时样品总回收率最低。解吸时间从3分钟增加到5分钟。在100°C下的回收率接近200°C下的回收率。峰展宽最小,仅在100°C的入口温度下观察到。根据这些结果,

更新日期:2021-01-18
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