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A generic approach for expanding homolog-targeted residue screening of sulfonamides using a fast matrix separation and class-specific fragmentation-dependent acquisition with a hybrid quadrupole-linear ion trap mass spectrometer

机译:一种通用方法,可通过快速基质分离和混合四极杆-线性离子阱质谱仪对特定类别的片段化进行捕获来扩展磺酰胺类的同系物靶向残留物筛选

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摘要

A generic and efficient homolog-targeted approach was used to expand screening and detection of target class of sulfonamides and structural analogs, based on a fast single-tube extraction/partitioning-multifunction adsorption cleanup (SEP/MAC) for class-specific fragmentation-dependent acquisition with a liquid chromatography-hybrid triple-quadrupole linear ion trap mass spectrometer (LC-QqLIT). By combining the two-stage process conducted in a single tube as one-pot protocol, the straightforward SEP/MAC procedure was optimized to offer clean extracts with reasonable recovery (71-109% with RSDs < 20%) and decreased matrix interferences (-9 to 19%) of multiresidual sulfonamide extraction from different tissue samples. The novel use of neutral loss scan of 66 Da (NLS) or precursor ion scanning of m/z 108 (PreS) in positive ion mode was found to achieve more comprehensive coverage of protonated molecular ions of a wide array of sulfonamides including N4-acetyl and hydroxylamine metabolites plus their possible dmers. Moreover, the PreS-triggered automatically enhanced product ion spectral acquisition enabled simultaneous screening, profiling and confirmation of an unlimited number of analytes belonging to the sulfonamide class within a single analysis. The validation and application results of the generic SEP/MAC-based LC-QqLIT strategy consistently demonstrated favorable performances with acceptable accuracy (67-116%), precision (RSDs <25%), and sensitivity (LOQs≤7.5ngg~(-1)) to meet the
机译:基于快速的单管萃取/分配-多功能吸附净化(SEP / MAC),针对类特定的片段依赖性,使用通用且有效的针对同源物的方法扩展了对目标类磺酰胺和结构类似物的筛选和检测液相色谱-混合三重四极杆线性离子阱质谱仪(LC-QqLIT)进行质谱分析。通过将在单管中进行的两阶段过程结合为一锅法,对简单的SEP / MAC程序进行了优化,以提供具有合理回收率(71-109%的RSD <20%)和减少的基质干扰(-从不同组织样品中提取9%至19%的多残留磺酰胺。发现在正离子模式下使用66 Da(NLS)的中性损失扫描或m / z 108(PreS)的前体离子扫描的新方法可实现对包括N4-乙酰基在内的多种磺酰胺的质子化分子离子的更全面覆盖和羟胺代谢物及其可能的二聚体。此外,PreS触发的自动增强的产物离子光谱采集功能可在一次分析中同时筛选,分析和确认不限数量的属于磺酰胺类的分析物。通用的基于SEP / MAC的LC-QqLIT策略的验证和应用结果始终显示出良好的性能,具有可接受的精度(67-116%),精度(RSDs <25%)和灵敏度(LOQs≤7.5ngg〜(-1) ))满足

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