PDF(Pubmed)
Abstract：
Accurate measurement of the composition of complex samples is key for the safety and efficacy of a range of products used in daily life, with sample preparation a critical step in this workflow. QuEChERS is one such method, however published protocols do not explicitly address acidic, basic, neutral, and amphiphilic species in a single protocol and often use extra steps or an alternative preparation to recover the breadth of chemical types. Our work addresses this need by investigating the use of QuEChERS for monitoring this wide range of chemistries within environmental solids and blood plasma, using a protocol that can accommodate both milliliter and microliter sample volumes. While published methods can require significant resource and time, our approach offers a reduction in preparation time (for environmental samples), with the \"micro-QuEChERS\" protocol offering a further reduction in cost. The analytical performance of these methods were assessed using reversed-phase LC-MS and showed good accuracy, precision, and sensitivity for the expected concentrations in the tested applications. Target analytes of variable lipophilicity/acidity were extracted and isolated from soil, with largely repeatable matrix effects < 15%RSD and recoveries of 39-100%. An initial \"proof-of-concept\" investigation using the \"micro-QuEChERS\" protocol showed reduced matrix enhancement (median value of 90%ME) for soil, and improved matrix effects and recovery (>65%) for blood plasma. This novel sample preparation method can therefore offer an improved approach with wider applicability providing \"cleaner\" extracts than other methods used for high-throughput clinical analysis.
摘要：
准确测量复杂样品的成分是日常生活中使用的一系列产品的安全性和有效性的关键，样品制备是此工作流程中的关键步骤。QuEChERS就是这样一种方法，然而，公布的协议没有明确解决酸性问题，基本的，中性,和两亲性物种在一个单一的方案，并经常使用额外的步骤或替代准备来恢复化学类型的广度。我们的工作通过研究QuEChERS用于监测环境固体和血浆中的广泛化学物质的使用来满足这一需求。使用可以容纳毫升和微升样品体积的方案。虽然已发布的方法可能需要大量的资源和时间，我们的方法减少了制备时间(对于环境样品)，与“micro-QuEChERS”协议提供了进一步降低成本。使用反相LC-MS评估了这些方法的分析性能，并显示出良好的准确性，精度,和灵敏度的预期浓度在测试的应用。从土壤中提取并分离了亲油性/酸度可变的目标分析物，具有基本上可重复的基体效应<15%RSD和39-100%的回收率。使用“micro-QuEChERS”协议进行的初步“概念验证”调查显示，土壤的基质增强（中值为90％ME）降低，并改善基质效应和血浆回收率(>65%)。因此，这种新颖的样品制备方法可以提供一种改进的方法，该方法具有更广泛的适用性，比其他用于高通量临床分析的方法提供“更清洁”的提取物。
