Abstract A convenient method based on microwave-assisted hydrothermal extraction coupled to ion chromatography was proposed for comprehensive analysis of chemical composition in biological samples. Water was used as extraction solvent and a small amount of alkali or a small volume of acid was served as modifier to improve extraction efficiency. Factors affecting extraction efficiency were investigated using multi-response optimization method on the base of the Derringer’s desirability function. Owing to the specific role of microwave irradiation, the approach could greatly shorten sample treatment time, leading to high sample throughput. The lowest limits of quantification of procedure were 0.02 mg L −1 for F − , NO 3 − and cations, and 0.04 mg L −1 for five anions, respectively. Recoveries ranged from 85.7 to 110.0% with the relative standard deviations in the range of 0.95–4.6%. The strategy was successfully applied to the determination of elemental species of both an inorganic and organic nature in vesical, renal, and urethral stones. Thirteen compounds in human stone were accurately diagnosed resulting from elemental speciation in calculi could be well maintained in the extraction process. The proposed protocol could achieve batch samples pretreatment and provided a powerful tool for the analysis of intracorporeal calculi, which would be very beneficial for therapy and prevention recurrence of stone-forming patient. Graphic Abstract

中文翻译：

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微波辅助水热萃取结合离子色谱法的发展，用于综合分析体内结石中的化学成分

摘要 提出了一种基于微波辅助水热萃取结合离子色谱的简便方法，用于生物样品中化学成分的综合分析。以水为萃取溶剂，以少量碱或少量酸为改性剂，以提高萃取效率。基于Derringer的合意性函数，采用多响应优化方法研究了影响提取效率的因素。由于微波辐射的特殊作用，该方法可以大大缩短样品处理时间，从而提高样品通量。F - 、NO 3 - 和阳离子的最低定量限分别为0.02 mg L -1 和五个阴离子的0.04 mg L -1 。回收率从 85.7 到 110 不等。0%，相对标准偏差在 0.95-4.6% 的范围内。该策略已成功应用于测定膀胱结石、肾结石和尿道结石中的无机和有机元素种类。人石中的 13 种化合物被准确诊断，由结石中的元素形态形成，可以在提取过程中得到很好的保持。该方案可以实现批量样本预处理，为分析体内结石提供了有力的工具，对结石患者的治疗和预防复发非常有益。图形摘要 人石中的 13 种化合物被准确诊断，由结石中的元素形态形成，可以在提取过程中得到很好的保持。该方案可以实现批量样本预处理，为分析体内结石提供了有力的工具，对结石患者的治疗和预防复发非常有益。图形摘要 人石中的 13 种化合物被准确诊断，由结石中的元素形态形成，可以在提取过程中得到很好的保持。该方案可以实现批量样本预处理，为分析体内结石提供了有力的工具，对结石患者的治疗和预防复发非常有益。图形摘要