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Quantitative Determination of Bisphenol A from Human Saliva by Bulk Derivatization and Trap-and-Elute HPLC-ESI-MS

机译:通过散衍衍生化和陷阱 - 洗脱液HPLC-ESI-MS对人唾液中双酚A的定量测定

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Use of bulk derivatization in conjunction with restricted access media (RAM) allowed for expedited sample preparation relative to traditional methods while still imparting high recovery levels with enhanced sensitivity. Extensive optimization was conducted on the bulk derivatization reaction as well as the sample preparation protocol in order to reach the optimal conditions outlined in the finalized procedure. Bulk derivatization and RAM also provides a route for the integration of the entire procedure towards a fully automated online quantitative method. Three separate validated methods (a single 5 (mu)L injection method, a multiple injection loading (3 X 20 (mu)L) method, and MIL method with an internal standard) are presented for the detection of trace levels of BPA from human saliva. Two applications of trace BPA analysis from canned food goods are presented demonstrating the viability of these validate methods in a real-world scenario. The detected concentrations of BPA from the canned green chili salsa from Mexico were below the reported limit of detection from method validation. However, the concentrations detected from the hot and sour soup from Taiwan were well within the limit of detection as well as the limit of quantification.
机译:使用散装衍生化与限制的接入介质(RAM)相对于传统方法加速样品制备,同时仍然赋予具有增强灵敏度的高恢复水平。在大量衍生化反应以及样品制备方案上进行了广泛的优化,以达到最终过程中概述的最佳条件。批量衍生化和RAM还提供了一条途径,用于整合整个过程朝向全自动在线定量方法。三种单独的验证方法(单个5(mU)L注射方法,呈现多喷射载荷(3×20(mu))和具有内标的MIL方法),用于检测来自人的痕量BPA唾液。提出了两种痕量BPA分析从罐头食品中的应用,证明了这些验证方法在真实世界的情况下的可行性。从墨西哥罐装绿辣椒辣酱盐的检测到的BPA浓度低于报告的方法验证的检测极限。然而,从台湾的热和酸汤中检测到的浓度在检测极限内很好,以及量化的限制。

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