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Application of a Novel Large-Volume Injection Method Using a Stomach-Shaped Inlet Liner in Capillary Gas Chromatographic Trace Analysis of Dioxins in Human Milk and Plasma

机译:胃形进样口的新型大体积进样方法在人奶和血浆中二恶英的毛细管气相色谱痕量分析中的应用

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A newly developed large-volume injection (LVI) technique that employs a unique stomach-shaped inlet liner (SSIL) inside of a programmable temperature vaporizer was used for the determination of trace amounts of dioxins in human milk and plasma. The initial temperature and the initial dwelling time of the inlet and the kind of solvent used were found to be critical in determining the analytical sensitivity of dioxins due to the loss of these relatively volatile compounds during solvent vaporization. Human milk and plasma were purified and fractionated by pre-packed multi-layered silica-gel chromatography and activated carbon silica-gel column chromatography. A 20-µL aliquot of the fraction collected from the chromatography with toluene was directly applied to the LVI system in high-resolution gas chromatography/high-resolution mass spectrometry. Excellent correlation (r 0.97) between the values obtained by the LVI method using the SSIL device and those by the conventional regular-volume splitless injection method was obtained for PCDDs, PCDFs and non-ortho PCBs in human milk and plasma samples.
机译:一种新开发的大容量注射(LVI)技术,该技术在可编程温度蒸发器内部采用了独特的胃形入口衬里(SSIL),用于测定母乳和血浆中的痕量二恶英。已发现进样口的初始温度和初始停留时间以及所用溶剂的种类对于确定二恶英的分析灵敏度至关重要,这是由于溶剂蒸发过程中这些相对挥发性化合物的损失所致。人乳和血浆通过预装的多层硅胶色谱和活性炭硅胶柱色谱进行纯化和分级分离。从甲苯色谱法中收集的馏分的20 µL等分试样直接用于高分辨率气相色谱/高分辨率质谱法中的LVI系统。对于人乳和血浆样品中的PCDD,PCDF和非邻苯二甲酸多氯联苯,使用SSIL装置的LVI方法获得的值与常规常规体积不分流进样方法获得的值之间具有极好的相关性(r> 0.97)。

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