Division of Environmental Health and Occupational Medicine, National Health Research Institutes, Zhunan, Miaoli County, Taiwan, ROC.
Talanta. 2010 Sep 15;82(4):1434-8. doi: 10.1016/j.talanta.2010.07.015. Epub 2010 Jul 13.
A method using automated on-line solid-phase extraction (SPE) liquid chromatography-electrospray tandem mass spectrometry (LC-ESI-MS/MS) for the determination of 8-iso-PGF2alpha in human exhaled breath condensate (EBC) was developed and validated. A C18 SPE column with an affinity sorbent was used for on-line extraction. A C18 column was employed for LC separation and ESI-MS/MS was utilized for detection. 8-iso-PGF2alpha-d(4) was used as an internal standard for quantitative determination. The extraction, cleanup and analysis procedures were controlled by a fully automated six-port switch valve. Identification and quantification were based on the following transitions: m/z 353-->193 for 8-iso-PGF2alpha and m/z 357-->197 for 8-iso-PGF2alpha-d(4), respectively. Good recoveries from 98.94 to 99.86% were measured and satisfactory linear ranges for these analytical compounds were determined. Intra-day and inter-day precision showed that coefficients of variance (CV) ranged from 6.5 to 8.0% and 5.2 to 6.3%, respectively. The applicability of this newly developed method was demonstrated by analyzing human EBC samples for an evaluation of the future risk of human exposure to nanoparticles.
建立并验证了一种采用自动化在线固相萃取(SPE)-液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)测定人呼出气冷凝液(EBC)中 8-异前列腺素 F2α(8-iso-PGF2α)的方法。采用带亲和吸附剂的 C18 SPE 柱进行在线萃取,C18 柱用于 LC 分离,ESI-MS/MS 用于检测。8-iso-PGF2α-d(4)被用作定量测定的内标。提取、净化和分析过程由全自动六通切换阀控制。鉴定和定量基于以下转变:m/z 353→193 用于 8-iso-PGF2α,m/z 357→197 用于 8-iso-PGF2α-d(4)。回收率良好,范围为 98.94%99.86%,这些分析物的线性范围也令人满意。日内和日间精密度表明,变异系数(CV)分别在 6.5%8.0%和 5.2%~6.3%之间。该方法可用于分析人 EBC 样本,以评估人类暴露于纳米颗粒的未来风险,从而证明了其适用性。