3M Environmental Laboratory, 3M Center, Building 0260-05-N-17, St. Paul, MN 55144-1000, USA.
Anal Chim Acta. 2011 Jan 10;683(2):248-57. doi: 10.1016/j.aca.2010.10.028. Epub 2010 Nov 3.
We report herein a simple protein precipitation extraction-liquid chromatography tandem mass spectrometry (LC/MS/MS) method, validation, and application for the analysis of perfluorinated carboxylic acids (C7-C12), perfluorinated sulfonic acids (C4, C6, and C8), and perfluorooctane sulfonamide (FOSA) in fish fillet tissue. The method combines a rapid homogenization and protein precipitation tissue extraction procedure using stable-isotope internal standard (IS) calibration. Method validation in bluegill (Lepomis macrochirus) fillet tissue evaluated the following: (1) method accuracy and precision in both extracted matrix-matched calibration and solvent (unextracted) calibration, (2) quantitation of mixed branched and linear isomers of perfluorooctanoate (PFOA) and perfluorooctanesulfonate (PFOS) with linear isomer calibration, (3) quantitation of low level (ppb) perfluorinated compounds (PFCs) in the presence of high level (ppm) PFOS, and (4) specificity from matrix interferences. Both calibration techniques produced method accuracy of at least 100±13% with a precision (%RSD) ≤18% for all target analytes. Method accuracy and precision results for fillet samples from nine different fish species taken from the Mississippi River in 2008 and 2009 are also presented.
我们在此报告了一种简单的蛋白质沉淀提取-液相色谱串联质谱（LC/MS/MS）方法，该方法经过验证并应用于鱼肉组织中全氟羧酸（C7-C12）、全氟磺酸（C4、C6 和 C8）和全氟辛烷磺酰胺（FOSA）的分析。该方法结合了使用稳定同位素内标（IS）校准的快速均化和蛋白质沉淀组织提取程序。在蓝鳃太阳鱼（Lepomis macrochirus）鱼片组织中的方法验证评估了以下内容：（1）在提取基质匹配校准和溶剂（未提取）校准中方法的准确性和精密度；（2）使用线性异构体校准对全氟辛酸（PFOA）和全氟辛烷磺酸（PFOS）的混合支链和线性异构体进行定量；（3）在存在高浓度（ppm）PFOS 的情况下对低浓度（ppb）全氟化合物（PFC）进行定量；（4）来自基质干扰的特异性。对于所有目标分析物，这两种校准技术均产生了至少 100±13%的方法准确性和≤18%的精密度（%RSD）。还介绍了 2008 年和 2009 年从密西西比河采集的 9 种不同鱼类鱼片样本的方法准确性和精密度结果。
