Department of Chemistry, University of La Rioja, C/Madre de Dios 51, E-26006 Logroño (La Rioja), Spain.
J Chromatogr A. 2013 Aug 9;1302:88-94. doi: 10.1016/j.chroma.2013.06.024. Epub 2013 Jun 19.
A focused ultrasound solid-liquid extraction (FUSLE) and liquid chromatography (HPLC) coupled to quadrupole-time of flight mass spectrometry (QTOF-MS/MS) based method is proposed to determine six perfluorocarboxylic acids (PFCA) and perfluorooctane sulfonate (PFOS) in food-contact packaging. FUSLE, a simple, inexpensive and fast extraction technique, has been carried out with just 8mL of ethanol in one cycle of only 10s. The whole method presented good repeatability and intermediate precision, with RSDs below 11% and 15%, respectively; limits of detection, with values between 0.5ng/g and 2.2ng/g, and successful recovery values, around 100% in all cases. The developed method has been validated and applied to the analysis of real food-contact packaging samples. FUSLE results have been compared to those obtained with pressurized liquid extraction (PLE) and no significant differences between them have been found. PFAA were detected in all the packaging samples analyzed, in a concentration range between 4ng/g and 29ng/g, being PFHpA (perfluoroheptanoic acid) the most abundant of them.
一种基于聚焦超声固液萃取（FUSLE）和液相色谱（HPLC）与四极杆飞行时间质谱（QTOF-MS/MS）联用的方法，用于测定食品接触包装材料中的六种全氟羧酸（PFCA）和全氟辛烷磺酸（PFOS）。FUSLE 是一种简单、廉价和快速的萃取技术，仅在一个 10 秒的循环中使用 8mL 乙醇即可完成。该方法具有良好的重复性和中间精密度，相对标准偏差（RSD）分别低于 11%和 15%；检测限（LOD）在 0.5ng/g 至 2.2ng/g 之间，回收率均在 100%左右。该方法已经过验证，并应用于实际食品接触包装样品的分析。FUSLE 的结果与加压液体萃取（PLE）的结果进行了比较，两者之间没有显著差异。在所分析的所有包装样品中均检测到了全氟羧酸，浓度范围在 4ng/g 至 29ng/g 之间，其中 PFHpA（全氟庚酸）的含量最丰富。
