The Macaulay Land Use Research Institute, Craigiebuckler, Aberdeen AB158QH, UK.
J Chromatogr A. 2011 Feb 25;1218(8):1203-9. doi: 10.1016/j.chroma.2010.12.098. Epub 2011 Jan 1.
We describe a selective pressurized liquid extraction (SPLE) method, followed by gas chromatography-mass spectrometry (GC-MS), for the simultaneous extraction and clean-up of polybrominated diphenyl ethers (PBDEs) and polychlorinated biphenyls (PCBs) in sheep liver tissue samples. The on-line clean-up of liver tissue by SPLE was tested using differing amount of acid-modified silica (sulphuric acid:silica gel, 1:2, w/w), the most effective amount being 20 g. Different extraction solvents (iso-hexane and dichloromethane), either alone or in various combinations, were used to extract these target compounds from spiked liver samples. Variables affecting the SPLE extraction efficiency, including temperature, pressure, number of extraction cycles and static extraction time were studied; the optimum parameters were 80 °C, 10.3 MPa, 2 cycles and 5 min, respectively. The SPLE based method was compared with more traditional Soxhlet, off-line PLE, ultrasonic and heating extraction methods. Overall the mean percentage recoveries for all target chemicals using SPLE were 86-103% (n=3, SD < 9%), and compared favourably with the Soxhlet (63-109%, n=3, SD < 8%), off-line PLE (82-104%, n=3, SD < 18%), ultrasonic (86-99%, n=3, SD < 11%) and heating (72-102%, n=3, SD < 21%) extraction methods. The limits of detection of the proposed method were 5-96 pg g⁻¹ and 2-29 pg g⁻¹ for the different PBDE and PCB chemicals studied, respectively. The outputs of the proposed method were linear over the range from 0.02 to 30 ng g⁻¹, for all PCB and PBDE congeners except for PBDE 100 and 153 (0.05-30 ng g⁻¹) and PBDE 183 (0.1-30 ng g⁻¹). The method was successfully applied to sheep liver samples for the determination of the target PBDE and PCB compounds.
我们描述了一种选择性加压液体萃取（SPLE）方法，结合气相色谱-质谱（GC-MS），用于同时提取和净化绵羊肝组织样品中的多溴二苯醚（PBDEs）和多氯联苯（PCBs）。通过 SPLE 对肝组织进行在线净化，使用不同量的酸改性硅胶（硫酸：硅胶，1:2，w/w）进行了测试，最有效的量为 20g。使用不同的提取溶剂（异己烷和二氯甲烷），单独或组合使用，从加标肝样品中提取这些目标化合物。研究了影响 SPLE 萃取效率的变量，包括温度、压力、萃取循环次数和静态萃取时间；最佳参数分别为 80°C、10.3MPa、2 个循环和 5min。将基于 SPLE 的方法与更传统的索氏提取、离线加压液体萃取、超声和加热提取方法进行了比较。总体而言，使用 SPLE 提取所有目标化学物质的平均回收率为 86-103%（n=3，SD<9%），与索氏提取（63-109%，n=3，SD<8%）、离线加压液体萃取（82-104%，n=3，SD<18%）、超声（86-99%，n=3，SD<11%）和加热（72-102%，n=3，SD<21%）提取方法相比具有优势。该方法的检出限为 5-96pg g⁻¹和 2-29pg g⁻¹，分别用于研究的不同 PBDE 和 PCB 化学物质。该方法的输出在 0.02 至 30ng g⁻¹范围内呈线性，除了 PBDE 100 和 153（0.05-30ng g⁻¹）和 PBDE 183（0.1-30ng g⁻¹）外，所有 PCB 和 PBDE 同系物的检出限均为 0.02 至 30ng g⁻¹。该方法成功应用于绵羊肝组织样品中目标 PBDE 和 PCB 化合物的测定。
