Grupo de Investigación y Desarrollo en Química Analítica, Av. Ruiz Leal S/N, Parque General San Martín, 5500 Mendoza, Argentina.
Talanta. 2010 Jun 30;82(1):359-66. doi: 10.1016/j.talanta.2010.04.050. Epub 2010 May 20.
Ultrasound-assisted leaching-dispersive solid-phase extraction followed by dispersive liquid-liquid microextraction (USAL-DSPE-DLLME) technique has been developed as a new analytical approach for extracting, cleaning up and preconcentrating polybrominated diphenyl ethers (PBDEs) from sediment samples prior gas chromatography-tandem mass spectrometry (GC-MS/MS) analysis. In the first place, PBDEs were leached from sediment samples by using acetone. This extract was cleaned-up by DSPE using activated silica gel as sorbent material. After clean-up, PBDEs were preconcentrated by using DLLME technique. Thus, 1 mL acetone extract (disperser solvent) and 60 microL carbon tetrachloride (extraction solvent) were added to 5 mL ultrapure water and a DLLME technique was applied. Several variables that govern the proposed technique were studied and optimized. Under optimum conditions, the method detection limits (MDLs) of PBDEs calculated as three times the signal-to-noise ratio (S/N) were within the range 0.02-0.06 ng g(-1). The relative standard deviations (RSDs) for five replicates were <9.8%. The calibration graphs were linear within the concentration range of 0.07-1000 ng g(-1) for BDE-47, 0.09-1000 ng g(-1) for BDE-100, 0.10-1000 ng g(-1) for BDE-99 and 0.19-1000 ng g(-1) for BDE-153 and the coefficients of estimation were > or =0.9991. Validation of the methodology was carried out by standard addition method at two concentration levels (0.25 and 1 ng g(-1)) and by comparing with a reference Soxhlet technique. Recovery values were > or =80%, which showed a satisfactory robustness of the analytical methodology for determination of low PBDEs concentration in sediment samples.
超声辅助浸取-分散固相萃取结合分散液液微萃取（USAL-DSPE-DLLME）技术已被开发为一种新的分析方法，用于从沉积物样品中提取、净化和预浓缩多溴二苯醚（PBDEs），然后进行气相色谱-串联质谱（GC-MS/MS）分析。首先，使用丙酮从沉积物样品中浸提 PBDEs。该提取物通过 DSPE 使用活化硅胶作为吸附材料进行净化。净化后，通过 DLLME 技术对 PBDEs 进行预浓缩。因此，将 1 mL 丙酮提取液（分散溶剂）和 60 μL 四氯化碳（萃取溶剂）加入 5 mL 超纯水中，并应用 DLLME 技术。研究并优化了控制该方法的几个变量。在最佳条件下，计算 PBDEs 的方法检测限（MDLs）作为信噪比（S/N）的三倍，范围为 0.02-0.06 ng g(-1)。五个重复的相对标准偏差（RSDs）<9.8%。校准曲线在 BDE-47 的浓度范围为 0.07-1000 ng g(-1)、BDE-100 的浓度范围为 0.09-1000 ng g(-1)、BDE-99 的浓度范围为 0.10-1000 ng g(-1)和 BDE-153 的浓度范围为 0.19-1000 ng g(-1)时呈线性，估计系数> =0.9991。通过在两个浓度水平（0.25 和 1 ng g(-1))进行标准添加法和与参考索氏萃取技术进行比较，对方法进行了验证。回收率> =80%，表明该分析方法对于测定沉积物样品中低浓度 PBDEs 具有令人满意的稳健性。
