College of Food Sciences, Shanghai Ocean University, Shanghai 201306, China.
Institute for Agro-food Standards and Testing Technology, Shanghai Academy of Agricultural Science, Shanghai 201403, China.
Molecules. 2021 Mar 4;26(5):1376. doi: 10.3390/molecules26051376.
An effective and sensitive method is necessary for the determination of polybrominated diphenyl ethers (PBDEs) pollutants in water. In this study, effervescent-assisted dispersive liquid-liquid microextraction with solidification of the aqueous phase (EA-DLLME-SAP), followed by Gas Chromatography-Tandem Mass Spectrometry (GC-MS-MS) quantitative analysis, was established for the preconcentration and determination of PBDEs in real environmental water samples. 1,1,2,2-Tetrachloroethane was used as the extractant and directly dispersed into the water phase of the aqueous samples with the aid of a large number of carbon dioxide bubbles generated via the acid-base reaction of acetic acid and sodium bicarbonate, which did not require the use of a dispersant during the extraction process. The key factors affecting the extraction recovery were optimized, and an internal standard was used for quantitative analysis, which gave good linearity ranges of 1-100 ng·L (BDEs 28, 47, 99, and 100), 2-200 ng·L (BDEs 153, 154, and 183) and 5-500 ng·L (BDE 209) with limits of quantification in the range of 1.0-5.0 ng·L. The accuracy was verified with relative standard deviations < 8.5% observed in tap, lake, river and reservoir water samples with relative recoveries ranging from 67.2 to 102.6%. The presented method contributes to the determination of PBDEs in environmental water samples.
一种有效且灵敏的方法对于水中多溴二苯醚（PBDEs）污染物的测定是必要的。在本研究中，建立了鼓泡辅助分散液-液微萃取结合水相固化（EA-DLLME-SAP），随后采用气相色谱-串联质谱（GC-MS-MS）定量分析，用于实际环境水样中 PBDEs 的预浓缩和测定。1,1,2,2-四氯乙烷被用作萃取剂，并在大量二氧化碳气泡的辅助下直接分散到水样的水相中，这些二氧化碳气泡是通过乙酸和碳酸氢钠的酸碱反应产生的，在萃取过程中不需要使用分散剂。优化了影响萃取回收率的关键因素，并使用内标进行定量分析，得到了良好的线性范围，BDEs 28、47、99 和 100 的线性范围为 1-100ng·L（BDEs 28、47、99 和 100），BDEs 153、154 和 183 的线性范围为 2-200ng·L，BDE 209 的线性范围为 5-500ng·L，定量限在 1.0-5.0ng·L 范围内。在自来水中、湖泊、河流和水库水样中，相对标准偏差<8.5%，相对回收率在 67.2%至 102.6%之间，验证了该方法的准确性。该方法有助于环境水样中 PBDEs 的测定。
