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采用鼓泡辅助分散液液微萃取与水相固化法测定水样中的多溴联苯醚。

Determination of Polybrominated Diphenyl Ethers in Water Samples Using Effervescent-Assisted Dispersive Liquid-Liquid Icroextraction with Solidification of the Aqueous Phase.

机构信息

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.

出版信息

Molecules. 2021 Mar 4;26(5):1376. doi: 10.3390/molecules26051376.

Abstract

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.

摘要

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。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/e69b/7961388/2381d7a5dbbf/molecules-26-01376-g001.jpg

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