A suspect screening analysis for contaminants of emerging concern in municipal wastewater and surface water using liquid-liquid extraction and stir bar sorptive extraction.,Analytical Methods

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A suspect screening analysis for contaminants of emerging concern in municipal wastewater and surface water using liquid-liquid extraction and stir bar sorptive extraction.
Analytical Methods ( IF 2.7 ) Pub Date : 2020-08-26 , DOI: 10.1039/d0ay01179g
Kyra A Murrell ₁ , Frank L Dorman

Affiliation

The presence of contaminants of emerging concern (CECs) in wastewater effluent and surface waters is an important field of research for analytical scientists. This study takes a suspect screening approach to wastewater and surface water analysis using comprehensive two-dimensional gas chromatography with time-of-flight mass spectrometry (GC × GC-TOFMS). Two extraction procedures, traditional liquid–liquid extraction (LLE) and stir bar sorptive extraction (SBSE), were utilized and evaluated for their application to wastewater and surface water samples. Both techniques were evaluated regarding their recovery rates, range of compound classes extracted, and on their application to discovery of CECs. For the 14 surrogate compounds analyzed, LLE was able to extract all of them in each matrix with a recovery range of 19% to 159% and a median value of 74%. For SBSE, the recovery rates ranged from 19% to 117% with the median value at 66%, but only 8 of the compounds were able to be extracted because of the polarity bias for this extraction method. A new method of SBSE calibration was also developed using direct liquid injection of the internal standards before desorption of the stir bars. Initial findings indicate increased sensitivity and a greater range of unknown analyte recovery for SBSE, especially in the more dilute effluent and surface water samples. With the methods used in this study, SBSE has a concentration factor of approximately 416, improving that of LLE, which is 267. Suspect screening analysis was utilized to tentatively identify 32 CECs in the samples, the majority of which were pharmaceuticals and personal care products. More CECs were found using SBSE than LLE, especially in the surface water samples where 13 CECs were tentatively identified in the SBSE samples compared to 6 in the LLE samples.

中文翻译：

使用液-液萃取和搅拌棒吸附萃取对市政废水和地表水中新出现的污染物进行可疑筛查分析。

废水和地表水中新兴关注污染物（CEC）的存在是分析科学家研究的重要领域。这项研究采用了一种可疑的筛选方法，即使用具有飞行时间质谱（GC×GC-TOFMS）的全面二维气相色谱法对废水和地表水进行分析。利用了两种萃取程序，即传统的液液萃取（LLE）和搅拌棒吸附萃取（SBSE），并评估了它们在废水和地表水样品中的应用。评估了这两种技术的回收率，提取的化合物类别的范围以及它们在发现CEC中的应用。对于分析的14种替代化合物，LLE能够在每个基质中提取所有这些替代化合物，回收率范围为19％至159％，中位数为74％。对于SBSE，回收率介于19％至117％之间，中位数为66％，但由于该萃取方法的极性偏差，只能萃取8种化合物。还开发了一种新的SBSE校准方法，该方法是在搅拌棒解吸之前直接注入内标物。初步发现表明，SBSE的灵敏度提高了，未知分析物回收的范围也更大，尤其是在更稀释的废水和地表水样品中。通过本研究中使用的方法，SBSE的浓缩系数约为416，改善了LLE的浓缩系数，为267。利用可疑筛查分析初步确定了样品中的32个CEC，其中大多数是药品和个人护理产品。使用SBSE发现的CEC多于LLE，

更新日期：2020-09-24

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