Development of a Dispersive Liquid-Liquid Microextraction Followed by LC-MS/MS for Determination of Benzotriazoles in Environmental Waters

Abstract

Emerging environmental pollutants are becoming a global concern, since the acceptable concentrations are currently not set by legislation in EU or elsewhere. Benzotriazoles are an important group of emerging pollutants found in low µg/L concentrations, entering the environment through wastewater treatment facilities due to their insufficient removal, and through industrial and other use. Two new dispersive liquid-liquid microextraction (DLLME) methods were developed for the extraction of hydrophilic and hydrophobic benzotriazoles from environmental waters. Liquid chromatographic method coupled to tandem mass spectrometric detection (LC-MS/MS) was developed and validated for surface water. Validation parameters were satisfactory and the overall DLLME-LC-MS/MS method was found to be applicable to analysis of the chosen analytes in environmental waters. It was used to determine benzotriazoles in surface water and wastewater from a municipal wastewater treatment plant. In surface waters, concentration was below the limit of detection, while concentrations determined in wastewater were estimated between 2.7 and 12.0 µg/L.

Bar Adsorptive Microextraction Coated with Carbon-Based Phase Mixtures for Performance-Enhancement to Monitor Selected Benzotriazoles, Benzothiazoles, and Benzenesulfonamides in Environmental Water Matrices

“…This can be attributed to the more polar nature of these compounds, making them more hydrophilic in comparison with the other target compounds. Nevertheless, by applying the developed methodology through SAM, it was possible to determine the presence of MeBT (11.9 µg L −1 ) and OHBTh (10.8 µg L −1 ) in the wastewater sample ( Figure 3 ), similar to values already reported in literature for similar matrices [ 1 , 8 , 29 ].…”

“…In the present work, we decided to compare the proposed methodology (BAµE(R, 12.5%/CN1, 87.5%)-µLD/HPLC-DAD) with other microextraction-based approaches proposed in the literature ( Table 2 ), including SPME [ 11 , 27 ], SBSE [ 10 ], DLLME [ 8 , 28 , 29 ], AALLME [ 9 ], gas chromatography coupled to mass spectrometry (GC-MS) [ 10 , 28 ] or tandem mass spectrometry (GC-MS/MS) [ 11 ], liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) [ 8 ] or quadrupole time-of-flight mass spectrometry (LC-qTOF/MS) [ 27 ], HPLC-ultraviolet detection (HPLC-UV) [ 9 ], as well as HPLC-fluorescence-ultraviolet detection (HPLC-FLD-UV) [ 29 ].…”

“…Several analytical methods have been proposed for the determination of these compounds in environmental water matrices [ 1 , 5 , 6 , 7 ], including microextraction-based techniques such as dispersive liquid-liquid microextraction (DLLME) [ 8 ], air assisted liquid-liquid microextraction (AALLME) [ 9 ], stir bar sorptive extraction (SBSE) [ 10 ], and solid phase microextraction (SPME) [ 11 ]. Nevertheless, these technologies present recovery and reproducibility limitations, since the most commonly used sorbents/solvents are devoted to the enrichment of semi-polar to non-polar compounds, of which BTRs, BTs, and BSDs are not (−1.74 ≤ log D ≤ 2.49; 2.0 ≤ matrix pH ≤ 11.0 [ 12 ]; Table S1 ).…”

Simultaneous Determination of Fifteen Polyphenols in Fruit Juice Using Ultrahigh-Performance Liquid Chromatography-Tandem Mass Spectrometry Combining Dispersive Liquid-Liquid Microextraction

“…Moreover, this technique has extra advantages over other liquid microextraction techniques in terms of rapidity, low cost, simplicity of operation, high recovery, and enrichment factor. So far, as a green and novel microextraction technique, DLLME has been successfully applied to the extraction and preconcentration of various compounds in food [ 29 ], medicine [ 30 ], environment [ 31 ], and other fields. However, there is no report about the enrichment of polyphenols in fruit juice.…”