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Rapid ultra-trace analysis of sucralose in multiple-origin aqueous samples by online solid-phase extraction coupled to high-resolution mass spectrometry

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Abstract

Because of its widespread consumption and its persistence during wastewater treatment, the artificial sweetener sucralose has gained considerable interest as a proxy to detect wastewater intrusion into usable water resources. The molecular resilience of this compound dictates that coastal and oceanic waters are the final recipient of this compound with unknown effects on ecosystems. Furthermore, no suitable methodologies have been reported for routine, ultra-trace detection of sucralose in seawater as the sensitivity of traditional liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis is limited by a low yield of product ions upon collision-induced dissociation (CID). In this work, we report the development and field test of an alternative analysis tool for sucralose in environmental waters, with enough sensitivity for the proper quantitation and confirmation of this analyte in seawater. The methodology is based on automated online solid-phase extraction (SPE) and high-resolving-power orbitrap MS detection. Operating in full scan (no CID), detection of the unique isotopic pattern (100:96:31 for [M−H]−, [M−H+2]−, and [M−H+4]−, respectively) was used for ultra-trace quantitation and analyte identification. The method offers fast analysis (14 min per run) and low sample consumption (10 mL per sample) with method detection and confirmation limits (MDLs and MCLs) of 1.4 and 5.7 ng/L in seawater, respectively. The methodology involves low operating costs due to virtually no sample preparation steps or consumables. As an application example, samples were collected from 17 oceanic and estuarine sites in Broward County, FL, with varying salinity (6–40 PSU). Samples included the ocean outfall of the Southern Regional Wastewater Treatment Plant (WWTP) that serves Hollywood, FL. Sucralose was detected above MCL in 78 % of the samples at concentrations ranging from 8 to 148 ng/L, with the exception of the WWTP ocean outfall (at pipe end, 28 m below the surface) where the measured concentration was 8418 ± 3813 ng/L. These results demonstrate the applicability of this monitoring tool for the trace-level detection of this wastewater marker in very dilute environmental waters.

Ultra-trace detection of the intact sucralose anion and it isotopic signature in waters using online SPE and orbitrap HRMS

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Acknowledgments

The authors want to gratefully acknowledge Dr. Ken Banks and Dr. Nancy Craig from Broward County Natural Resources Planning and Management Division, Environmental Protection and Growth Management Department (EPGMD-NRPMD), for providing the logistic support needed for sample collection. We also acknowledge the support from the Thermo Scientific Corporation in the development of this work. This is contribution number 715 from the Southeast Environmental Research Center at Florida International University.

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Authors and Affiliations

  1. Department of Chemistry and Biochemistry, Florida International University, Miami, FL, 33199, USA

    Cesar E. Ramirez & Piero R. Gardinali

  2. Southeast Environmental Research Center, Florida International University, 3000 NE 151 ST, MSB 350, North Miami Beach, FL, 33181, USA

    Sudha Rani Batchu, Cesar E. Ramirez & Piero R. Gardinali

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  1. Sudha Rani Batchu
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  2. Cesar E. Ramirez
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  3. Piero R. Gardinali
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Correspondence to Cesar E. Ramirez.

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Batchu, S.R., Ramirez, C.E. & Gardinali, P.R. Rapid ultra-trace analysis of sucralose in multiple-origin aqueous samples by online solid-phase extraction coupled to high-resolution mass spectrometry. Anal Bioanal Chem 407, 3717–3725 (2015). https://doi.org/10.1007/s00216-015-8593-6

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  • DOI: https://doi.org/10.1007/s00216-015-8593-6

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