Jump to Main Content
Analysis of dinitro- and amino-nitro-toluenesulfonic acids in groundwater by solid-phase extraction and liquid chromatography–mass spectrometry
- Ma, Wai-Tang, Steinbach, Klaus, Cai, Zongwei
- Analytical and bioanalytical chemistry 2004 v.378 no.7 pp. 1828-1835
- composite polymers, detection limit, formic acid, groundwater, high performance liquid chromatography, ionization, ions, nitric oxide, nitrogen dioxide, solid phase extraction, sulfur dioxide, tandem mass spectrometry, wells, Germany
- A reversed-phase LC–MS method with quadrupole-time of flight (QTOF) detection has been developed for the determination of four dinitro-toluenesulfonic acids and two amino-nitro-toluenesulfonic acids in groundwater. The analytes were separated by HPLC with 0.1% (v/v) formic acid as mobile phase modifier compatible with mass spectrometric detection. QTOF-MS analysis with negative ion electrospray ionization afforded good selectivity and sensitivity for analysis of the dinitro- and amino-nitro-toluenesulfonic acids. Structure elucidation and confirmation were accomplished by tandem mass spectrometry. Characteristic ions resulting from the loss of NO, NO₂, and SO₂ from the [M−H]⁻ ions were detected. An intense fragment ion at m/z 80 representing the [SO₃]⁻ ion was detected for all dinitro- and amino-nitro-toluenesulfonic acids. Solid-phase extraction using a co-polymer cartridge was developed for preconcentration of the analytes from water. Good recovery (>85%) was achieved when 0.1% formic acid was added into the water samples before extraction. Method detection limits ranged from 10 to 76 ng L⁻¹ for the targeted compounds when 10 mL water was analyzed. Groundwater samples collected from wells close to a former ammunition plant in Stadtallendorf, Germany, were analyzed for the dinitro- and amino-nitro-toluenesulfonic acids.