Abstract:
We developed a quantitative analytical method to detect four classes of surfactants, and the enantiomeric mixture of α- and β-ethylhexyl sulfosuccinate (α-/β-EHSS). The enantiomeric mixture of α-/β-EHSS is the hydrolysis product of bis-(2-ethylhexyl) sulfosuccinate (DOSS) The four surfactants studied were DOSS, Span 80, Tween 80, and Tween 85. These surfactants were used to study long term stability at a single temperature, short term stability at 3 temperatures, matrix effects, and recovery after filtration. Results were generated through sample analysis using liquid-chromatography tandem mass spectrometry (LC-MS/MS). These results are presented in the related paper: Place, B. J., Perkins, M. J., Sinclair, E., Barsamian, A. L., Blakemore, P. R., and Field, J. A. (2014). Trace analysis of surfactants in Corexit oil dispersant formulations and seawater. Deep Sea Research Part II: Topical Studies in Oceanography. doi:10.1016/j.dsr2.2014.01.015. The results of seawater analysis for surfactants are presented in the related dataset R1.x132.134:0036. [13C]4-α-EHSS and [13C]4-β-EHSS were synthesized in the lab due to their potential use as analytical standards and their constitutional isomers were analyzed using Nuclear Magnetic Resonance (NMR) spectroscopy in Fourier transform mode using 5 mm diameter tubes. 1H and 13C NMR spectra for the constitutional isomers of 13C EHSS (Sodium [13C]4-1-carboxy-2-(2-ethylhexyloxycarbonyl)ethanesulfonate (α-EHSS) and sodium [13C]4-2-carboxy-1-(2-ethylhexyloxycarbonyl)ethanesulfonate (β-EHSS) are provided in this dataset, as described in the paper: Barsamian, A. L., Perkins, M. J., Field, J. A., and Blakemore, P. R. (2014). Regioselective syntheses of [13C] 4 labelled sodium 1-carboxy-2(2-ethylhexyloxycarbonyl)ethanesulfonate and sodium 2-carboxy-1-(2-ethylhexyloxycarbonyl)ethanesulfonate from [13C] 4-maleic anhydride . Journal of Labelled Compounds and Radiopharmaceuticals, 57(5), 397–401. doi:10.1002/jlcr.3189
Data Parameters and Units:
Retention time on column (RT, min); Peak Area (Area, unitless); Internal Standard Area (IS Area, unitless); Response factor of instrument (Response, unitless), Conc. (concentration of analyte ug/L); Percent deviation (percent deviation of analyte off standard), limit of detection (LOD, ng/L), lower limit of quantification (LLOQ, ng/L), recovery (%); relative standard deviation of recovery (RSD, %), Depth (m), Analyte (analyte name), Retention Time (min), MS Polarity, Parent Ion (m/z), Daughter Ion (m/z), Cone Voltage (V), Collision Energy (V) limitof-detection.xlsx - limit of detection (LOD, ng/L), lower limit of quantification (LLOQ, ng/L), recovery (%); relative standard deviation of recovery (RSD, %) stability-of-analytes.xls - Stability of analytes in parent stock standards prepared in methanol (DOSS) and isopropanol (Span 80, Tween 80, Tween 85). Retention time on column (RT, min); Peak Area (Area, unitless); Internal Standard Area (IS Area, unitless); Response factor of instrument (Response, unitless), Conc. (concentration of analyte ug/L); Percent deviation (percent deviation of analyte off standard). individual-surfactant-components.xlsx - Short term stability of the individual surfactant components of Corexit in seawater : isopropanol (75:25). Stability of analytical standards in HPLC autosampler vials with/without 25% isopropanol. Solvent, Time in hours, normalized area (the resultant area counts divided by the largest area counts for that compound). LOD-and-LLOQ.xls - LOD and LLOQ for quantitative analysis of DOSS, Span 80, Tween 80, and Tween 85. Short-term-stability-analytes.xlsx - Short-term stability (≤13h) of analytes in seawater in HDPE centrifuge tubes at various temperatures. Time (hours), Average concentration (ug/L), SD, Loss from T0, SD, 95%Cl, temperature, analyte. matrix-effects-on-the-non-ionics.xlsx - normalized peak area counts, of nonionic analytes (DOSS, 13DOSS, Span 80, Tween 80, Tween 85, EHSS) prepared in buffered water (0.5 mM ammonium acetate) (Buffer), Instant Ocean (IO), and Oregon Coast (ORC) water. Columns 1-4 for each matrix are replicates followed by the mean and relative standard deviation. stability-of-analytical-standards.xls - Stability of analytical standards in HPLC autosampler vials with/without 25% isopropanol, RT (retention time), area, Normalized area (resultant area counts divided by the largest area counts for that compound). recovery-of-all-analytes.xls - Recovery of all analytes before and after filtration through a Sterivex 0.2-μm sterilization filter. RT (retention time), area, IS area, peak end, peak start. quantitative-analysis-of-EHSS.xlsx: Accuracy and precision worksheet: vial concentration, RT, area, IS area, response, concentration; LOD LLOQ worksheet: raw data for low level cal curve; short term stability - sample text, S/N, normalized concentration, time: matrix effects: buffered water, instant ocean, Oregon coast water, RT, area, IS, response, detection flag, concentration (ng/L), normalized area. MS-Parameters-analytes.xlsx - MS Parameters for the detection of all analytes. * indicates secondary MRM transitions used for analyte verification. Analyte Retention Time (min) MS Polarity Scan Mode Parent Ion (m/z) Daughter Ion (m/z) Cone Voltage (V) Collision Energy (V) NMR-spectra-12C-13C (folder)- 1H and 13C NMR spectra, field strength (MHz)
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