On April 22, 2010, the explosion on and subsequent sinking of the Deepwater Horizon oil drilling platform resulted in the release of crude oil into the Gulf of Mexico. At least 4.4 million barrels had been released into the Gulf of Mexico through July 15, 2010, 10 to 29 percent of which was chemically dispersed, primarily using two dispersant formulations. Initially, the dispersant Corexit 9527 was used, and when existing stocks of that formulation were exhausted, Corexit 9500 was used. Over 1.8 million gallons of the two dispersants were applied in the first 3 months after the spill. This report presents the development of an analytical method to analyze one of the primary surfactant components of both Corexit formulations, di(ethylhexyl) sodium sulfosuccinate (DOSS), the preliminary results, and the associated quality assurance/quality control (QA/QC) from samples collected from various points on the Gulf Coast between Texas and Florida. Seventy water samples and 8 field QC samples were collected before the predicted landfall of oil (pre-landfall) on the Gulf Coast, and 51 water samples and 10 field QC samples after the oil made landfall (post-landfall). Samples were collected in Teflon(Registered) bottles and stored at -20(degrees)C until analysis. Extraction of whole-water samples used sorption onto a polytetrafluoroethylene (PTFE) filter to isolate DOSS, with subsequent 50 percent methanol/water elution of the combined dissolved and particulate DOSS fractions. High-performance liquid chromatography/tandem mass spectrometry (LC/MS/MS) was used to identify and quantify DOSS by the isotope dilution method, using a custom-synthesized 13C4-DOSS labeled standard. Because of the ubiquitous presence of DOSS in laboratory reagent water, a chromatographic column was installed in the LC/MS/MS between the system pumps and the sample injector that separated this ambient background DOSS contamination from the sample DOSS, minimizing one source of blank contamination. Laboratory and field QA/QC for pre-landfall samples included laboratory reagent spike and blank samples, a total of 34 replicate analyses for the 78 environmental and field blank samples, and 11 randomly chosen laboratory matrix spike samples. Laboratory and field QA/QC for post-landfall samples included laboratory reagent spike and blank samples, a laboratory 'in-bottle' duplicate for each sample, and analysis of 24 randomly chosen laboratory matrix spike samples. Average DOSS recovery of 89(+/-)9.5 percent in all native (non-13C4-DOSS ) spikes was observed, with a mean relative percent difference between sample duplicates of 36 percent. The reporting limit for this analysis was 0.25 micrograms per liter due to blank limitations; DOSS was not detected in any samples collected in October (after oil landfall at certain study sites) above that concentration. It was detected prior to oil landfall above 0.25 micrograms per liter in 3 samples, but none exceeded the Environmental Protection Agency aquatic life criteria of 40 micrograms per liter.