Extending the use of USEPA method 1625 for the analysis of 4,4′-DDT, 4,4′-DDD, and 4,4′-DDE

Add time:07/19/2019    Source:sciencedirect.com

This paper describes an isotope dilution GC/MS technique for the analysis of low-partsper-trillion (ppt) concentrations of 4,4′-DDT, 4,4′-DDD, and 4,4′-DDE in waters and soils. These pesticides are known to be pervasive and dangerous. Known amounts of stable labeled isotopes such as 4,4′-DDT-d8, 4,4′-DDD-d8, and 4,4′-DDE-d8 were spiked into each sample prior to extraction. The water samples were extracted with methylene chloride. The soil samples were extracted initially with a mixture of acetone and methylene chloride. Analyses were performed on a high-resolution GC/low resolution MS with the mass spectrometer operated in the selected ion monitoring mode (SIM). Accuracy greater than 90% and precision better than 6% were demonstrated by use of the spiked samples. This technique has been used successfully in the analysis of 100 water samples and 50 soil samples. Those samples showing less than the detection limit were “spiked” with pure 4,4′-DDT, 4,4′-DDD, and 4,4′-DDE, and then rerun to ensure that the analysis was not faulty. Detection limits of 0.1–1.0 ppb (parts per billion) were achieved for the test compounds by selected ion monitoring GC/MS.

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