Analysis of 2,2,2-trifluoroethyl derivatives of carboxylic acid herbicides by gas chromatography with mass-selective and electron capture detection.

A method for derivatizing carboxylic acid herbicides with 2,2,2-trifluoroethanol (TFE) in preparation for gas chromatographic (GC) analysis was developed. Esterification efficiency was determined by GC with electron capture detection (ECD), and esters were identified by GC with mass-selective detection (MSD). On the basis of reaction temperature for optimum esterification efficiency, 13 common carboxylic acid herbicides were separated into 2 groups before reaction with TFE. TFE derivatization was optimized for simultaneous analyses by altering reaction temperature, re action time, and concentration of sulfuric acid in reaction solutions. The method is simple, safe, and economical, and it gives good resolution without a laborious cleanup. Recovery of 13 analytes from water, taken from a pesticide residue well, was greater than 80% for all except 2 analytes. The well-water was fortified with analytes at the lower microgram-per-liter concentrations required for detection of pesticide residues in potable water systems. The method can simultaneously determine multiple herbicide residues in water samples with a high degree of accuracy and precision.