Capillary electrophoresis determinative and LC-MS confirmatory method for screening selected imidazolinone herbicides from soil.
Residues of imazapyr, imazamox, imazapic, imazethapyr, imazaquin, and imazamethabenz (meta and para) are extracted from soil with 0.5 N sodium hydroxide. The pH is adjusted to 2.0-2.2, and the resulting precipitate is filtered. Compounds are trapped onto a tC18 solid-phase extraction (SPE) cartridge, then eluted from the cartridge and passed through a strong anion exchange (SAX) SPE cartridge onto a benzenesulfonic acid strong cation exchange (SCX) cartridge using ethyl acetate. After eluting the analytes from the SCX cartridge using saturated potassium chloride in methanol, the solution is evaporated and redissolved in 1% formic acid in water. The sample is then desalted using a tC18 SPE cartridge and eluted with methanol. After evaporating the methanol to dryness, the compounds are partitioned from acidic solution (pH 3.5) into methylene chloride. The methylene chloride is evaporated to dryness and the residues are then dissolved in Milli-Q water (Millipore, Bedford, MA, U.S.A.) in preparation for analysis by capillary electrophoresis. Results are calculated by direct comparison of the sample peak heights to the peak heights of bracketing standards. The validated sensitivity of the method (LOQ, limit of quantitation) is 2.0 ppb for each compound. Confirmation for individual residues greater than 2.0 ppb is provided by liquid chromatography-electrospray ionization mass spectrometry (LC-ESMS) of the final extract.
D002853:Chromatography, Liquid / Q000379:methods; D019075:Electrophoresis, Capillary / Q000379:methods*; D006540:Herbicides / Q000032:analysis*; D007093:Imidazoles / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods; D015394:Molecular Structure; D012987:Soil; D012989:Soil Pollutants / Q000032:analysis*