An analytical method for the determination of glyphosate and its principal metabolite, aminomethylphosphonic acid (AMPA), in water of different hardnesses (5, 20, and 30 degrees DH, french hardness) has been developed. Samples were fortified at different levels (0.05, 0.1, 1, and 5 microg/L) and were purified by column chromatography on ion-exchange resins. After derivatization with TFAA/HFB mixture, the derivatives were quantified by using capillary gas chromatography with an ion-trap tandem mass spectrometric detector. Analytical conditions for MS/MS detection were optimized, and the quantification was carried out on the sum of areas of the three most representative ions: m/z 283, 223, and 181 for AMPA and m/z 440, 321, and 261 for glyphosate. The limit of quantification was demonstrated to be at 0.05 microg/L for each compound. The mean recovery value and the relative standard deviation (n = 65) were 93 and 12% for AMPA and 95 and 13% for glyphosate.

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An analytical method for the determination of glufosinate ammonium and its principal metabolites, AE F064619 and AE F061517, in water of two different hardnesses (5 and 30 DH, French hardness) has been developed and validated. Samples were spiked at different levels (0. 05 and 0.5 microgram/L) and were purified by column chromatography on ion-exchange resins. After derivatization with glacial acetic acid and trimethylarthoacetate mixture, the derivatives were quantified by using capillary gas chromatography with an ion-trap tandem mass spectrometric detector. Analytical conditions for MS/MS detection were optimized, and the quantification was carried out on the areas of the most representative ions. The limit of quantification was validated at 0.05 microgram/L for each compound. The mean recovery value and the relative standard deviation (n = 20) were 92.0% and 17. 8% for glufosinate ammonium, 90.2% and 15.8% for AE F064619, and 89. 7% and 12.7% for AE F061517.

The determination of dithiocarbamates in plant matrixes is generally carried out by spectrophotometric (European Norm EN 12396-1, 1996) or gas chromatography headspace (European Norm EN 12396-2, 1999) methods. However, the former method presents a risk of carbon disulfide loss during hydrolysis and distillation and its sensitivity is low, whereas the latter method is time-consuming. In comparison to these European methods and in compliance with norm V03-110, we have developed an automated gas chromatography headspace method. This method offers a good level of accuracy and precision and is specific to the compound determined (CS(2)). The limit of detection is below 0.020 mg/kg and the limit of quantification is below 0.050 mg/kg. Moreover, the recovery rates are between 85 and 103% with RSD less than 20%. The automated headspace method has several advantages when compared to the spectrophotometric and manual headspace methods, including the reduction of reagents employed for extraction and a greater number of analyses achievable per day than the other methods (approximately 40 samples of food).