Determination of seventeen s-triazine herbicides and derivatives by high-pressure liquid chromatography

Abstract

Mixtures of simazine, atrazine, ametryne, prometryne, deethylsimazine, deethylatrazine, hydroxysimazine, hydoxyatrazine, hydoxyprometryne, N-ethyl-and N-isopropylammeline, N-ethyl-and N-isopropylammelide, melamine, ammeline, ammelide, and cyanuric acid in aqueous solution were separated and determined in a single analysis with a detection limit of 30-400 pmol. The s-triazines were detected by a UV detector after elution from a reversed-phase high-pressure liquid chromatography column using a phosphate buffer-methanol gradient at 2 "C.The s-triazine herbicides are widely used, accounting for 28% of herbicide manufacture in 1974 (Kiihle, 19761, and s-triazines have many other industrial uses [e.g., Cook and Hutter (1981a)l. However, no single method is available for the routine identification and quantification of these compounds, especially the more polar derivatives like ammeline, ammelide, and their N-alkylated derivatives. The available techniques all apply only to limited ranges of compounds. Paper chromatography and thin-layer chromatography require many solvent systems for the desired separations and offer poor and time-consuming quantification [reviews by Fishbein (1970Fishbein ( ,1975; see also Loos and Kearney (1978)l. Gas chromatography has been used extensively, but derivatization is essential for many compounds and there seems to be no universal derivatizing agent; furthermore, derivatization is seldom quantitative, and several columns are required to cover the whole range of compounds (Fishbein, 1970(Fishbein, ,1975Lusby and Kearney, 1978;Muir and Baker, 1978;Stoks and Schwartz, 1979;Muir, 1980). Low-pressure column chromatography, which has poor separative properties and is time consuming, has been used occasionally (Plaisted and Thornton, 1964). High-pressure liquid chromatography (HPLC) of s-triazines overcomes many difficulties arising from low volatility, low solubility, and chemical inertness. Thus, e.g., Smolkovi and Pacikovi (1978) We report here a simple method to identify and quantify chloro-and (methy1thio)-s-triazine herbicides, dealkylatrazines, hydroxyparents, N-alkylammelines, N-alkylammelides, melamine, ammeline, ammelide, and cyanuric acid in aqueous solutions by reversed-phase HPLC of underivatized samples. EXPERIMENTAL SECTIONApparatus. HPLC was done using jacketed stainless steel analytical columns (25 cm X 4.6 mm inner diameter) containing a reversed-phase packing of 5-pm mean particle diameter (LiChrosorb RP-18; Merck, Darmstadt, FRG). The mobile phase was delivered through a dynamic mixer (Altex, Berkeley, CA) by two pumps (Altex Model 110) which were controlled by a gradient programmer (Altex Model 420), and samples were applied to the column by using a high-pressure sample injector with pneumatic actuator (Model 7010/70-01; Rheodyne, Berkeley, CA) connected to an automatic sampler (AS1 45; Kontron, Ziirich, Switzerland). The sample loop of the injector was normally 20 wL. The eluate from the column passed through a UV detector (Uvikon LCD 725; Kontron) coupled to an inte...

s-Triazines as nitrogen sources for bacteria

“…NED (or NID) was not present in the substrate or in the stock cell suspension and was tentatively identified by cochromatography with authentic NED (or NID) by HPLC. The identification of the NED (or NID) was supported by UV spectra (Table V) and was confirmed by mass spectrometry (Table VI) problem has been governed by the fact that s-triazines are sparingly soluble in water (generally 0.5 mM or less; Beilstein et al, 1981) but that, e.g., 0.5 mM NID represents 2.0 mM nitrogen which allows the synthesis of about 100 pg of protein/mL ( Table IV; cf. Zeyer (1979), Wolf and Martin (1975), and Saldick (1974)], and they are thus unavailable to heterotrophic organisms.…”

“…Turbidity was measured in a Bausch & Lomb Spectronic 20 colorimeter with round cells of 12-mm path length. High-pressure liquid chromatography (HPLC) was done as described in the preceding paper (Beilstein et al, 1981). The identity of an organic compound, tentatively assigned by cochromatography with HPLC, was confirmed by obtaining mass spectra by direct insertion in a Hitachi Perkin-Elmer RMU 6M mass spectrometer using electron impact ionization at 70 eV.…”

“…s-Triazines were routinely measured and tentatively identified by HPLC as described in the preceding paper (Beilstein et al, 1981). Ammonium ion was routinely determined and tentatively identified by the method of Weatherburn (1967).…”

“…The ring carbon was released as carbon dioxide. A portion of these data was discussed in a review (Cook and Hutter, 1981).…”

Spectrofluorimetric Method for Quantification of Triazine Herbicides in Agricultural Matrices

“…2 A large number of methods have been reported in the literature for determination of triazine herbicides. These include LCelectrospray ionization mass spectrometry, 4,5 capillary electrophoresis, 6,7 gas chromatography (GC), [8][9][10] GC after liquid-liquid extraction, 11 GC with SPE, 12,13 separation by solid phase extraction-liquid chromatography-UV (SPE-LC-UV), 14,15 molecularly imprinted polymer, 16 dispersive liquid-liquid microextraction method based on solidification of floating organic droplet (DLLME-SFO), 17 HPLC 18 and immunoaffinity chromatography. 19 Most of the methods cited above involve time-consuming sample preparation, complex derivatization and need sophisticated instruments and trained personnel for operation.…”