Trennung und bestimmung von carbamat- und harnstoffherbiziden durch reaktions-gaschromatographie

doi:10.1016/S0021-9673(00)93624-0

Journal of Chromatography A

Volume 49, 1970, Pages 205-214

https://doi.org/10.1016/S0021-9673(00)93624-0 Get rights and content

Zusammenfassung

Separation and determination of carbanate and urea herbicides by reaction gas chromatography

The behaviour of a number of carbamate and urea herbicides during thermal degradation in the interior of the gas chromatographic apparatus and during chromatography through a KOH-layered reaction separation column is studied. Methods are developed for the direct gas chromatographic analysis of the herbicidal active substances proximpham, propham, chlorpropham, fenuron, monuron, diuron, monolinuron, linuron, and metobromuron. Results show that the rapid separation and quantitative determination of these herbicides is possible.

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Cited by (35)

Determination of linuron in water samples by high performance liquid chromatography after preconcentration with octadecyl silanized magnetite
2007, Microchemical Journal
A sensitive and selective batch adsorption method is proposed for the preconcentration and determination of linuron. Linuron was preconcentrated on octadecyl silanized (ODS) magnetite as an adsorbent and then determined by high performance liquid chromatography (HPLC). Several parameters on the recovery of the analyte were investigated. The experimental results showed that it was possible to obtain sufficient preconcentration efficiency when the solution pH was 6 using 100 mL of sample solution containing 1.0 μg of linuron and 3 mL of ethanol as a desorption solution. Recovery of linuron was 50.7 ± 1.9% with a relative standard deviation for five determinations of 3.0% under optimum conditions. The calibration curve of linuron was linear up to 200 ng mL^− 1 with a correlation coefficient of 0.998 and the detection limit (3S/N) was 1.0 ng mL^− 1. The capacity of the adsorbent was also examined and found to be 0.15 mg g^− 1 for linuron. ODS-magnetite is suitable for repeated use without decreasing recovery at least 4 adsorption–desorption cycles. The proposed method was successfully applied to the determination of linuron in river water with high precision and accuracy.
Solid-phase microextraction coupled with high-performance liquid chromatography for the determination of phenylurea herbicides in aqueous samples
2003, Journal of Chromatography A
Solid-phase microextraction coupled with high-performance liquid chromatography was successfully applied to the analysis of nine phenylurea herbicides (metoxuron, monuron, chlorotoluron, isoproturon, monolinuron, metobromuron, buturon, linuron, and chlorbromuron). Polydimethylsiloxane–divinylbenzene (PDMS–DVB, 60 μm) and Carbowax–templated resin (CW–TPR, 50 μm) fibers were selected from four commercial fibers for further study because of their better extraction efficiencies. The parameters of the desorption procedure were studied and optimized. The effects of the properties of analytes and fiber coatings, carryover, duration and temperature of absorption, pH, organic solvent and ionic strength of samples were also investigated. External calibration with an aqueous standard can be used for the analysis of environmental samples (lake water) using either PDMS–DVB or CW–TPR fibers. Good precisions (1.0∼5.9%) are achieved for this method, and the detection limits are at the level of 0.5–5.1 ng/ml.
New strategies for the determination of phenylurea pesticides by gas chromatography with hot splitless inlet systems
2001, Journal of Chromatography A
Direct gas chromatographic methods to analyse phenylurea pesticides are discouraged by the thermal instability of these compounds, that in conventional hot splitless inlet systems leads to extensive and irreproducible formation of isocyanates and amines. However a careful control of the operating conditions, like the inlet temperature, the pressure and the presence of suitable chemical additives (as acetic acid, low-molecular-mass amines, organic anhydrides) can either: (i) minimise the thermal decomposition enabling the direct GC–MS analysis of phenylureas, or (ii) lead to reproducible conversion to isocyanates. Experimental design was employed to study the effect of the experimental variables on the thermal transformation of phenylurea pesticides in splitless inlet system. Two strategies were alternatively optimised: (i) the minimisation of degradation reactions to increase the signal of phenylureas; (ii) the maximisation of the degradation to isocyanates that are in turn determined. The maximal yields in isocyanate were obtained with high inlet temperatures, low carrier flows in the injection phase and the presence of acetic anhydride. By contrast, the use of relatively low inlet temperatures, high carrier flows during the injection and the presence of an amine maximise the response of the parent compounds.
Comparison of gas and liquid chromatography for analysing polar pesticides in water samples
1996, Journal of Chromatography A
This review describes the applications of gas chromatography (GC) and liquid chromatography (LC) in the analysis of selected groups of pesticides in water. The attention is focussed on the most popular (in terms of amounts produced and applied) pesticide classes, i.e., carbamates, phenylureas, triazines, phenoxy acetic acid derivatives and chlorinated phenols. The use of GC and LC for the analysis of these compounds in water samples in the past and at present is reviewed separately for each group. Sample concentration and detection techniques are discussed in relation to their influence on the performance of the particular separation technique. Special attention is given to mass spectrometry (MS) because it is the most intensively developed detection technique in environmental analysis. The potential of another novel approach - large volume injections into the GC - is discussed separately. Methods using GC or LC coupled to an appropriate detector and using suitable sample handling procedures provide detection limits typically in the range of 0.001–1 ppb. At these levels, target or unknown compounds can be determined/identified by means of their retention and spectral characteristics. Principally, most of the analytes can be determined by both techniques, however, GC methods, when applicable, still have the advantages of great separation efficiency, high speed of analysis and the availability of a wide range of highly sensitive detectors; on the other hand, LC is often a method of choice when polar, non-volatile or thermolabile compounds are to be analyzed. Neither of the two separation techniques reviewed seems to have an overall priority in environmental analysis of pesticides. They can be considered as complementary.
Determination of phenylurea pesticides in water by derivatization with heptafluorobutyric anhydride and gas chromatography-mass spectrometry
1993, Journal of Chromatography A
The application of direct gas chromatographic methods to phenylurea pesticides is difficult because these compounds are thermally unstable and rapidly give isocyanates and amines when using standard gas chromatography. However, derivatization to more thermally stable compounds can be used. Procedures for solid-liquid extraction, catalytic heptafluorobutyrylation, clean-up and determination by GC-MS of phenylurea pesticides in water samples are reported. Detection limits are of the order of 10–50 ng/l.
Determination of phenylurea herbicides via direct derivatisation with heptafluorobutyric anhydride
1984, Journal of Chromatography A
Direct derivatisation of fifteen phenylurea herbicides with heptafluorobutyric anhydride (HFBA) has been studied. Quantitative conversion is obtained within 1 h at 60°C, using hexane as solvent. The nuclear magnetic resonance and mass spectrometric characteristics of the HFB-herbicides are reported, as well as their behaviour in adsorption high-performance liquid chromatography and capillary gas chromatography; detection limits are of the order of 50 pg and 1 pg, respectively, using electron-capture detection. Applications to water and crop samples are reported.

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Trennung und bestimmung von carbamat- und harnstoffherbiziden durch reaktions-gaschromatographie☆

Zusammenfassung

J. Chromatog.

J. Chromatog.

J. Chromatog.

J. Chromatog.

J. Chromatog.

Mitt. Gebiet Lebensm. Hyg.

European Potato J.

Anal. Chem.

Bunseki Kagaku

Anal. Chem.