An improved method for the determination of the systemic fungicide fosetyl-aluminum (aluminum tris(ethyl phosphonate)), in commercial formulations, via the quantitative determination of the phosphonate anion is described. The method employs HPIC using eluent suppression and conductivity detection. Two different kinds of chromatographic columns were utilized in the study, together with several eluents. The method has good sensitivity and reproducibility (CV% 3.2), and the sample preparation required is very simple. Under the analytical conditions adopted, the detection limit of fosetyl-aluminum in the commercial formulation "Aliette" was 0.008 g/kg. Chromatographic conditions for gradient elution were also investigated in the study, which were able to reveal the possible presence of phosphorous acid. The detection limit for this compound was 0.03 mg/liter. An atomic absorption spectroscopy name technique was also applied to the samples as an indirect analysis of fosetyl-aluminum via the determination of aluminum.
"The literature also contains two methods for the determination of fosetyl- Al in commercial pesticide formulation. The method proposed by Giordano et al. (1995) recommends the use of a high-performance ion chromatographic system with eluent suppression and conductivity. A survey in the literature indicated that ion chromatography has found only limited applications in the pesticide industry (Gangal et al., 2000). "
[Show abstract][Hide abstract] ABSTRACT: An isocratic reversed-phase high-performance liquid chromatographic (RP-HPLC) method with diode array detection (DAD) was developed for the determination of aluminium tris(ethyl phosphonate) (fosetyl-aluminium, fosetyl-Al) in plant-protection products. The method involves extraction of the active ingredient by sonication of the sample with water and direct measurement by RPHPLC. The isocratic RP-HPLC method for the analysis of fosetyl-Al thus developed was then validated for specificity, linearity, precision, and accuracy. The chromatographic peak confirmation was performed by LC-MS using electron spray ionisation in the negative-ion mode. The repeatability of the method, expressed as relative standard deviation (RSD, %), was found to be 0.5 % and the limit of detection was 0.035 mg mL−1. The average recoveries of the three fortification levels varied from 96.7 % to 100.6 % and the RSDs ranged between 2.6 % and 6.3 %. The precision of the method was also considered to be acceptable as the experimental repeatability relative standard deviation (RSDr) was lower than the RSDr, calculated using the Horwitz equation. The method is rapid, simple, accurate, cost-effective, and provides a new and reliable means for the analysis of fosetyl-Al in formulated products.
Chemical Papers- Slovak Academy of Sciences 06/2014; 68(6). DOI:10.2478/s11696-013-0522-6 · 1.47 Impact Factor
"A survey and testing of the published HPIC-related methods revealed that the majority of the protocols were not applicable for the analysis of large numbers of plant samples. Indeed, either the appropriate commercial columns were no longer available (El-Hamalawi et al., 1995), the reported methodology was restricted only to standards and could not readily be applied to plant material from the field (Mehra and Pelletier, 1990; Giordano et al., 1995; Alltech Associates, 1997), or the sample preparation was impractical because of its complexity (Saindrenan et al., I985). The single procedure that had none of the limitations outlined above was reported by Ryder (1986), who had developed an appropriate method that relied on a silicabased column. "
[Show abstract][Hide abstract] ABSTRACT: This contribution describes a simple, reliable, high throughput, and cost efficient method for the determination of phosphite and phosphate concentrations in plant samples from a range of plant families using high performance ion chromatography (HPIC). This protocol is a marked improvement over existing methodologies in terms of the practicalities of sample preparation and reliability of subsequent analysis.
Communications in Soil Science and Plant Analysis 10/1999; 30(17). DOI:10.1080/00103629909370376 · 0.39 Impact Factor
[Show abstract][Hide abstract] ABSTRACT: The potential of microcolumn liquid chromatography (μlC) and capillary electrophoresis (CE) with on-line, flame photometric
detection (FPD) in the P-selective mode has been studied for determination of polar P-containing pesticides, glyphosate and
its main metabolite, aminomethylphosphonic acid (AMPA), ethephon, fosetyl-aluminium and acephate. Acephate was determined
by reversed-phase μLLC-FPD using large-volume injections with peak compression, the other compounds were determined by μLC-FPD
and CE-FPD using simple, large-volume injection procedures to obtain limits of detection of 7.5-500 ng·mL−1 and 1.0 μ·mL−1, respectively. The methods showed acceptable repeatability and robustness and were successfully applied for rapid and selective
determination of pesticides in fruit, vegetable and water samples.
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