Summary Norflurazon and Oxadixyl residues have been analysed by HRGC-ECD after extraction from field-treated sugar cane and grapes using classical solid-liquid extraction or supercritical fluid extraction. The extraction techniques were compared; the results indicate the advantages of SFE as an alternative method for analysis of pesticides in these samples. 相似文献
This paper presents the development of a single flow-through phosphorescence optosensor for simultaneous determination of pesticide N-1-naphthylphthlamic acid (NAP) and its metabolite 1-naphthylamine (NNA). The system works as a simple and rapid phosphorimetry-biparameter sensor. It is based in the on-line immobilization of the analytes onto a non-ionic resin solid support (Amberlite XAD 7) in a continuous flow system, followed by the measurement of their native phosphorescence. The determination was performed using 0.2 M TlNO3 and 15 mM Na2SO3 in a carrier flow. The developed sensor was satisfactorily applied to the determination of these pesticides in drinking and mineral waters (recovery percentages between 82.8 and 114.1% with inferior relative standard deviations to 3.1%). 相似文献
An analytical method is described for assessing the vapour concentration of 11 pesticides (bioallethrin, chlorpyriphos methyl, folpet, malathion, procymidone, quintozene, chlorothalonil, fonofos, penconazole and trimethacarb) in confined atmospheres (e.g. a greenhouse after pesticide application). This study is a successful extension of a method previously developed by the authors for dichlorvos to much less volatile pesticides. Sampling was performed by using polydimethylsiloxane–solid phase micro-extraction (PDMS–SPME) fibres immersed in a 250-mL sampling flask through which air samples were dynamically pumped from the analysed atmosphere. After a 40-min sampling duration, samples were analysed by GC/MS.Calibration was performed from a vapour-saturated air sample. The linearity of the observed signal versus pesticide concentration in the vapour phase was proved from spiked liquid samples whose headspace concentrations were measured by using the proposed method. This procedure gave calibration curves with regression coefficients (R2) greater than 0.98, and the repeatability of these measurements was found with RSDs of 1.9–7.6%. As a field application test, this analysis procedure was used for the determination of gaseous procymidone concentrations as a function of time in the atmosphere of an experimental 8-m2 and 20-m3 greenhouse. The pesticide was sprayed according to real cultivation conditions, and measurements were made for 80 h after application (8 measurements). The observed concentrations found ranged from 200 to 500 µg m–3, thus indicating the level of contamination of the air breathed by people in such working conditions.Abbreviations GC/MS
gas chromatography/mass spectrometry
- SIM
selective ion monitoring
- FC43
perfluorotributylamine
- RSD
relative standard deviation
- LOD
limit of detection
- LOQ
limit of quantification 相似文献
Summary The applicability of solid-phase extraction-LC using two short columns (SPE-LC) and/or single-short-column liquid chromatography
(SSC) combined on-line with tandem mass spectrometry (MS) was demonstrated for the rapid study of pesticide degradation. A
fast analytical procedure was developed to provide preliminary information concerning experimental conditions, approximate
rates of degradation and identity of the degradation products. Surface water samples were spiked at relevant concentration
levels with well-known microcontaminants and photolysis was used to transform parent compounds into their degradation products.
In general, the strategy was as follows: at 30-min intervals 10-mL samples were on-line enriched, separated by short-column
LC and recorded in full-scan MS to obtain information on the disappearance of the parent compound and the appearance of breakdown
products. To obtain structural information, product-ion spectra of selected compounds appearing in the full-scan MS chromatogram
were recorded; this enabled the identification of several degradation products. Total analysis time of enrichment/separation
and detection was about 10–15 min. 相似文献
In recent years the declaration of estimated uncertainty of measurement has become an integral part of analytical results. This study presents the assessment of results generated within the analysis of selected pesticides represented by carbamates, pyrethroides and azoles, residues of which may be found in treated apples. Multiresidue method used for analysis of spiked samples (residues at levels 0.040–0.163 mg/kg) consisted of (i) ethyl acetate extraction, (ii) GPC clean-up and (iii) identification/quantification of residues by GC. Procedures utilizing either conventional (electron-capture, nitrogen–phosphorus) or mass-selective detectors (quadrupole and ion trap analyzer) were evaluated. The results generated through alternative strategies of uncertainty estimation (“bottom-up”, “top-down”) were compared.
Using the “bottom-up” approach uncertainty of extraction which comprises two components—(i) repeatability of extraction and (ii) uncertainty of extraction recovery was shown to represent the main source of combined standard uncertainty (values of uncertainty of extraction for tested pesticides ranged from 4.6% to 21.6%). On the other hand, uncertainties associated with the GC calibration (uncertainties of weighing and diluting standards, uncertainties of purity of standards) were not so important (most of them did not exceed 2%). Combined standard uncertainties associated with the described analytical method ranged for individual compounds from 9.3% to 24.3%. Similar values of combined standard uncertainties were obtained using the alternative “top-down” approach. 相似文献
A rapid, reliable method has been developed for the multi-residue analysis of aniline metabolites of chlorpropham in potato samples. The method involves the precolumn derivatization of aniline metabolites with 5-(4,6-dichloro-s-triazin-2-ylamino) fluorescein (DTAF) and their subsequent separation and determination by micellar electrokinetic capillary chromatography with laser-induced fluorescence detection (MEKC-LIF). The optimum procedure includes a derivatization step of the aniline metabolites (3-chloroaniline, 3-chloro-4-hydroxyaniline and 3-chloro-4-methoxyaniline) at 40 degrees C for 40 min and a 5-fold dilution prior to MEKC analysis, which is conducted within about 7 min using negative-charged mixed micelles (SDS/Triton X-100) in the running buffer. Under these conditions, the DTAF-anilines were readily detected at 0.3-3.1 microg/L level with a precision of 4.8-6.4%. These results indicate that negative-charged mixed surfactant MEKC-LIF is useful as a selective, rapid, and sensitive tool for the determination of these anilines and surpasses other electrophoretic alternatives based on the use of fluorescein-isothiocyanate (FITC) as label reagent. Finally, the potato matrix showed no significant effects on the derivatization and determination of these analytes, since the analytical figures of merit for the real samples were similar to those obtained in aqueous solutions, and the average recovery at fortification levels of 10-250 microg/kg was over 97%. 相似文献
SEC is used for clean-up of food extracts obtained for analysis of pesticide residues primarily to remove high molecular weight material, among which fat may be present at the largest concentrations. The triglyceride peak, which is usually very large, is eluted before the components of interest. The problem described in this paper deals with the tail of the triglyceride peak: this may intrude into the fraction containing the pesticides and contaminate the GC. 相似文献
Summary A rapid method for the simultaneous determination of pentachlorophenol (PCP) and Carbaryl in water is described. A 1 liter water sample is extracted with hexane after acidification with concentrated H2SO4. After evaporation to a small volume, the extract is analyzed by gas chromatography-mass spectrometry, operating in the selected ion monitoring mode. Estimated detection limits are 0.08 g L–1 for PCP and 0.11 g L–1 for Carbaryl, with recoveries of 96% for PCP and 97% for Carbaryl. 相似文献