Extraction, Cleanup and Liquid Chromatographic‐Diode Array Determination of Carbamate Pesticides in Soil Samples

Author(s):  
Nathalie de Bertrand ◽  
Gaël Durand ◽  
Damià Barceló
2009 ◽  
Vol 92 (2) ◽  
pp. 680-688 ◽  
Author(s):  
Pei Chen ◽  
Renata Atkinson ◽  
Wayne R Wolf

Abstract The purpose of this study was to develop a single-laboratory validated (SLV) method using high-performance liquid chromatography with different detectors diode array detector (DAD); fluorescence detector (FLD); and mass spectrometry (MS) for determination of 7 B-complex vitamins (B1-thiamin, B2-riboflavin, B3-nicotinamide, B6-pyridoxine, B9-folic acid, pantothenic acid, and biotin) and vitamin C in multivitamin/multimineral dietary supplements. The method involves the use of a reversed-phase octadecylsilyl column (4 m, 250 2.0 mm id) and a gradient mobile phase profile. Gradient elution was performed at a flow rate of 0.25 mL/min. After a 5 min isocratic elution at 100 A (0.1 formic acid in water), a linear gradient to 50 A and 50 B (0.1 formic acid in acetonitrile) at 15 min was employed. Detection was performed with a DAD as well as either an FLD or a triple-quadrupole MS detector in the multiple reaction monitoring mode. SLV was performed using Standard Reference Material (SRM) 3280 Multivitamin/Multimineral Tablets, being developed by the National Institute of Standards and Technology, with support by the Office of Dietary Supplements of the National Institutes of Health. Phosphate buffer (10 mM, pH 2.0) extracts of the NIST SRM 3280 were analyzed by the liquid chromatographic (LC)-DAD-FLD/MS method. Following extraction, the method does not require any sample cleanup/preconcentration steps except centrifugation and filtration.


1999 ◽  
Vol 82 (5) ◽  
pp. 1214-1216 ◽  
Author(s):  
G Anthony Ohmes ◽  
Thomas C Mueller

Abstract A rapid method for the determination of sulfentrazone in soils is described. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components through a C18 column, and ultraviolet detection at 220 nm. Recoveries from fortified surface soils were >85% for sulfentrazone. Average relative standard deviations over the soils examined was 7.7%. A conservative lower limit of quantitation for sulfentrazone was 40 ng/g soil.


1994 ◽  
Vol 77 (3) ◽  
pp. 752-755 ◽  
Author(s):  
William T Willian ◽  
Thomas C Mueller

Abstract A rapid, sensitive method for the determination of norflurazon in 4 soils is described. Data on the initial soil metabolite is also obtained in soils with low organic matter. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanol-soluble components by using a C18 column, and fluorescence detection with excitation at 294 nm and emission measured at 398 nm. Recoveries from fortified soils were >90% for norflurazon and >80% for desmethylnorflurazon from the Shipps, Lexington, and Harkey soils. Average percent relative standard deviations over the soils examined was 5.5% for norflurazon and 8.7% for desmethylnorflurazon. The limit of detection for norflurazon was 10 ng/g soil, whereas the limit of detection for desmethylnorflurazon was 100 ng/g soil because of its smaller relative detector response.


1990 ◽  
Vol 73 (2) ◽  
pp. 298-299
Author(s):  
Thomas C Mueller ◽  
Philip A Banks ◽  
Parshall B Bush ◽  
William C Steen

Abstract A rapid, sensitive method is described for the determination of5-(methylamlno)-2-phenyl-4-[3-(trlfluoromethyl)phenyl]-3- (2M)-furanone (RE-40885) concentrations in 3 soil types. The method consists of extraction of soil samples with methanol, filtration, liquid chromatographic separation of methanolsoluble components using a C18 column, and UV detection at 275 nm. Recoveries were 94, 96, and 94% from the Greenville, Cecil, and Dothan soils, respectively. Average relative standard deviation was 8.0% in the Greenville soil. The qualitative limit of detection was 20 ppb and the limit of quantitation was 40 ppb in 25 g soil samples.


1976 ◽  
Vol 59 (2) ◽  
pp. 264-268
Author(s):  
Andrew J Pik ◽  
Gordon W Hodgson

Abstract A gas-liquid chromatographic (GLC) method has been developed for the determination of the experimental herbicide 3,6-dichloropicolinic acid (Dowco 290) in soils. The method involves extraction of 1 g soil samples with 1N NaCl at approximately pH 7, methylation with diazomethane utilizing a microgenerator, and detection by electron capture GLC. Interferences are small, so that a cleanup step is not necessary even at the 6 ppb level. The procedure is rapid, requiring only 45 min/sample. Recoveries range from 84 to 94% at the 6–1000 ppb level with a minimum detectable limit of 6 ppb. Standard deviations for the percentage recovery values vary from 10.9 to 2.3 for the tested range of 6.7–670 ppb, respectively.


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