Gas Chromatographic Determination of Benalaxyl Residues in Different Crops and Water

1993 ◽  
Vol 76 (3) ◽  
pp. 650-656 ◽  
Author(s):  
Teodoro Crisippi ◽  
Guido Zini ◽  
Riccardo Fabbrini
Keyword(s):  
Gas Chromatography ◽  
Column Chromatography ◽  
Active Ingredient ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Standard Deviations ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described that is suitable for the determination of benalaxyl residues ranging from 10 to 0.1 μg/kg in several crops, must, wine, and water. The compound is extracted with acetone and purified either by partitioning between water and n-hexane or by passing the extract through an Extrelut column with n-hexane. Further purification is achieved by column chromatography on alumina. The active ingredient is finally determined by gas chromatography with nitrogenphosphorus detection. Mean recoveries were ≥95% in the various crops tested and in the 0.01-1.05 mg/kg fortification range. Standard deviations for each crop were ≤6.5%.

Gas Chromatographic Determination of N-Butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-toluidine and α,α,α-Trifluoro-2,6-dinitro-N,N-dipropyl-p-toluidine in Formulations

1971 ◽  
Vol 54 (3) ◽  
pp. 711-712
Author(s):  
Martha Fuzesi
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Electron Capture ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Electron Capture Detector ◽  
Reference Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method is described for the quantitative determination of N-butyl-N-ethyl-α,α,α-trifluoro-2,6-dinitro-p-tolindine and α,α,α-trifluoro-2,6-dinitro-N,N-dipropyI-p-toluidine herbicides in formulations. The sample is extracted with benzene, and equal amounts of sample and reference solution in the same concentration range are analyzed by gas chromatography, using an electron capture detector and an SE-30/Diatoport S column. The method has been applied successfully to laboratory-prepared and commercial samples.

Capillary Column Gas Chromatographic Determination of Trace Residues of the Herbicide Chlorsulfuron in Agricultural Runoff Water

1987 ◽  
Vol 70 (4) ◽  
pp. 745-748
Author(s):  
Uaz Ahmad
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Capillary Column ◽  
Methylene Chloride ◽  
Chromatographic Determination ◽  
Agricultural Runoff ◽  
Runoff Water ◽  
Florisil Column ◽  
Gas Chromatographic Method

Abstract A capillary column gas chromatographic method is described for determining parts-per-trillion (ppt) levels of chlorsulfuron in agricultural runoff water. The water sample is acidified with acetic acid and extracted with methylene chloride. The chlorsulfuron in the extract is derivatized to its monomethyl derivative. After Florisil column cleanup, the methylated chlorsulfuron is determined by electron-capture gas chromatography. Recovery of chlorsulfuron from fortified water samples is greater than 80%. Detection limit of the method is 25 ng chlorsulfuron/L water (25 ppt). There are 2 reaction sites on the chlorsulfuron molecule, both of which are susceptible to methylation leading to monomethyl chlorsulfuron and dimethyl chlorsulfuron. A procedure is described to methylate selectively the sulfonamide nitrogen of chlorsulfuron.

Gas-Liquid Chromatographic Determination of Acephate and Ortho 9006 Residues in Crops

1974 ◽  
Vol 57 (1) ◽  
pp. 189-191
Author(s):  
James B Leary
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Chromatographic Determination ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Ether Solution ◽  
Liquid Chromatographic Determination ◽  
Gas Chromatographic Method ◽  
Liquid Chromatographic

Abstract A gas chromatographic method is described for determining acephate (O,S-dimethyl acetylphosphoramidothioate) and a metabolite, Ortho 9006 (O,S-dimethyl phosphoramidothioate), in a variety of crops. After extraction of the sample with ethyl acetate, the solvent is evaporated, and an ether solution of the residue is passed through a silica gel column to remove interferences. Acephate and Ortho 9006 are eluted from the column with 10% methanol in ether and measured simultaneously by programmed temperature gas chromatography, using an alkali flame ionization detector.

Gas Chromatographic Determination of Isofenphos in Technical and Formulated Products: Collaborative Study

1987 ◽  
Vol 70 (1) ◽  
pp. 55-57
Author(s):  
Daniel E Terry
Keyword(s):  
Thermal Conductivity ◽  
Gas Chromatography ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Flame Ionization ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of isofenphos (OFTANOL®) in isofenphos technical and liquid formulations has been developed and collaboratively studied by 11 laboratories. Two technical samples and 2 liquid flowable samples were analyzed after shaking/extracting in methanol which contained diisobutyl phthalate as an internal standard. The extracts were analyzed by gas chromatography using an SP-2100 column and either flame ionization or thermal conductivity detection. Coefficients of variation were 0.57 and 1.27% for the technical and formulated products, respectively. The GC method has been adopted official first action as a AOACCTPAC method.

Gas Chromatographic Determination of Synthetic Musk (7-Acetyl-6-Ethyl-1,1,4,4-Tetramethyltetralin) in Fragrances

1982 ◽  
Vol 65 (3) ◽  
pp. 598-601
Author(s):  
Harris H Wisneski ◽  
Ronald L Yates ◽  
Henry M Davis
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Soluble Fraction ◽  
Chromatographic Determination ◽  
Gas Chromatography Mass Spectrometry ◽  
Hplc Fraction ◽  
Synthetic Musk ◽  
Gas Chromatographic Method ◽  
Water Alcohol

Abstract A gas chromatographic method has been developed for the determination of the synthetic fragrance musk, 7-acetyl-6-ethyl-1,1,4,4-tetramethyltetralin (AETT). The fragrance is first added to water and extracted with ether to separate the fragrance oil from the water-alcohol mixture. The AETT, present in the ether-soluble fraction, is purified further by preparative high pressure liquid chromatography (HPLC). The AETT in the collected HPLC fraction is then determined by gas chromatography using external standardization. Recoveries from samples spiked with AETT at levels ranging from 100 to 1000 μg/mL varied from 80 to 96% with an average of 90%. AETT was verified in each sample by gas chromatography/mass spectrometry.

Gas Chromatographic Determination of Pentachlorophenol in Gelatin: Collaborative Study

1985 ◽  
Vol 68 (3) ◽  
pp. 419-421
Author(s):  
George Yip
Keyword(s):  
Gas Chromatography ◽  
Coefficient Of Variation ◽  
Chromatographic Method ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Coefficients Of Variation ◽  
Gas Chromatographic Method ◽  
Hydrolysis Of ◽  
Ppm Level

Abstract Eleven collaborators participated in this study of a gas chromatographic method for the determination of pentachlorophenol (PCP) in gelatin. Following acid hydrolysis of a 2 g sample, PCP is extracted with hexane and partitioned into KOH solution. After reacidification, PCP is again extracted with hexane for determination by electron capture gas chromatography on a 1 % SP-1240DA column. Three duplicate practice samples (0.0, 0.5, and 1.5 ppm) and 5 blind duplicate collaborative samples (0.0, 0.02, 0.1, 0.5, and 2.0 ppm) were analyzed by each collaborator. Mean recoveries of PCP in the collaborative samples ranged from 88% at the 0.02 ppm fortification level to 102% at the 0.1 ppm level; the overall mean recovery was 96%. Interlaboratory coefficients of variation ranged from 16.4% for the 0.1 ppm fortification level to 22.9% for the 0.5 ppm level; the overall interlaboratory coefficient of variation was 19.5%. The method has been adopted official first action.

Capillary Column Gas Chromatographic Determination of Trace Residues of the Herbicide Chlorsulfuron in Agricultural Runoff Water

1987 ◽  
Vol 70 (4) ◽  
pp. 745-748
Author(s):  
Uaz Ahmad
Keyword(s):  
Gas Chromatography ◽  
Chromatographic Method ◽  
Capillary Column ◽  
Methylene Chloride ◽  
Chromatographic Determination ◽  
Agricultural Runoff ◽  
Runoff Water ◽  
Florisil Column ◽  
Gas Chromatographic Method

Abstract A capillary column gas chromatographic method is described for determining parts-per-trillion (ppt) levels of chlorsulfuron in agricultural runoff water. The water sample is acidified with acetic acid and extracted with methylene chloride. The chlorsulfuron in the extract is derivatized to its monomethyl derivative. After Florisil column cleanup, the methylated chlorsulfuron is determined by electron-capture gas chromatography. Recovery of chlorsulfuron from fortified water samples is greater than 80%. Detection limit of the method is 25 ng chlorsulfuron/L water (25 ppt). There are 2 reaction sites on the chlorsulfuron molecule, both of which are susceptible to methylation leading to monomethyl chlorsulfuron and dimethyl chlorsulfuron. A procedure is described to methylate selectively the sulfonamide nitrogen of chlorsulfuron.

Gas Chromatographic Determination of Micro Amounts of Cyanide Residues in Wines, Distilled Liquors, and Other Alcoholic Beverages

1976 ◽  
Vol 59 (6) ◽  
pp. 1390-1395 ◽  
Author(s):  
Brian L Bates ◽  
Donald R Buick
Keyword(s):  
Cyanogen Bromide ◽  
Chromatographic Method ◽  
Limit Of Detection ◽  
Chromatographic Determination ◽  
Alcoholic Beverages ◽  
Relative Standard ◽  
Standard Deviations ◽  
Absorber Solution ◽  
Gas Chromatographic Method

Abstract A gas chromatographic method for the determination of cyanide residues in alcoholic beverages has been developed from procedures previously reported for application to water samples. Quantitatively isolating HCN from alcoholic beverages presented difficulties not encountered with aqueous solutions, particularly in the presence of SO2 in the sample. HCN was liberated from the acidified sample by heating at 70°C, flushed into an NaOH absorber solution, converted to cyanogen bromide (CNBr), extracted into diisopropyl ether, chromatographed on a Porapak Q column, and detected by an electron capture detector. SO2 that is present in most wines interfered with the bromination step and caused low recoveries. This interference was eliminated by initially converting any cyanide present in the sample to the stable mercuric cyanide salt and then purging the acidified sample solution of all SO2. The Hg(CN)2 present was then dissociated by adding KI and the analysis proceeded as previously described. Mean recoveries of 80–97 % were obtained for 2–20 μg cyanide from replicate analyses of spiked samples of distilled liquors free of SO2. The relative standard deviations ranged from 6.1 to 11.1%. Mean recoveries of 65 to 91% were obtained in the same range of cyanide from replicate analyses of spiked wine samples known to contain SO2, with relative standard deviations ranging from 0.8 to 10.2%. The limit of detection was 0.2 μg HCN.

Gas Chromatographic Determination of O,O-Diethyl S-(N-Isopropylcarbamoylmethyl) Phosphorothiolothionate (Prothoate) in Technical Products and Liquid Formulations

1972 ◽  
Vol 55 (6) ◽  
pp. 1336-1338
Author(s):  
Brunetto Bazzi ◽  
Guglielmo Galluzzi ◽  
Luigi Abruzzese
Keyword(s):  
Thermal Conductivity ◽  
Gas Chromatography ◽  
Chromatographic Method ◽  
Concentration Level ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Thermal Conductivity Detector ◽  
Gas Chromatographic Method ◽  
Technical Products

Abstract A gas chromatographic method has been developed for the analysis of O,O-diethyl S-(N-isopropylcarbamoylmethyl) phosphorothiolothionate . The acaricide or a convenient amount of an acaricidal preparation is dissolved in xylene, together with malathion as an internal standard, and analyzed by gas chromatography, using a thermal conductivity detector. The precision (P = 0.05) of the method is ±1.5% of the concentration level.

Gas Chromatographic Determination of Carbetamide Residues in Rape and Soil

1989 ◽  
Vol 72 (4) ◽  
pp. 660-662
Author(s):  
Jia-Lun Wu ◽  
De-Fang Fan
Keyword(s):  
Gas Chromatography ◽  
Petroleum Ether ◽  
Chromatographic Method ◽  
Direct Determination ◽  
Chromatographic Determination ◽  
Soil Samples ◽  
Nitrogen Phosphorus Detector ◽  
Gas Chromatographic Method ◽  
Nitrogen Phosphorus

Abstract A gas chromatographic method is described for direct determination of carbetamide residues in rape and soil. Rapeseed, leaves and stem of rape, and soil samples are extracted with acetone and the extracts are cleaned up by coagulation and partition with petroleum ether, followed by extraction with dichloromethane. Carbetamide is determined by gas chromatography using a nitrogen-phosphorus detector. Recovery ranges for rapeseed, leaves and stem of rape, and soil samples fortified with 0.1-10 ppm carbetamide were 91.4-103% [average 97.2 ± 12% (n = 9)], 94.4-102% [98.2 ± 4.4% (n = 12)], 87.9-93.9% [91.2 ± 6.5% (n = 9)1, and 86.7-102% [94.5 ± 4.5% (n = 15)], respectively.

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