Improved Multiresidue Gas Chromatographic Determination of Organophosphorus, Organonitrogen, and Organohalogen Pesticides in Produce, Using Flame Photometric and Electrolytic Conductivity Detectors

1981 ◽  
Vol 64 (5) ◽  
pp. 1187-1195 ◽  
Author(s):  
Milton A Luke ◽  
Jerry E Froberg ◽  
Gregory M Doose ◽  
Herbert T Masumoto

Abstract The multiresidue procedure of Luke et al., which uses extraction with acetone and partition with petroleum ether and methylene chloride, was simplified and shortened by eliminating the Florisil cleanup. Double concentration with petroleum ether in the Kuderna-Danish evaporator following the initial concentration removed the last traces of methylene chloride. The extract was then injected into a gas chromatograph, using a Hall electrolytic conductivity detector for organohalogen, organonitrogen, and organosulfur pesticides or a flame photometric detector for organophosphorus pesticides. Recoveries of 79 pesticides are presented.

1967 ◽  
Vol 50 (6) ◽  
pp. 1236-1242
Author(s):  
Robert K Stevens

Abstract Organophosphate pesticides in cold pressed citrus oils can be determined rapidly by a method using gas chromatographic procedures and the flame photometric detector developed by Brody and Chaney. This study revealed that cold pressed citrus oils obtained from the 1965— 1966 citrus crops from Florida and California contained from 1.5 to 20 ppm thiophosphate pesticides. The analytical procedure required approximately 40 min per analysis and eliminated the need for extensive preparation of the sample prior to introduction into the gas chromatograph. The procedure is more specific and less time consuming than methods previously described


1984 ◽  
Vol 67 (2) ◽  
pp. 280-284
Author(s):  
Promode C Bardalaye ◽  
Willis B Wheeler

Abstract Residue analysis of the herbicide ametryn (2-methyIthio-4-ethylamino-s-isopropylamino-s-triazine) is widely known but an analytical method for determining its metabolites has not yet been reported in the literature. A method has been developed for the extraction and determination of ametryn and 3 metabolites, 2-methylthio-4-amino-6-isopropylammo- s-triazine (GS-11354), 2-methylthio-4,6-diamino-.s-triazine(GS- 26831), and 2-methylthio-4-amino-6-ethylamino-s-triazine (GS-11355) in taniers, yams, cassava. Residues were extracted from crops with ethyl acetate-toluene (3 + 1 v/v), using a Polytron homogenizer and anhydrous sodium sulfate added for drying. The extracts were cleaned up by automated gel permeation chromatography on Bio-Beads SX-3 gel in the same solvent system. Quantitative determination was performed by gas chromatographic (GC) analysis on a column packed with 5% DEGS-PS on 100-120 mesh Supelcoport using either an N-P detector or a flame photometric detector (FPD) in the sulfur mode. Minimum detection by the flame photometric detector is 10 ng each for ametryn, GS-11354, and GS-11355 and 21 ng for GS-26831; by the N-P detector, 0.3 ng of each component gives easily quantitatable peaks. On a parts per million basis, starting with 25 g sample, the FPD detected a minimum level of 0.04 p.g/g each for ametryn, GS-11354, and GS-11355, and 0.08 p.g/g for GS-26831. The N-P detector could detect 0.0024 p.g/g for all 4 compounds. In addition to superior sensitivity, instrumental conditions allowed the complete separation of components in 10 min, for the N-P detector; more than 30 min was required for the FPD. Recoveries from fortified crops ranged from 67 to 111% at levels of 0.1-1.0 μg/g.


1968 ◽  
Vol 51 (4) ◽  
pp. 825-828
Author(s):  
Laura A Roberts

Abstract A method for the gas chromatographic determination of methylene chloride, ethylene dichloride, and trichloroethylene residues in spice oleoresins was studied collaboratively. The method employs a microcoulometric gas chromatograph fitted with a Porapak Q column and is based on the volatility of the solvent residues, their relative retention times on a polyaromatic bead chromatographic column, and their detectability by a halide-specific microcoulometric method. Recoveries were adequate when the method was closely followed; recoveries were erratic when collaborators deviated from the method. Further study is recommended.


1986 ◽  
pp. 100-104
Author(s):  
Toshiro MATSUMURA ◽  
Katsuaki KAMETANI ◽  
Hitoshi TODORIKI ◽  
Tadanori TAKEMURA ◽  
Mariko TODOME ◽  
...  

1984 ◽  
Vol 67 (4) ◽  
pp. 840-843
Author(s):  
William R Betker ◽  
◽  
D Anderson ◽  
J M Bajovich ◽  
O O Bennett ◽  
...  

Abstract A collaborative study was conducted on a gas chromatographic method for determining metribuzin. Two 75% dry flow able and two 42% liquid flowable formulations were analyzed by 18 laboratories. Formulations were extracted by shaking or ultrasonic mixing for 1-5 min with methylene chloride which contained di-n-butyl phthalate as an internal standard. The extracts were injected into a gas chromatograph equipped with an OV-225 column. Peak area ratios and peak height ratios showed no significant difference. The reproducibility coefficient of variation was 0.75% for the 75% formulation and 1.41% for the 42% formulation. This GC method has been adopted official first action.


1973 ◽  
Vol 56 (2) ◽  
pp. 333-337 ◽  
Author(s):  
Linwood D Haines ◽  
Irving L Adler

Abstract Residues of ethylene thiourea on food crops are determined by extracting the sample with methanol, partially purifying the extract on an alumina column, and derivatizing the ethylene thiourea extracted with 1-bromobutane in the presence of dimethylformamide and sodium borohydride. The resulting derivative is measured by gas chromatography, using a flame photometric detector. The method is suitable for routine use and is sensitive to 0.01 ppm.


1986 ◽  
Vol 69 (3) ◽  
pp. 488-490
Author(s):  
William R Betker ◽  
◽  
E W Balcer ◽  
O O Bennett ◽  
W R Coffman ◽  
...  

Abstract A collaborative study was conducted on a gas chromatographic method for determination of fensulfothion. Eleven laboratories analyzed 2 technical and two 6 lb/U.S. gal. spray concentrate samples. In the analysis, samples are dissolved in methylene chloride which contains 4-chlorophenyl sulfoxide as an internal standard, and solutions are injected into a gas chromatograph equipped with an OV-330 column. Withinlaboratory repeatability was 0.79% for technical product and 0.37% for the spray concentrate samples, with coefficients of variation of 0.88 and 0.58%, respectively. Among-laboratories reproducibility was 0.81% for technical product and 0.53% for the spray concentrate, with coefficients of variation of 0.91 and 0.84%, respectively. The method has been adopted official first action.


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