Quantitative Determination of Individual Chlorinated Biphenyls in Milkfat by Splitless Glass Capillary Gas Chromatography

1980 ◽  
Vol 63 (5) ◽  
pp. 952-958
Author(s):  
Louis G M T Tuinstra ◽  
Wim A Traag ◽  
Henk J Keukens
Keyword(s):  
Gas Chromatography ◽  
Polychlorinated Biphenyls ◽  
Stationary Phase ◽  
Quantitative Determination ◽  
Capillary Gas Chromatography ◽  
Capillary Column ◽  
Glass Capillary ◽  
Basic Alumina ◽  
Better Than

Abstract A method is described for determining individual polychlorinated biphenyls (PCBs) in milkfat at the ppb level. Extraction and major cleanup are done simultaneously by saponification of the milkfat. After final cleanup on basic alumina, the concentrated extract is injected under splitless conditions on a capillary column coated with CPSil 7 stationary phase. The recovery of several individual PCBs from milkfat at a level of 25 ppb is better than 80%. The reproducibility for duplicates analyzed on several days showed standard deviations from 0.2 to 0.9 ppb for 19 individual chlorinated biphenyls. Some preliminary results for 165 samples of milkfat are reported.

scholarly journals Determination of Residues of Eight Synthetic Pyrethroids in Tobacco by Capillary Gas Chromatography

1994 ◽  
Vol 16 (2) ◽  
pp. 65-75
Author(s):  
BS Dattilo ◽  
S Gallo ◽  
G Lionetti
Keyword(s):  
Gas Chromatography ◽  
Film Thickness ◽  
Stationary Phase ◽  
Capillary Gas Chromatography ◽  
Capillary Column ◽  
Limit Of Detection ◽  
Synthetic Pyrethroids ◽  
Gas Chromatograph ◽  
Limit Of Determination

AbstractA method was developed for the simultaneous determination of the residues of the following eight synthetic pyrethroids and their isomers in tobacco: tetramethrin, permethrin, cyfluthrin, cypermethrin, alfamethrin, flucythrinate, fluvalinate and deltamethrin. The pesticides were extracted from ground tobacco by means of acetone:water 9:1 for 5 hours. The extract was diluted with water and partitioned into n-hexane. The organic phase was concentrated to about 1 ml and then purified by a Florisil-SPE column. The gas-chromatographic analyses were run with a gas-chromatograph Carlo Erba Series Mega HRGC 5300 equipped with a capillary column (stationary phase OV-1 - 0.10-0.15 µm film thickness, 25 m long) and a 63Ni electron-capture detector. Two different injection ports were used: split-splitless and cold split-splitless, working both with isothermal and programmed temperatures. Both the limit of detection and the limit of determination were estimated for each compound. Recoveries from fortified samples at level of 1 µgKg-1 are reported.

Determination of volatile alcohols and acetone in serum by non-polar capillary gas chromatography after direct sample injection.

1984 ◽  
Vol 30 (10) ◽  
pp. 1672-1674 ◽  
Author(s):  
N B Smith
Keyword(s):  
Gas Chromatography ◽  
Capillary Gas Chromatography ◽  
Capillary Column ◽  
Internal Standard ◽  
Fused Silica ◽  
Gas Chromatograph ◽  
Ionization Detector ◽  
Flame Ionization ◽  
Split Ratio

Abstract In this method for detection and quantification of volatile alcohols by capillary gas chromatography, the serum sample is deproteinized, then directly injected into the gas chromatograph with 1-propanol as the internal standard. The capillary column is a 30-m bonded methylsilicone-coated, fused-silica column. With helium as the carrier gas, the injector inlet is set at a split ratio of 1/30 and the average linear velocity in the column is 25 cm/s. Injector and flame-ionization detector temperatures are 280 degrees C, oven temperature 35 degrees C. Chromatography time is less than 3 min.

Quantitative Determination of Specified Chlorobiphenyls in Fish with Capillary Gas Chromatography and its use for Monitoring and Tolerance Purposes

1983 ◽  
Vol 14 (2) ◽  
pp. 147-157 ◽  
Author(s):  
Louis G. M. Th. Tuinstra ◽  
Jaap J. M. Driessen ◽  
Henk J. Keukens ◽  
Ton J. Van Munsteren ◽  
Arle H. Roos ◽  
...  
Keyword(s):  
Gas Chromatography ◽  
Quantitative Determination ◽  
Capillary Gas Chromatography

Surrogate-Assisted Determination of 2,3,7,8-Tetrachlorodibenzo-p-Dioxin in Fish by Electron Capture Capillary Gas Chromatography

1986 ◽  
Vol 69 (6) ◽  
pp. 976-980
Author(s):  
Richard A Niemann
Keyword(s):  
Gas Chromatography ◽  
Electron Capture ◽  
Capillary Gas Chromatography ◽  
Capillary Column ◽  
Electron Capture Detection ◽  
Matrix Interference ◽  
Relative Standard ◽  
Tetrachlorodibenzo P Dioxin ◽  
Liquid Chromatographic

Abstract Surrogate spiking the sample with 1000 parts per trillion (pptr) 1,3,7,8-tetrachlorodibenzo-p-dioxin (1378-TCDD) has doubled analytical throughput in determining toxic 2378-TCDD (analyte) at the low partper- trillion level in fish, using multicolumn high resolution liquid chromatographic cleanup before quantitation by capillary gas chromatography with electron capture detection. The 1378- and 2378-TCDD were recovered equally and were well separated by the capillary column so that the earlier-eluting surrogate did not interfere with the quantitation of levels of analyte many-fold lower. Matrix interference contributed <1 % bias in surrogate quantitation. Using surrogate recovery to correct for analyte losses during analysis, accuracy averaged (n = 7) 105% in determining 18 or 45 pptr 2378-TCDD added to fish without detectable bioincurred analyte. Analyses of selected fish with bioincurred 2378-TCDD gave results comparable to earlier work where recovery correction required a second analysis of sample fortified with analyte. With surrogate fortification, repeatability of determination (n = 3 or 4) improved markedly to <5% relative standard deviation at 37-46 pptr.

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