Trace analysis of 3,3'-dichlorobenzidine in animal chow, wastewater and human urine by three gas chromatographic procedures.
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Biomedical subjects
Publications and source records attributed to M C Bowman.
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An analytical method is described for determining residues of the synthetic estrogen diethylstilbestrol (DES) in animal chow at levels as low as 1 ppb. A methanol extract of the chow is subjected to a 3-step cleanup procedure including a Sephadex LH-20 column, liquid-liquid partitioning at pH 14 and 10.2, and a silica gel column. Residues of DES in the cleaned-up extract are analyzed directly by high-speed liquid chromatography or derivatized to pentafluoropropionyl-DES and assayed by electron-capture gas chromatography. Tests with 14C-DES were used to develop and validate the procedure. Ancillary data concerning extraction efficiencies of various solvents, comparisons of various derivatizing reagents, rates of trans-cis isomerization in two solvents, P-values of DES in various solvent-systems and thin-layer chromatographic behavior i
An analytical method is described for determining residues of the estrogens zearalenone and/or zearalanol in animal chow at levels as low as 10 ppb. The chow is extracted with methanol and cleaned up by a 3-step procedure employing a Sephadex LH-20 column, liquid-liquid partitioning at pH 13 and 8.3, and a silica gel column. Residues of the 2 compounds, separated on silica gel, are assayed by using high pressure liquid chromatography with ultraviolet detection. Additional data are also included concerning p-values of the compounds in several solvent systems, Rf values from thin layer chromatography with 9 solvent systems, solubilities in 3 solvents, and a procedure for preparing their pentafluoropropionyl derivatives for analysis by electron capture gas-liquid chromatography.
Chemical methods were developed for the trace analysis of the herbicide 2,4,5-trichlorophenoxyacetic acid, its glycineamide, and their alkaline hydrolyzable conjugates in mouse blood, urine, and feces. The salient elements of the methods are extraction of the free acids with benzene, methylation, cleanup on a silica gel column, and quantification via electron-capture GLC. Any unextracted conjugates remaining in the substrates are then subjected to alklaline hydrolysis, and the liberated 2,4,5-trichlorophenoxyacetic acid is assayed. Data are presented concerning recoveries of the compounds from the three spiked substrates. The utility of the procedures is illustrated by a preliminary pharmacolinetic study employing parallel electron-capture GLC and radioassays of the three substrates from mice injected with a single intravenous dose of 14C-2,4,5-trichlorophenoxyacetic acid. GLC characteristics and partition values of the the compounds and hydrolysis of the glycineamide under various conditions also are discussed.
Spectrophotofluorimetric (SPF) methods are described for the trace analysis of benzidine, 3,3'-dimethylbenzidine, 3,3'-dimethoxybenzidine, and their dihydrochloride salts in microbiological growth media, waste water, potable water, human urine, and rat blood. The salient elements of the methods for these known or suspected carcinogens are: extraction of the residues as the free amine with benzene, rapid cleanup on an alumina column, and quantification of the free amine in methanol via SPF. Potable water solutions of the salts are diluted with buffer (pH-4) and quantified directly by SPF. Ancillary analytical information concerning the solubility and stability of these compounds in water, p-values, gas chromatographic analysis of the free amines, and thin layer chromatographic data in ten solvent systems are also presented.
Methods for monitoring trace levels of 4-aminobiphenyl, 2-naphthylamine, and their hydrochloride salts in waste water, microbiological growth media, potable water, human urine, and mouse blood utilizing spectrophotofluorometry (SPF) are described. The salient elements of the methods are extraction of the residues as the free amine with benzene, rapid cleanup on an alumina column, and quantification of the free amine in methanol via SPF. Potable water solutions of the salts are diluted with 0.01 N aqueous HCL and quantified directly by SPF. Ancillary analytical information concerning gas chromatography of the free amines, partitioning properties of the compounds between solvent pairs, their solubility and stability in water, and thin-layer chromatographic data is presented. The compositions of various admixtures of 1- and 2-naphthylamine or their salts were determined by using SPF with calculations based on simultaneous equations.
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An adsorption system is described for the removal of part per billion levels of the chemical carcinogen, 2-acetylaminofluorene (2-AAF), from industrial wastewater. The system consists primarily of filters and activated carbon and non-ionic polymeric adsorbents arranged in tandem. It is highly efficient, operates at low cost, and requires minimal attention. The chemical monitoring of the raw and/or cleaned-up wastewater is based on a highly sensitive and specific spectrophotofluorometric method that allows acceptance or rejection of samples at the 0.2 part per billion level. The system is presented as a model for evaluating the removal of traces of organic chemicals from wastewater prior to recycling or discharging it into the environment. Results of laboratory evaluations of several other approaches to the purification of 2-AAF-containing wastewater are also presented.
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Background information concerning the concept of insect chemosterilization and analytical methods for determining trace levels of 19 P- and/or S- containing chemicals of current interest are presented. GC retention times of the compounds on 6 different columns and their p-values in 11 solvent systems are tabulated. The utility of the flame photometric detector for determining subnanogram levels of the sterilants in biological substrates is illustrated.
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