Determination of acrylamide in rat serum and sciatic nerve by gas chromatography-electron-capture detection.

A modified method for the derivatization and determination of acrylamide as 2-bromopropenamide by gas chromatography-electron-capture detection was developed and applied to serum and sciatic nerve from rats. The method was accurate and precise over the calibration range 2.24-7.47 micrograms/ml in serum diluted 1:125 and 4-122 micrograms/g in sciatic nerve homogenate (5 mg/ml). limits of detection were estimated to be 1200 ng/ml in undiluted serum and 3 micrograms/g in intact sciatic nerve. The use of less dilute samples to allow for lower limits of detection appears feasible. The time-course of acrylamide in serum and sciatic nerve was studied after acute dosing and indicated elimination half-lives of 1.8 and 2.0 h for serum and sciatic nerve, respectively. A dose-effect relationship was established for each matrix after acute dosing and the measured acrylamide concentrations in serum (microgram/ml) were approximately the same as in sciatic nerve (microgram/g).

Paired-ion liquid chromatographic method for the analysis of a phenanthrenemethanol antimalarial in whole blood.

A sensitive and specific high-performance liquid chromatographic (HPLC) assay was developed for the determination of the candidate antimalarial (+/-)-(1,3-dichloro-6-trifluoromethyl-9-phenanthryl)-3-di-(n-butyl )aminopropanol hydrochloride in whole blood. A reversed-phase, paired-ion (lauryl sulfate) system achieved separation of the antimalarial and internal standard from interfering constituents with a sensitivity limit of 10 ng/mL by UV detection (254 nm). Chromatographic variables (counterion concentration, pH, and column temperature) were examined to determine their effect on assay characteristics (retention, efficiency, and relative response) in clinical analysis. The antimalarial was isolated from 2.0 mL of whole blood using overnight extraction with 30% ethyl acetate in hexane followed by an acid/base partition sequence to remove major interferences. Overall recovery for the antimalarial was 84% with a CV of 5.0%, and the recovery of the internal standard was 81% (CV = 3.6%). The assay was validated by analysis of both intra- and interlaboratory samples. The assay was applied to the analysis of whole blood samples taken from a 30-year-old healthy human male who had received a single 14.1-mg/kg oral dose. The stability of the antimalarial in whole blood for up to 4 months and in sample extracts for up to 34 d at -17 degrees C was also demonstrated.

The human body burden of mirex in the southeastern United States.

Mirex is an organochlorine chemical with pesticidal and other industrial usages. Biologically, mirex was used as an insecticide for the control of imported fire ants in large areas of the southeastern United States. Evidence of mirex exposure in a national survey of chemicals in adipose tissue led to a more intensive survey of the general population in treated counties of the southeastern United States. Forty sites were selected randomly from 8 southeastern states where mirex was used widescale to combat fire ants; a total of 624 adipose tissue specimens were collected from these 40 sites. Tissue specimens were prepared by a modified Mills-Onley-Gather procedure and analyzed for mirex and selected other organochlorine compounds by electron-capture gas chromatography. Positive residue findings were confirmed by combined gas chromatography and mass spectrometry. Weighted statistical analysis of the data was conducted to estimate the level of mirex in the study area. It was estimated that 10.2% of the population of southern United States had quantifiable levels of mirex in adipose tissue. The estimated geometric mean of the quantifiable residue amounts was 0.286 ppm (lipid basis). Statistical tests of association and regression were used to investigate possible relationships between the presence and levels of mirex, and the Census Division or state of tissue-specimen collection, by age, race, and sex. These analyses indicated that region or location of tissue specimen collection (assumed to be area of residence) strongly related to both the presence of mirex residue and the amount of mirex residue detected. This may be correlated with the amount of mirex applied for fire ant control or with some other exposure patterns in different regions.