araldite and hexahydrophthalic-acid

A method for the simultaneous determination of hexahydrophthalic acid (HHP acid) and methylhexahydrophthalic acid (MHHP acid) in human plasma was developed. The procedure was a rapid, single step extractive derivatisation with pentafluorobenzyl bromide as the derivatisation agent. The formed pentafluorobenzyl esters were analysed by gas chromatography-mass spectrometry in negative ion chemical ionisation mode with ammonia as the moderating gas. Deuterium-labeled HHP acid and MHHP acid were used as internal standards. The detection limit was 0.4 ng/ml for HHP acid (m/z 153) and 0.3 ng/ml for MHHP acid (m/z 365). The within-day precision of the method was between 2 and 3% and the between-day precision was between 3 and 12%. The overall recovery was between 65 and 83%. A comparison between HHP acid determinations with a previous and this method showed that the methods gave similar results. The method was applicable for analysis of plasma from occupationally exposed workers.

Topics: Cyclohexanecarboxylic Acids; Epoxy Resins; Fluorobenzenes; Gas Chromatography-Mass Spectrometry; Humans; Phthalic Acids; Phthalic Anhydrides; Quaternary Ammonium Compounds

A method for generating controlled atmospheres of hexahydrophthalic anhydride (HHPA) in an 8 m3 exposure chamber was developed. The permeation principle was used for gaseous HHPA generation. HHPA concentration was monitored by sampling on XAD-2 tubes and by a Fourier-transform infrared (FTIR) spectrometer using the partial least-square quantitative method. The repeatability of the FTIR was 5%, the reproducibility 12%, and the limit of detection 10 micrograms/m3. A bubbler method determined the sum of HHPA and HHP acid by using gas chromatography/mass spectrometry detection after derivatization with methanol/boron trifluoride. The precision of the work-up procedure was 3% and the recovery was 94% at 300 ng sampled amount of HHPA. The limit of detection was 10 ng HHPA. The variation in the permeation rate was 3% over 3 days. Different concentrations in the exposure chamber were generated by changing the temperature of the permeation tubes. The generated HHPA concentration range, at human exposure, was 3-90 micrograms/m3. The concentration at one temperature was reproducible even after major changes in the temperature. The coefficient of variation (CV) of six samples from different places in the breathing zone was 3%. The variation in the concentration, during an 8-hour human exposure at 10 micrograms/m3, was 3%. Time-weighted averages (8 hour) for human exposures of 10 micrograms/m3 (CV = 15%; n = 6); 37 micrograms/m3 (CV = 5%; n = 5); and 81 micrograms/m3 (CV = 6%; n = 9) were obtained at intended concentrations of 10 micrograms/m3, 40 micrograms/m3, and 80 micrograms/m3. The loss of HHPA in the exposure chamber was 54% (CV = 17%).(ABSTRACT TRUNCATED AT 250 WORDS)

Topics: Air Pollutants; Chromatography, Gas; Cyclohexanecarboxylic Acids; Environmental Exposure; Environmental Monitoring; Epoxy Resins; Fourier Analysis; Gas Chromatography-Mass Spectrometry; Humans; Least-Squares Analysis; Phthalic Anhydrides; Reproducibility of Results; Spectrophotometry, Infrared

Urinary hexahydrophthalic acid (HHP acid) levels were determined in 20 workers occupationally exposed to hexahydrophthalic anhydride (HHPA) air levels of 11-220 micrograms/m3. The levels of HHP acid in urine increased rapidly during exposure and the decreases were also rapid after the end of exposure. The elimination half-time of HHP acid was 5 h, which was significantly longer than in experimentally exposed volunteers, possibly indicating distribution to more than one compartment. There was a close correlation between time-weighted average levels of HHPA in air and creatinine-adjusted levels of HHP acid in urine collected during the last 4 h of exposure (r = 0.90), indicating that determination of urinary HHP acid levels is suitable as a method for biological monitoring of HHPA exposure. An air level of 100 micrograms/m3 corresponded to a postshift urinary HHP acid level of ca. 900 nmol/mmol creatinine in subjects performing light work for 8 h. Percutaneous absorption of HHPA was studied by application of HHPA in petrolatum to the back skin of three volunteers. The excreted amounts of HHP acid in urine, as a fraction of the totally applied amount of HHPA, were within intervals of 1.4%-4.5%, 0.2%-1.3%, and 0%-0.4% respectively, indicating that the contribution from percutaneous absorption is of minor importance in a method for biological monitoring.

Topics: Adult; Air Pollutants, Occupational; Cyclohexanecarboxylic Acids; Environmental Monitoring; Epoxy Resins; Female; Humans; Male; Middle Aged; Occupational Exposure; Phthalic Anhydrides; Skin Absorption

Six healthy volunteers were exposed to gaseous hexahydrophthalic anhydride (HHPA) concentrations of 10, 40, or 80 micrograms.m-3 (65, 260 or 520 nmol.m-3, respectively) for 8 h. The respiratory uptake of the inhaled HHPA was almost complete. Rapid increases in plasma and urinary levels of hexahydrophthalic acid (HHP acid) were seen. During the first 4 h after the end of exposure, the half-time of HHP acid in plasma was about 2 h. A corresponding decay was seen in urine. The correlations (r > 0.90) between the air concentrations of HHPA and the levels of HHP acid in plasma and urine were close. They were even closer (r > 0.96) when the total respiratory uptake of HHPA was used. Urinary pH adjustment by intake of ammonium chloride or sodium hydrogen carbonate did not significantly alter the excretion of HHP acid. The results show that the analysis of HHP acid in plasma or urine is useful as a biological monitor for exposure to HHPA.

Topics: Adult; Air Pollutants; Atmosphere Exposure Chambers; Breath Tests; Cyclohexanecarboxylic Acids; Environmental Monitoring; Epoxy Resins; Gases; Humans; Male; Middle Aged; Phthalic Anhydrides; Time Factors

A method for the determination of hexahydrophthalic acid, a metabolite of hexahydrophthalic anhydride, in human urine has been developed. The urine was worked-up by liquid-solid extraction, esterified with boron trifluoride-methanol, and analysed by capillary gas chromatography and selected-ion monitoring. Hexadeuterium-labelled hexahydrophthalic acid was used as the internal standard. The precision was 4% at 0.7 microgram/ml and 5% at 0.07 microgram/ml. The recovery of the acid for the overall method was 101% at 0.07 micrograms/ml of urine (with a coefficient of variation of 4%) and 95% at 0.7 microgram/ml (coefficient of variation 2%). The limit of detection was 20 ng/ml urine.

Topics: Chromatography, Gas; Cyclohexanecarboxylic Acids; Epoxy Resins; Humans; Hydrolysis; Mass Spectrometry; Occupational Exposure; Phthalic Anhydrides; Reference Standards