Evaluation of dynamic headspace with gas chromatography/mass spectrometry for the determination of 1,1,1-trichloroethane, trichloroethanol, and trichloroacetic acid in biological samples

In situ derivatization/solid‐phase microextraction coupled with gas chromatography/negative chemical ionization mass spectrometry for the determination of trichloroethylene metabolites in rat blood

“…However, decarboxylation of TCA to chloroform often occurred at high sampling temperatures, and relatively high LODs (limits of detection) were obtained, because no sample pre‐concentration steps were involved. A dynamic headspace method for the determination of TCA in urine was developed with a LOQ of 10 µg L −1 , but simultaneous determination of DCA and TCOH was not achieved 29. These methods involve the use of solvents and significant numbers of sample preparation steps that are quite time‐consuming.…”

Determination of haloacetic acids in human urine by headspace gas chromatography–mass spectrometry

“…DCAA are excreted in humans between 20 and 36 min after an intravenous administration of sodium dichloroacetate [23] and more than 50% of the dose administered is recovered in rat urine, unchanged [24]. With regard to TCAA, several experiments have been carried out in workers exposed to trichloroethylene since it is mainly metabolised into TCAA; in this case the sampling time is critical because the metabolite is excreted, from 50 until 120 h after exposure, over the range 0.5 and 90 mg/l [15,16,19,20]. There is very little information in the literature about direct ingestion of TCAA in humans [12] and nothing about MCAA since its concentration in urine is too low to detect.…”

“…Dichloroacetic and trichloroacetic (TCAA) acids have previously been measured in urine by using liquid chromatography [10,11], although gas chromatography (GC) is the most widely used technique due to its inherent advantages. GC determination requires a preliminary derivatisation step due to the low volatility and high polarity of these compounds; several of the derivatising reagents employed have been dimethylsulphate [9], acid-alcohol [12][13][14][15], BF 3 -methanol [16] or pentafluorobenzyl bromide [17]. These methods are characterised by numerous separation steps such as: centrifugation of the urine sample, acidification and extraction with methyl tert-buthyl ether (MTBE), centrifugation, evaporation and finally derivatisation.…”

“…In all cases the sensitivity is inadequate to quantify TCAA in human urine and, in addition, it is difficult to discriminate between the amount of TCAA and chloroform (both DBPs) present in the native sample. Dynamic HS (purge and trap, P&T) CG-MS has also been used to determine TCAA in human urine, providing a low sensitivity (LOD, 3 g/l); the derivatising reagent is 600 l of sulphuric acid-methanol per 300 l of urine using the soil module of a modified P&T autosampler [15].…”

Functionalization of Carbon Nanotubes with Water‐Insoluble Porphyrin in Ionic Liquid: Direct Electrochemistry and Highly Sensitive Amperometric Biosensing for Trichloroacetic Acid

“…[2,3] Thus, the World Health Organization has urgently appealed for the development of rapid, reliable, and accurate analytical methods for the detection of TCA. [4] Currently, TCA is generally measured by gas chromatography with precolumn trap enrichment and microwave plasma emission detection, [5] headspace gas chromatography with electron capture or mass spectrometric detection, [6,7] and high-performance liquid chromatography with solid-phase microextraction and electrospray mass spectrometric detection. [8] Although these methods have adequate sensitivity, they suffer from the need for expensive equipment, time-consuming derivatization and extraction processes, and professional operation.…”