Quantitative detection of trichloroacetic acid in human urine using isotope dilution high-performance liquid chromatography-electrospray ionization tandem mass spectrometry.
The chemical disinfection of drinking water to control microbial contaminants results in the formation of disinfection byproducts (DBPs). The volatile trihalomethanes and the nonvolatile haloacetic acids (HAAs) are the most prevalent DBPs. It is important to monitor human exposure to HAAs because of their potential adversehealth effects, such as cancer. Among the HAAs, urinary trichloroacetic acid (TCAA) is a potential valid biomarker for assessing chronic ingestion exposure to HAAs from drinking water. We have developed a rugged, high-throughput, sensitive, accurate, and precise assay for the measurement of trace levels of TCAA in human urine using a simple solid-phase extraction (SPE) cleanup followed by isotope dilution high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). TCAA is extracted from the urine using SPE, separated from other extract components by reversed-phase HPLC, and analyzed by negative ion electrospray ionization-isotope dilution-MS/MS using a multiple reaction monitoring experiment. The method is simple and fast and is not labor intensive (sample preparation and analysis can be performed in approximately 15 min) with a limit of detection of 0.5 ng/mL in 1 mL of urine.
Determination of haloacetic acids in human urine by headspace gas chromatography-mass spectrometry.
Haloacetic acids (HAAs) are water disinfection byproducts (DBPs) formed by the reaction of chlorine oxidizing compounds with natural organic matter in water containing bromine. HAAs are second to trihalomethanes as the most commonly detected DBPs in surface drinking water and swimming pools. After oral exposure (drinking, showering, bathing and swimming), HAAs are rapidly absorbed from the gastrointestinal tract and excreted in urine. Typical methods used to determine these compounds in urine (mainly from rodents) only deal with one or two HAAs and their sensitivity is inadequate to determine HAA levels in human urine, even those manual sample preparation protocols which are complex, costly, and neither handy nor amenable to automation. In the present communication, we report on a sensitive and straightforward method to determine the nine HAAs in human urine using static headspace (HS) coupled with GC-MS. Important parameters controlling derivatisation and HS extraction were optimised to obtain the highest sensitivity: 120 microl of dimethylsulphate and 100 microl of tetrabutylammonium hydrogen sulphate (derivatisation regents) were selected, along with an excess of Na(2)SO(4) (6 g per 12 ml of urine), an oven temperature of 70 degrees C and an equilibration time of 20 min. The method developed renders an efficient tool for the precise and sensitive determination of the nine HAAs in human urine (RSDs ranging from 6 to 11%, whereas LODs ranged from 0.01 to 0.1 microg/l). The method was applied in the determination of HAAs in urine from swimmers in an indoor swimming pool, as well as in that of non-swimmers. HAAs were not detected in the urine samples from non-swimmers and those of volunteers before their swims; therefore, the concentrations found after exposure were directly related to the swimming activity. The amounts of MCAA, DCAA and TCAA excreted from all swimmers are related to the highest levels in the swimming pool water.
“ PARTIALLY-ACTIVATED ” FLUX RESIDUE IMPACTS ON ELECTRONIC ASSEMBLY RELIABILITIES
The reliabilities of the flux residue of electronic assemblies and semiconductor packages are attracting more and more attention with the adoption of no-clean fluxes by majority of the industry. In recent years, the concern of “partiallyactivated” flux residue and their influence on reliability have been significantly raised due to the miniaturization along with high density design trend, selective soldering process adoption, and the expanded use of pallets in wave soldering process. When flux residue becomes trapped under low stand-off devices, pallets or unsoldered areas (e.g. selective process), it may contain unevaporated solvent, “live” activators and metal complex intermediates with different chemical composition and concentration levels depending on the thermal profiles. These partially-activated residues can directly impact the corrosion, surface insulation and electrochemical migration of the final assembly. In this study, a few application tests were developed internally to understand this issue. Two traditional liquid flux and two newly developed fluxes were selected to build up the basic models. The preliminary results also provide a scientific approach to design highly reliable products with the goal to minimize the reliability risk for the complex PCB designs and assembly processes.