Fractionation of butyltin species during sample extraction and preparation for analysis

Solvent extraction and evaporative concentration steps are often used in procedures for the measurement of butyltins in environmental samples. As part of a larger study utilizing radiolabeled butyltins, the loss and fractionation of butyltins during sample preparation was investigated. TBT, DBT, and MBT were extracted from acidified seawater by hexane with efficiencies of about 95–99, 50–60 and 11% respectively. In addition, losses of about 70% of DBT were found during evaporative concentration of hexane. A variety of sediment extraction procedures were tested and none were found to be highly efficient for total butyltin extraction.     

Fractionation of Cu, Pb and Zn in certified reference soils SRM 2710 and SRM 2711 using the optimized BCR sequential extraction procedure

Sequential extraction of metals from solid media is a common analytical tool used in environmental and exploration geochemistry. A number of procedures exist, but without harmonization and standardization, meaningful comparisons are tenuous without baseline data. A newly developed, standardized sequential extraction procedure (optimized BCR) was applied to two contaminated certified reference soils from Montana, US (SRM 2710 and SRM 2711) for Cu, Pb and Zn. Four operationally defined fractions were isolated, acid extractable, reducible, oxidizable, and residual (by aqua regia). Fraction-specific concentrations, percentages and recoveries for Cu, Pb and Zn were used to explore differences between the optimized BCR procedure and three other sequential extraction schemes with published data for SRM 2710 and 2711 (i.e. Tessier scheme, Geological Survey of Canada scheme and the original BCR scheme). Results indicate significant differences between the four schemes, even for schemes that are closely associated (i.e. the original and optimized BCR schemes). Order-of-magnitude fraction-specific concentration differences were observed, especially for Pb in the reducible fraction. Differences between schemes are worrisome because trends varied between metals, between fractions and between reference soils. These data reinforce the need for increased adoption of standardized sequential extraction procedures and further examination of different solid media.     

Prenatal diagnosis of a true mosaic trisomy 20 substantiated by demonstration of a gene dosage effect for adenosine deaminase (ADA)

Fibroblasts from a fetus with the prenatal diagnosis of mosaic trisomy 20 were cloned by dilution plating. Adenosine deaminase (ADA), a biochemical marker for chromosome 20, was assayed in trisomic clones and normal clones as control. The cytogenetic diagnosis was substantiated by demonstration of a triplex gene dosage effect for ADA in the trisomic cells.     

Quantification of human amniotic fluid constituents by high resolution proton nuclear magnetic resonance (NMR) spectroscopy

We have investigated the ability of high-resolution proton NMR spectroscopy to provide a biochemical constituent screening of human amniotic fluid (AF). Proton NMR spectra were obtained at 300 MHz on AF from patients undergoing amniocentesis in the mid-trimester. Only AF from normal pregnancies (normal fetal karyotype, normal a-fetoprotein levels, normal birth outcome) was used in this study. The AF supernatant was lyophilized and resuspended in deuterated water containing 0.1 mm phosphate buffer and 6.02 mm disodium maleate. Identification of low molecular weight compounds was confirmed by two-dimensional NMR spectra (primarily correlated spectroscopy, or COSY) and standard addition techniques. A broad profile of compounds were ‘NMR visible’ in a single proton spectrum, including creatinine, glucose, organic acids (acetate, citrate, and lactate) and several amino acids (alanine, histidine, leucine, phenylalanine, tyrosine and valine). The proton spectrum was unaffected by prior freezing/thawing of AF samples. We were able to quantify compounds by comparison with an added concentration standard (maleate) at concentrations as low as 30 μm. Good agreement with literature values based on other analytical techniques was obtained.