Trace analysis of airborne haloacetates

Haloacetates in various environmental compartments can be determined by gas chromatography-negative-ion chemical-ionization mass spectrometry after derivatization with 1-pentafluorophenyl diazoethane. Detection limits in absolute amounts per injection are between 0.01 fg (chlorodifluoroacetate) and 80 fg (monofluoroacetate). Sampling of haloacetates in urban air was performed by means of cylindrical denuders coated with alkalized glycerol. The haloacetates detected are trifluoro-, monochloro-, dichloro-, trichloro-, monobromo-, and dibromoacetate. The concentrations in ambient air fluctuate strongly, e.g. between 20 and 3000 pg/m³ for TFA. Haloacetates are also found in river waters and tree foliage. A major problem is interference from contamination with trifluoro- and trichloroacetate.     

The IL-10 gene is not involved in the predisposition to inflammatory bowel disease

Although genetic predisposition for inflammatory bowel disease (IBD) is well established, little is known about the accountable genes. The pathogenesis of IBD is characterized by an imbalanced activation of Th1- and Th2-lymphocytes. IL-10 represents an anti-inflammatory cytokine which downregulates the production of Th1-derived cytokines. To evaluate the role of the IL-10 gene in IBD, two polymorphisms in the promoter region (G/A at position -1082 and C/A at position -592) were genotyped in 142 patients with Crohn's disease (CD), 104 patients with ulcerative colitis (UC), and 400 healthy controls. Significant differences were not apparent, neither in the allele frequencies of either polymorphism, nor in the haplotype frequencies. Screening of the coding region of the IL-10 gene by polymerase chain reaction--single strand conformation polymorphism (PCR-SSCP) analysis revealed a rare sequence variation in exon 1 leading to an amino acid exchange (G-->A; G15R) in two patients with CD and five healthy controls. Therefore, polymorphisms of the IL-10 gene are not demonstrably involved in the predisposition of IBD in our cohorts of patients.     

Analysis of volatiles emitted by potato plants by means of a Colorado beetle electroantennographic detector

An electroantennographic detector based on the antenna of the Colorado potato beetle (Leptinotarsa decemlineata Say, 1824) was used to investigate volatile organic compounds emitted by injured potato plants (Solanum tuberosum L., 1753). Samples were collected on charcoal traps using the CLSA method. Analyses were performed with a GC-EAD-FID setup as well as a GC-MS system. The experiments revealed that several groups of compounds are perceptible to the Colorado potato beetle. The ability of the Colorado potato beetle to detect green leaf odours (e.g. (Z)-3-hexen-1-ol and (E)-2-hexenal), linalool and some terpenes has been noticed before [Visser et al., J. Chem. Ecol. 5 (1979) 13]. In this work the presence of (Z)-3-hexen-1-ol, (E)-2-hexenal and linalool in the potato odour could be confirmed. Moreover, β-myrcene, benzeneethanol, and several sesquiterpenes (e.g. caryophyllene and germacrene-D) were identified. The GC-EAD experiments reveal that apart from the green leaf odours and linalool prominent reactions of the Colorado bettle antenna are induced by benzeneethanol and the sesquiterpene fraction.     

Synthesis of Alumina and Silica-Containing Alumina Xerogel Hosts

Using the sol-gel process, we prepared two types of xerogels. Thin, transparent, crack-free alumina disks were prepared from aluminum tri-secondary butoxide (ASB). Addition of partially hydrolyzed tetraethylortho-silicate (TEOS) to such alumina sols produced translucent, warped silica-containing alumina xerogels. While the pure alumina xerogels were water soluble, addition of silica improved their durability. To understand the change in water solubility, we investigated the chemical and structural changes that occurred when silica was added. Characterization was performed using X-ray diffraction analysis, thermal analysis, nitrogen sorption analysis and ²⁷Al NMR spectroscopy.     

A diastereoselective approach for an asymmetric synthesis in pinnaic acid series

An enantiopure spiran-bearing advanced intermediate in pinnaic acid series was obtained in 11 steps starting with CN(R,S) building block.     

Solid phase micro-extraction of metal ions

A fused silica fibre coated with poly(dimethylsiloxane) was modified to produce a micro probe with ion exchanging capability. The liquid ion exchanger, di-(2-ethylhexyl)phosphoric acid (HDEHP), was used for the modification. The probe was used for the extraction of bismuth(III) from aqueous nitric acid solution. The extracted Bi(III) was desorbed into an acidic potassium iodide solution. The yellow colored BiI₄ ^– complex formed was determined by spectrophotometry.     

Electron paramagnetic resonance spectroscopic studies on the zero-valent rhodium complex [Rh(P(OPri)3)4] at X-and Q-band frequencies

The EPR spectroscopic properties of the zero-valent rhodium complex [Rh(P(OPrⁱ)₃)₄] have been examined at both X- and Q-band frequencies. The spectra show a large, essentially axial anisotropy and ligand hyperfine coupling to four equivalent ³¹P phosphorous nuclei. No resolved coupling to ¹⁰³Rh was detected. The data indicate a tetragonally compressed tetrahedral structure (D_2d) rather than the alternative C_3v geometry provisionally proposed for the related [Co(P(OMe)₃)₄] complex.     

Synthesis, characterization, and reactivity of new copper(II) complexes of 2-methylthio-N-(2-pyridylmethyl)acetamide

Copper(II) complexes were prepared with the new N(2)S(thioether) ligand 2-methylthio-N-(2-pyridylmethyl)acetamide (2-HL(N2S)). [Cu(2-L(N2S))Cl(MeOH)], which formed in the presence of excess triethylamine, is a distorted square pyramidal complex containing the ligand with the amide nitrogen deprotonated. The structurally analogous complex, [Cu(2-HL(N2S))Cl(2)], which formed in the absence of triethylamine, contains 2-HL(N2S) in the tautomeric imidic acid form. Neutral copper(II) N(2)S(thioether)S(thiolate) species were generated by addition of alkyl or aromatic thiolates to [Cu(2-L(N2S))Cl(MeOH)] and an unusual decomposition pathway was discovered.     

Validation study of a lateral-flow immunoassay for detection of ruminant by-product material in animal feeds and feed ingredients

An immunoassay with a lateral flow format has been developed for the detection of ruminant by-product material in animal feeds and feed ingredients. The test is designed for the analysis of animal feeds destined for feeding to ruminants to ensure that they do not contain ruminant by-products in violation of the ruminant-to-ruminant feed ban established by the U.S. Food and Drug Administration in 1997. This feed ban was established as a firewall against exposure of ruminant livestock animals to the prion agents responsible for neurological diseases such as bovine spongiform encephalopathy and scrapie. The test is designed for field use, e.g., at a feed mill, and yields a qualitative (presence/absence) result in 15-20 min. The objective of the study was to validate the lateral-flow test for detection of ruminant by-product material in a variety of finished animal feeds and feed ingredients. Results indicate that the test is specific for ruminant material and can detect as little as 1% ruminant material in these commodities.