Determination of cyanide in blood by electrospray ionization tandem mass spectrometry after direct injection of dicyanogold

An electrospray ionization tandem mass spectrometric (ESI-MS-MS) method has been developed for the determination of cyanide (CN^–) in blood. Five microliters of blood was hemolyzed with 50 μL of water, then 5 μL of 1 M tetramethylammonium hydroxide solution was added to raise the pH of the hemolysate and to liberate CN^– from methemoglobin. CN^– was then reacted with NaAuCl₄ to produce dicyanogold, Au(CN)₂^–, that was extracted with 75 μL of methyl isobutyl ketone. Ten microliters of the extract was injected directly into an ESI-MS-MS instrument and quantification of CN^– was performed by selected reaction monitoring of the product ion CN^– at m/z 26, derived from the precursor ion Au(CN)₂^– at m/z 249. CN^– could be measured in the quantification range of 2.60 to 260 μg/L with the limit of detection at 0.56 μg/L in blood. This method was applied to the analysis of clinical samples and the concentrations of CN^– in the blood were as follows: 7.13 ± 2.41 μg/L for six healthy non-smokers, 3.08 ± 1.12 μg/L for six CO gas victims, 730 ± 867 μg for 21 house fire victims, and 3,030 ± 97 μg/L for a victim who ingested NaCN. The increase of CN^– in the blood of a victim who ingested NaN₃ was confirmed using MS-MS for the first time, and the concentrations of CN^– in the blood, gastric content and urine were 78.5 ± 5.5, 11.8 ± 0.5, and 11.4 ± 0.8 μg/L, respectively.     

Palladium-catalyzed stereospecific 1,4-hydrogen migration of cis-cyclohex-2-en-1,4-diol systems

It has been revealed that the generation of 2-cyclohexenones from cis-1,4-dihydroxycyclohexene derivatives under PdCl₂(PPh₃)₂-HCO₂NH₄ system takes place in an intramolecular pathway involving unprecedented mode of suprafacial 1,4-hydrogen migration across the 1,4-allylic centers.     

Determination of tin by resin-suspension electrothermal atomic absorption spectrometry after enrichment as the complex with ammonium pyrrolidinedithiocarbamate.

A resin-phase extraction method has been optimized for the trace determination of tin(II) by ETAAS. Tin(II) was extracted on a finely divided anion exchange resin as the complex with ammonium pyrrolidinedithiocarbamate (APDC). The resin was collected on a membrane filter and then dispersed in 1.00 ml of 1 mol l(-1) nitric acid containing 100 microg of Pd(II) and 60 microg of Ni(II). The resulting resin suspension was subjected to GFAAS. The proposed method was applied to the determination of tin(II) in hydrochloric acid.     

Nonstoichiometric polycondensation of 4‐acetoxybenzoic acid in the presence of monoacetate

Nonstoichiometric polycondensation of 4‐acetoxybenzoic acid (ABA) was examined in the presence of three kinds of aromatic monoacetates: 4‐hexyloxyphenyl acetate, 4‐decyloxyphenyl acetate, and 4‐octadecyloxyphenyl acetate. Polymerizations were carried out in liquid paraffin at 320 °C under nonstoichiometric conditions, in which the acetoxy group was in large excess of the carboxyl group. Poly(4‐oxybenzoyl) (POB) was obtained as crystal at the molar ratio of monoacetates in feed (χ) of less than 80 mol %, meaning that the concentration of the acetoxy group was five times that of the carboxylic group. The obtained POB possessed much higher number average degree of polymerization (DP_n), ranging from 353 to 467, than the calculated DP_n on the basis of χ. High molecular weight polymer was synthesized even under nonstoichiometric conditions via crystallization of oligomers and the following solid‐state polymerization in the crystals. © 2005 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 43: 1757–1766, 2005     

Invariance of selfinjective algebras of quasitilted type under stable equivalences

We prove that the class of finite dimensional selfinjective algebras over a field which admit Galois coverings by the repetitive algebras of the quasitilted algebras, with Galois groups generated by compositions of the Nakayama automorphisms with strictly positive automorphisms, is invariant under stable and derived equivalences. Dedicated to Claus Michael Ringel on the occasion of his sixtieth birthday     

On the relaxation of trapped electrons in glassy hydrocarbons irradiated at 4 K

In contrast to previous reports e^?_t in 3MHx produced at 4 K shows trap relaxation when warmed to 77 K. The relaxation in 3 MHx and 3MP occurs without loss of e^?_t, and results in an increase in ?_max as well as a shift of λ_max.     

Synthesis and characterization of poly[4-(4-hydroxyphenoxy) benzoic acid]

Poly[4-(4-hydroxyphenoxy) benzoic acid] was prepared by the bulk polycondensation of 4-(4-acetoxyphenoxy) benzoic acid. Polycondensation was conducted at 350°C for 3 h under a reduced pressure of 0.1 mmHg and gave a polymer with X?n of 255. The polymer was characterized by elemental analysis, IR spectroscopy, differential scanning calorimetry, and wide-angle X-ray measurement. The crystal/nematic and nematic/isotropic phase transition temperatures of polymer, which depend on the molecular weight, were observed at about 300°C and 410°C, respectively. The polymers with low molecular weights showed nematic textures above 300°C. This nematic/isotropic phase transition temperature is lower than that of poly (4-hydroxybenzoic acid). This thermal behavior of polymer comes from ether units, which increase the flexibility (the rotation or torsion of skeletal bonds) of the polymer chain. © 1994 John Wiley & Sons, Inc.     

A new route to 1-phenylnaphthalenes by cycloaddition: a simple and selective synthesis of some naphthalene lignan lactones

2-(2-Dithianyl)benzhydrols ($\text{2}$ a-c) undergo facile cycloaddition reaction with maleic anhydride under thermal conditions to give 1-phenyl-naphthalenes ($\text{7}$ a-c) in one step. The naphthalenes ($\text{7}$ a-c) have been converted into the naphthalene lignan lactones, ($\text{9}$ a-c) and ($\text{10}$ a-c).