Detection of Anti-Ulcer Drugs and Their Metabolites in Horse Urine by Liquid Chromatography – Mass Spectrometry

This paper describes a convenient method for the extraction and detection of eight anti-ulcer drugs simultaneously in horse urine, a relatively complex and viscous matrix, using a single-step liquid-liquid extraction followed by high-performance liquid chromatography – mass spectrometry (LC-MS). Anti-ulcer drugs were isolated from horse urine by salting out and liquid-liquid extraction. Detection of these drugs at concentrations below 1 ng mL^?1 could be achieved using LC-MS-MS in the positive atmospheric pressure chemical ionisation (APCI) mode. The above analysis was also extended to elimination studies of horses administered with ranitidine and omeprazole. The urinary elimination data of these two drugs suggest that ranitidine was eliminated from horse urine at a much slower rate than omeprazole. In addition, three ranitidine metabolites and six omeprazole metabolites were identified for the first time in equine urine samples.     

Mechanical analysis on rocket propellants

The mechanical properties of solid rocket propellants are very important for good functioning of rocket motors. During use and storage the mechanical properties of rocket propellants are changing, due to chemical and mechanical influences such as thermal reactions, oxidation reactions or vibrations. These influences can result in malfunctioning, leading to an unwanted explosion of the rocket motor. Most of modern rocket propellants consist of a polymer matrix (i.e. HTPB) filled with a crystalline material (i.e. AP, AN). However, the more conventional double base propellants consist of a solid gel matrix with additives, such as stabilizers. Both materials show a mechanical behaviour, quite similar to that of general polymers. To describe the material behaviour of both propellants a linear visco-elastic theory is often used to describe the mechanical behaviour for small deformations. Because the time-temperature dependency is also valid for these materials a mastercurve can be constituted. With this mastercurve the response properties (stiffness) under extreme conditions can be determined. At TNO-PML a mastercurve of a double base propellant was constituted using dynamical mechanical analysis (DMA) and compared with a mastercurve reduced from conventional (static) stress relaxation tests. The mechanical properties of this double base propellant determined by DMA were compared with conventional (quasi-static) tensile test results. This revised version was published online in July 2006 with corrections to the Cover Date.     

THE PRESENCE OF PHOTOREACTIVE β-CARBOLINE FLUOROPHORES IN WEATHERED WOOL KERATIN

Abstract Solvent-cleaned Merino wool, which was enzymatically digested with protease K, displayed a fluorescence maximum at 500 nm when excited at 430 nm. The yield of this emission was approximately 15 times greater for a fiber tips digest than for a digest of the mid-length region of the same fibers.
Separation of the components in the wool tip digest by silica gel thin-layer chromatography revealed the presence of several fluorescent species. The chromatographic mobility of these species was similar to the behavior observed in a preparation of authentic 1-methyltetrahydro-P-carboline, 1,3-dicarboxylic acid.
Mass spectroscopy of the fluorescent compounds in the wool tip digest displayed molecular ions, [M + H]⁺ with m/z = 273.0890 and 257.0560, and molecular weights that define the formulae C₁₄H₁₂N₂O₄ and C₁₁H₈O₄N₂, respectively, which correspond to β-carboline 1,3-dicarboxylic acids. Mass spectral evidence also indicates the presence of two other β-carbolines.     

BIOLOGICAL ACTIVITIES OF PHTHALOCYANINES-X. SYNTHESES AND ANALYSES OF SULFONATED PHTHALOCYANINES

Abstract— Synthetic methods to obtain selectively sulfonated metallo phthalocyanines are compared. Both condensation and direct sulfonation procedures lead to mixtures of mono- to tetrasulfonated products which are resolved by reverse phase liquid chromatography in buffered aqueous-methanol. The proportion of sulfonated derivatives is examined as a function of the starting reagents in the case of the condensation method, and as a function of the temperature and reaction time in the case of the direct sulfonation procedure. The number of sulfonate groups per phthalocyanine molecule is determined by oxidative degradation of the phthalocyanine ring followed by quantitative chromatographic analysis of the sulfophthalamide and phthalamide fragments.     

The synthesis of 1,4-diazacycl[3,2,2]azine

The diazaanalog of “cycl[3,2,2]azine”, “1,4-diazacycl[3,2,2]azine” (1,4,7b-triazacyclopent-[cd]indene) and its 2-methyl derivative were prepared. These compounds are subject to facile acid-catalyzed hydrolysis affording substituted imidazo[1,2-a]pyridines.     

Thermal decomposition of the composite hydrotalcites of iowaite and woodallite

The thermal stability and thermal decomposition pathways for synthesized composite iowaite/woodallite have been determined using thermogravimetry analysis in conjunction with evolved gas mass spectrometry. Dehydration of the hydrotalcites occurred over a range of 56–70°C. The first dehydroxylation step occurred at around 255°C and, with the substitution of more iron(III) for chromium(III) this temperature increased to an upper limit of 312°C. This trend was observed throughout all decomposition steps. The release of carbonate ions as carbon dioxide gas initialised at just above 300°C and was always accompanied by loss of hydroxyl units as water molecules. The initial loss of the anion in this case the chloride ion was consistently observed to occur at about 450°C with final traces evolved at 535 to 780°C depending of the Fe:Cr ratio and was detected as HCl (m/z=36). Thus for this to occur, hydroxyl units must have been retained in the structure at temperatures upwards of 750°C. Experimentally it was found difficult to keep CO₂ from reacting with the compounds and in this way the synthesized iowaite-woodallite series somewhat resembled the natural minerals.