a four-step synthesis of monoalkylated benzidin is reported for immunogen preparation against benzidin dye. Use of 10% H2SO4/ dioxan for N-Boc cleavage avoids the cyclisation of 4-benzidinyl butyric acid into the corresponding lactam observed with the classical TFA/ CH2Cl2 system. 相似文献
This article describes a rapid LC–MS/MS target screening method based on an automated extraction of 5 μL dried blood spots (DBS), two 5 min chromatographic runs on orthogonal phase columns (RP and Hilic) and a data dependent acquisition (DDA) of product ions spectra for the reliable identification of the detected compounds. The extraction step was performed in 2 min by using the LC autosampler itself in 96-well plates. This procedure was evaluated using 22 model compounds frequently encountered in forensic investigations, i.e., cocaine, benzodiazepines, amphetamines, opioids, antidepressants and antipsychotics. These investigations showed that even if the extraction step was reduced to a minimum, the extraction recoveries were satisfactory (median value of 40 %) and allowed for the detection of the model compounds in their therapeutic ranges, with the exception of morphine. Moreover, the use of two different chromatographic columns broadened the number of screening targets to those that behaved poorly under RP conditions, such as amphetamines or glucuronides, while keeping chromatographic gradients very short. This procedure was applied to 34 authentic post-mortem cases. It allowed the detection of 89 % of the compounds that were quantified in the routine procedures and the formal identification of 77 % of the compounds using their product ions spectra. These results were considered more than satisfactory compared to routine screening alone (GC–MS and LC-DAD, 55 % compound identification). The method described in this article is therefore a powerful approach for a fast, reliable and efficient target screening of drugs in forensic and clinical investigations. 相似文献
In this paper, we introduce a Hilbert style axiomatic calculus for intutionistic logic with strong negation. This calculus is a preservative extension of intuitionistic logic, but it can express that some falsity are constructive. We show that the introduction of strong negation allows us to define a square of opposition based on quantification on possible worlds. 相似文献
Synchrotron radiation techniques (μ-XRF and μ-XANES) were applied to the study of organic-rich phosphatized limestones of NW Greece (Epirus). The results revealed uranium accumulation in areas of the material containing, among others, carbonate apatite (francolite) and organic matter. The UL3-edge of μ-XANES spectra showed that uranium was present in tetravalent form. U-bearing francolite crystals were separated from the rock and characterized by Raman spectroscopy and microprobe. The analysis of the crystals also indicated the presence of sodium and sulfur. The uranium presence in the crystals was also visualized, after neutron irradiation and etching, by the observation of the fission tracks.
A graph is -colorable if it admits a vertex partition into a graph with maximum degree at most and a graph with maximum degree at most . We show that every -free planar graph is -colorable. We also show that deciding whether a -free planar graph is -colorable is NP-complete. 相似文献