Synthesis and some properties ofN-polynitromethyl derivatives of fused benzotriazoles

The procedures for the synthesis ofN-polynitromethyl derivatives of benzo[1,2-d;4,5d]ditriazole-4,8-dione are described. Some chemical properties of the compounds obtained are investigated.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 9, pp. 1623–1625, September, 1993.     

Determination of butyl- and phenyltin compounds in biological material by gas chromatography-flame photometric detection after ethylation with sodium tetraethylborate

A reliable and rapid speciation method for the simultaneous determination of butyl- and phenyltin species in biological samples has been developed. Three extraction procedures are compared: enzymatic hydrolysis and solubilization by ethanoic and hydrochloric acids. Derivatization is performed by the one-step ethylation/extraction procedure using the sodium tetraethylborate reagent directly in the aqueous phase in the presence of an isooctane layer. Analysis is performed using capillary gas chromatography coupled to flame photometric detection. The detection limits are in the range of a few ng(Sn)/g. Analysis of the environmental samples and the certified reference material demonstrates the accuracy of the analytical method.     

MULTIPHOTON EXCITATION OF A WATER MOLECULE IN INTENSE LASER FIELDS

A stretch vibration Hamiltonian of H_2O has been derived by using the second quantization, unitary transformations and the optimization of coefficients. The energy spectrum obtained from this Hamiltonian is in good agreement with that of experiments. The multiphoton excitation and the energy absorption of H_2O in intense laser fields have been calculated.     

The theoretical basis of column chromatography in multicomponent separations. Part 2: Peak capacity. Column systems with good selectivity

The selectivity of a column system, S, defined by equation 28, includes a variation coefficient (β) of plate number with capacity ratio which has a large influence on the peak capacity, as shown in Fig. 18. Some typical chromatograms are given. In order to predict S for a column system from Kovat's Index, equations 40 and 41 are given to calculate the constant of the carbon number rule for squalane at different temperatures or for different stationary phases. The specific retention value of heptane on squalane at different temperatures can be calculated from equation 42. The nonpolarity index, defined by equation 43, was used to calculate the retention value of heptane on various stationary phases. In liquid chromatography, the order of elution may be reversed by changing the composition of the eluent on the same chemically bonded silica (manufactured in China). The linear relations between the log retention values of different kinds of solutes or of a single solute on the silicas of different surface areas when using the same eluent are given.     

The properties of the metal complex hydrides

The essential features (geometries of the minima and of the saddle points, energy barriers) of the potential energy surface of the four hydrides YXH₄ mentioned in the title have been determined with two basis sets, of minimal and DZ quality respectively. The importance of the different extent of the deformation of the XH₄ group in the different structures of the four hydrides is brought out and discussed. The aspects of charge distribution and bonding are examined drawing on population analysis, comparison of the electrostatic molecular potentials and decomposition of the interaction energy (this last referred to the Y⁺ + XH ₄ ^– YXH₄ process). The capability of XH₃ in effecting the etherolytic disruption of the Y-H bond is finally brought out.     

Bestimmung von Melment in Zementmischungen durch UV-Spektralphotometrie

Ohne Zusammenfassung

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Determination of melment in cement mixtures by UV-spectrophotometry

     

Reactions of hexamethylditin and trimethyltin sulfide withN-thio-derivatives of phthalimide

The initial formation of organotin derivatives with Sn-S-N bonds in heterolytic reactions of hexamethylditin or trimethyltin sulfide withN-(chlorothio)phthalimide is suggested. Subsequent interaction of these compounds with sulfenyl chloride affordsN, N-thioorN, N-dithiobisphthalimide. Homolytic reaction of hexamethylditin withN, N-dithiobisphthalimide also occursvia an organotin intermediate, which, in the absence of a nucleophilic reagent, eliminates sulfur and converts intoN-trimethylstannylphthalimide.Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 12, pp. 2111–2114, December, 1993.     

Organic fuelled flames in selective ionization detectors for chromatography

Summary The selectivities of two flame-based ionization detectors identified as a Remote FID (RFID) and a Flame Thermionic Ionization Detector (FTID) have been improved by introducing methane as a fuel for the flame. Both the RFID and FTID feature a detector struture in which the ionization polarizer and collector are located several centimeters downstream of an oxygen-rich flame, rather than immediately adjacent to the flame as in a flame ionization detector. The RFID detects long-lived negative ions produced in the flame by the combustion of lead, tin, phosphorus, or silicon compounds. The FTID re-ionizes and detects neutral electronegative products generated by combustion of nitrogen, halogen, or phosphorus compounds. An organic-fuelled RFID can detect 1 pg Pb (Sn, P)/sec with a selectivity of the order of 10⁶ versus hydrocarbons. An organic fuelled FTID is applicable to detection of compounds at nanogram and higher levels. FTID selectivity for PCB compounds in a transformer oil matrix is of the order of 10⁵1. The improved selectivity achieved by using an organic-fuelled flame is also applicable to the detection of phospholipid and other non-volatile N, P, or Cl compounds using an FID/FTID detector accessory for a TLC/FID analyser.     

Astragalus membranaceus ultrafine powder alleviates hyperuricemia by regulating the gut microbiome and reversing bile acid and adrenal hormone biosynthesis dysregulation

Ethnopharmacological relevanceMetabolic syndrome is closely related to the intestinal microbiota and disturbances in the host metabolome. Hyperuricemia (HUA), a manifestation of metabolic syndrome, can induce various cardiovascular diseases and gout, seriously affecting a patient’s quality of life. Astragalus membranaceus has a long history as a commonly used traditional Chinese medicine to treat kidney disease in China and East Asia.Materials and methodsWe compared the therapeutic effect of benzbromarone and two different doses Astragalus membranaceus ultrafine powder (AMUP) in rats with HUA. Ultra-performance liquid chromatography-mass spectrometer was used to analyze the AMUP metabolism in the plasma, urine, and feces. Further, 16S ribosome RNA sequencing and feces metabolomic were performed to capture the variation of the gut microbiota and metabolites changes before and after drug administration.ResultsAMUP had a notable impact on reducing blood uric acid levels while protecting the liver and kidney. Drug metabolism analysis demonstrated that effective constituent flavonoids are distributed in the blood, whereas saponins remain in the intestine. Gut microbiota analysis showed that low-dose AMUP ameliorated HUA-induced gut dysbiosis by reducing the abundance of harmful bacteria and increasing that of some beneficial bacteria with anti-inflammatory properties, such as Clostridia, Lachnospiraceae, and Muribaculaceae. In addition, HUA-induced changes in metabolite contents in bile acid and adrenal hormone biosynthesis pathways were restored after treatment with AMUP.ConclusionLow-dose AMUP exerts remarkable therapeutic effects on HUA by regulating the gut microbiome and mediating gut metabolism pathways associated with uric acid excretion.     

Cycloarsanes (AsCF3)n (n = 4, 5) – Precursors for the Highly Reactive Diarsene F3CAs=AsCF3

Tetrakis(trifluoromethyl) cyclotetraarsane (F₃CAs)₄ ( 2 ) was used to repeat the UV initiated [4+2]‐cycloaddition reaction of the diarsene F₃CAs=AsCF₃ ( 1 ) with cyclohexa‐1,3‐diene (CHD) and to isolate single crystals of the cycloadduct 4 for a X‐ray diffraction analysis. 4 crystallizes in the space group and contains the diarsene group in its E‐configuration. 2 was also applied for [2+2]‐cycloaddition reactions of 1 with tBuC≡P and MeC≡CNⁱPr₂, but in contrast to positive results with (F₃CP)₄ the products were too labile for isolation. However, 2 was successfully used at room temperature as precursor for coordinating 1 as π‐donor ligand to the Pd(PPh₃)₂ complex fragment yielding η²‐bis(trifluoromethyl)diarsene‐bis(triphenylphosphane)‐palladium(0) 5 , which was characterized by X‐ray diffraction of single crystals and by spectroscopic investigations (NMR, IR, MS). Attempts to prove the existence of the diarsene 1 , generated by different methods, by spectroscopic studies very probably failed due to its extreme reactivity, not allowing the necessary concentrations for detection. Quantum chemical calculations of the stability of 1 with respect to dimerization, the stability of the [2+2]‐cycloadduct with 1‐di(isopropyl)aminopropyne and the energy difference between 4 and the 2,3‐dimethyl‐1,3‐butadiene cycloadduct of 1 were performed to understand the considerable differences between 1 and the related diphosphene F₃CP=PCF₃.