Liquid chromatography with triple-quadrupole or quadrupole-time of flight mass spectrometry for screening and confirmation of residues of pharmaceuticals in water

LC–MS–MS has been performed with triple-quadrupole (QqQ) and quadrupole-time of flight (Q-ToF) instruments and has been used for screening and confirmation of pharmaceuticals in surface, drinking, and ground water. Screening was based on monitoring of one specific MS–MS ion of the target compounds. Confirmation of the identity of the pharmaceuticals was based either on the monitoring of two specific MS–MS ions and calculation of the ratio of their intensities, or on the exact masses of MS–MS product ions obtained for a molecular ion by use of LC–Q-ToF MS. The set of pharmaceuticals included four analgesics (acetylsalicylic acid, diclofenac, ibuprofen, and paracetamol), three antibiotics (sulfamethoxazole, erythromycin, and chloramphenicol), five blood-lipid regulators and beta-blockers (fenofibrate, bezafibrate, clofibric acid, bisoprolol, and metoprolol), and the anti-epileptic drug carbamazepine. Limits of quantification ranged from 5 to 25 ng L^–1. Fifty-six samples were analysed and residues of the pharmaceuticals were detected in almost all surface and groundwater and in some drinking water samples. The identity of the compounds could be confirmed by use of both QqQ- and Q-ToF-based LC–MS–MS. However, the latter technique has the distinct advantage that a large number of pharmaceuticals can be screened and confirmed at low concentrations (1–100 ng L^–1) in one run.     

The question of the production of Plantaglyutsid

The stage of extracting Plantaglyutsid from the leaves of rippleseed platain has been optimized by the methods of mathematical statistics. Information has been obtained on the optimum parameters of performing the process, as a result of which the yield of desired product has been increased and the amount of energy used and the consumption of extractant have been decreased.Tahskent Pharmaceutical Institute. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 735–737, November–December, 1985.     

Molecular heterogeneity and antiviral and interferon-inducing activities of the drug Savrats

The molecular-mass distribution of the drug Savrats has been studied by gel filtration on HW-55 f. It has been shown that the drug is heterogeneous and that the fraction with a molecular mass of 25–25 kDa exhibits a high biological activity.Mirzo Ulugbek Tashkent State University, fax (3712) 46 24 72. Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 112–114, January–February, 1998.     

In vitro biosynthesis,isolation, and activities of nuclear glycoproteins

It has been shown by HPLC, electrophoresis, etc., that, in vitro, the nuclei of neurons of rabbit and cow brains synthesize two glycoproteins (M 25–30 kDa and 10–15 kDa). The influence of some neurotropic compounds on the kinetics of the nuclear protein synthesis has been investigated. New inhibitors of this biosynthesis have been found.A. S. Sadykov Institute of Bioorganic Chemistry, Academy of Sciences of the Republic of Uzbekistan, Tashkent, fax 627071. Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 112–118, January–February, 1994.     

Chemical composition of the rhizomes of the Rhodiola rosea by the HPLC method

The component composition of extracts of the rhizomes ofRhodiola rosea has been studied by the HPLC method; the amount of rosavin has been determined and its lability on the autofermention of the raw material has been established.All-Union Scientific-Research Institute of Medicinal Plants, Scientific-Production Combine, Moscow. Translated from Khimiya Prirodnykh Soedinenii, No. 2, pp. 188–193, March–April, 1991.     

Optimization of the precipitation of Plantaglyutsid from evaporated aqueous extracts

The optimization of one of the stages of the technology of Plantaglyutsid — its precipitation from the evaporated aqueous extract with ethanol — has been optimized by the methods of mathematical statistics. Information has been obtained on the optimum parameters for performing the process with the aim of achieving the maximum yield of preparation and lowering the consumption of raw material.Tashkent Pharmaceutical Institute. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 312–315, May–June, 1985.     

Adsorption of low level51Cr(VI) from aqueous solution by bismuth trioxide: Kinetic and IR study

Radiotracer technique has been used for the investigation of adsorption of chromium (VI) traces on bismuth trioxide from aqueous solution. The effect of pH (2–10), concentration of chromate solution (10^–6–10^–2M) and temperature (303–323 K) has been thoroughly investigated. The influence of certain foreign ions has also been studied. The calculated kinetic and thermodynamic parameters indicate the first order rate law, spontaneity and exothermic nature of the adsorption process. Further, IR studies have established the chemical interaction between the sorbate and sorbent and a possible mechanism of the sorption process based on ligand exchange has been proposed.     

Spectroscopic characterization of environmentally relevant C10-chloroterpenes from a photochemically modified toxaphene standard

Twenty-five pure environmentally relevant toxaphene components have been isolated from photochemically modified technical toxaphene by means of a combination of column chromatography on silica gel and preparative high resolution liquid chromatography. These compounds are 6 chlorinated camphenes (1–3, 5, 7, and 11) and 19 chlorinated bornanes (4, 6, 8–10, 12–16, 18–24, 26, and 27 according to Table 1). Two further chlorobornanes (17 and 25) have been isolated from a highly chlorinated mixture obtained by the excess chlorination of 2-exo,10-dichlorobornane. The structural elucidation of the isolated compounds has been carried out with spectroscopical methods.     

Competitive bindings of histones with DNA in formation of plant nucleohistones

An acid form of ricin — ricin T — with a molecular weight of 58 kDa, an isoelectric point, pI, of 7.0–7.1, and a sedimentation coefficient of 4.60 S has been isolated from the seeds of the Central Asian castor-oil plantRicinus communis by gel filtration on Sephadex G-75 followed by ion exchange chromatography on DEAE- and CM-celluloses. The amino acid composition and the N-terminal amino acid residues of ricin T have been determined.Institute of the Chemistry of Plant Substances, Uzbek Academy of Sciences, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 883–887, November–December, 1987.     

Effect of deprotonation of ion-radical pairs on yield of radicals

In the example of ion-radical pairs (IRPs) formed in electron-transfer quenching of triplet states of the dyes methylene blue and eosin (electron acceptors) by phthalohydrazides (electron donors) in aqueous caustic solutions, it has been found that phthalohydrazide radicals are deprotonated directly in the IRP during their lifetime by the external base (OH^–), and a study has been made of this reaction. The yields of radicals from the deprotonated IRPs are 2–3.8 times those from the original IRPs; this difference is related to an increase in AG of IRP recombination as a result of deprotonation. In the region of high concentrations of OH^–, experimentally determined dependences of the yield of radicals on [OH^–] deviate from the relationships calculated with an exponential model of IRP destruction; this deviation is explained by a nonstationary nature of the diffusion of OH^– to the IRP immediately after the IRP is formed.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 6, pp. 1291–1295, June, 1990.     

Hysteresis effect and autooscillation phenomena in the oxidation of 1-hexene on palladium

The gas-phase oxidation of 1-hexene on a palladium film has been investigated in a gradient-free reactor at atmospheric pressure and temperatures of 293–693 K, at flow rates of 0.3–0.15 liter/min and an initial concentration of hexene in air of 15.5·10^–4 M. Autooscillation phenomena have been observed and a hysteresis effect in the reaction rate as function of temperature, caused by the branched-chain heterogeneous-homogeneous reaction mechanism.Translated from Teoreticheskaya i éksperimental'naya Khimiya, Vol. 24, No. 1, pp. 107–110, January–February, 1988.     

Conformational Mobility of 4,4′-Bisdimethyl-Aminobenzophenone in the Excited State

Quantum-chemical calculations on various conformational states of the molecule of Michler’s ketone have been carried out by semi-empirical and non-empirical methods (HyperChem 7.0 suite of programs and Gaussian 98). The influence of solvation on the relative levels of different orbital types and on the spin states of the molecule has been examined. The possibility of the TICT process occurring in polar media, which may have an important effect on the spectral characteristics of Michler’s ketone, has been investigated.__________Translated from Teoreticheskaya i Eksperimental’naya Khimiya, Vol. 41, No. 3, pp. 185–189, May–June, 2005.     

Isolation of cholesterol isononatriacontanate from sheeps' wool wax

Summary Cholesterol isononatriacontanate has been isolated from sheep's wool wax by chromatography on silica gel and alumina.Institute of Organic Chemistry, Academy of Sciences of the Kirgiz SSR, Frunze. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 820–821, November–December, 1977.     

Membrane-active properties of crambin

A thionin-like protein with M. M. 5kDa has been isolated fromCrambe kotschyana seeds. It has been shown that crambin possesses, a low lytic action on erythrocytes but inhibits the Ca-ATPase of the sarcoplasmic reticulum of rabbit skeletal muscles. A disordering action of crambin on the structures of both the sarcoplasmic reticulum and liposomes has been established by ESR and microcalorimetry.Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 82–88, January–February, 1998.     

Solid-phase synthesis of oligonucleotides representing fragments of trp promoters

The self-complementary oligonucleotides AACTAGTT and AGTTAACT, which are homologs of functionally important sections of trp promoters of three related bacteria, have been synthesized by the solid-phase method. A new block variant of synthesis on a polymer has been worked out and has been used for obtaining the octanucleotides AACTAGTTp and AGTTAACTp.M. V. Lomonosov Moscow State University. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 362–369, May–June, 1984.     

Spectral-fluorescent properties of maize grain trypsin inhibitor

The trypsin inhibitor isolated from maize grain has been investigated by the methods of IR, UV, fluorescence, derivative, and differential spectroscopy. Its spectral characteristics have been determined and the influence of the temperature and of a detergent on the structure of the protein has been studied.Scientific-Research Institute of Biology, Dnepropetrovsk State University, Dnepropetrovsk. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 375–381, May–June, 1989.     

1,1,4,4-Tetranitrobutane-2,3-diol and its derivatives. 1. Reaction of dinitromethane potassium salt with glyoxal. Crystal structure of 1,1,4,4-tetranitrobutane-2,3-diol and its diacetate

The synthesis of 1,1,4,4-tetranitrobutane-2,3-diol has been carried out via the reaction of the dinitromethane potassium salt with glyoxal, at pH values of 7–8 after reagent mixing and 5.5 at the end of the reaction, in the temperature range 35–37°C. X-ray crystal structure analysis has been performed on 1,1,4,4-tetranitrobutane-2,3-diol and its diacetate. The conformations of these molecules are stabilized to a significant extent by O^–...N⁺-type electrostatic interaction, which was confirmed by quantum-mechanical calculations on 2,2-dinitroethanol as a model molecule.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 4, pp. 830–834, April, 1991.     

Refinement of the crystal structure of (RS)-carnitine hydrochloride

A single crystal of (RS)-carnitine hydrochloride has been obtained, and its crystal structure has been refined by an x-ray structural experiment.Tashkent Pharmaceutical Institute. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 842–844, November–December, 1991.     

Investigations in the fie ld of substituted furanurona ldehydes steric directivity of the nitromethane condensation

Summary 1. The condensation of the anomeric methyl 2,3-di-O-benzyl-D-xylofuranosiduronaldehydes with nitromethane has been studied.2. It has been shown that the position of the substituent at the glycosidic center has an influence on the steric directivity of this reaction.3. The structure of the 6-nitro-6-deoxyhexofuranosides synthesized has been confirmed by their conversion into known derivatives of methyl D-glucofuranosides.Translated from Khimiya Prirodnykh Soedinenii, No. 1, pp. 8–12, January–February, 1972.     

Denaturation and renaturation of the 11S globulin of cotton seeds by polarography

It has been established by a polarographic analysis of the globulins of cotton seeds that the 7S and 11S golublins possess a two-step polarographic wave with a half-wave potential of –1.42 V. On the basis of the results of a study of the kinetics of thermal denaturation the high lability of the 11S globulin on heating has been shown. The conditions have been determined of the complete denaturation of the 11S globulin in 8 M urea solution and it has been established that the latter is an irreversible process.Institute of the Chemistry of Plant Substances of the Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 6, pp. 809–813, November–December, 1980.