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Study on fluorination of 2,3-dideoxy-2,3-(N-tosylepimino)-alpha-D-allopyranosides, and synthesis of 3'-deoxy-3'-fluorokanamycin B and 3',4'-dideoxy-3'-fluorokanamycin B.
Reaction of the structurally rigid methyl 2,3-dideoxy-4,6-O-isopropylidene-2,3-(N-tosylepimino)-alpha-D-a llopyranoside (6) with KHF2 in DMF at 150 degrees gave initially methyl 2,3-dideoxy-2-fluoro-4,6-O-isopropylidene-3-tosylamido-alpha-D-altrop yranoside (10) by N-tosylepimine-ring opening, and 10 was gradually converted into the stable methyl 2,3-dideoxy-3-fluoro-4,6-O-isopropylidene-2-tosylamido-alpha-D-glucopyra noside (11). A reversible mechanism involving 6 and 10 has been proposed. In the mobile methyl 2,3-dideoxy-2,3-(N-tosylepimino)-alpha-D-allopyranoside (7) and the corresponding 4,6-di-O-acetyl (8) and -di-O-methyl derivatives (9), reactions with KHF2 proceeded comparatively rapidly giving the corresponding 3-deoxy-3-fluoro-alpha-D-glucopyranosides as the major products. A slightly different reaction mechanism for the mobile compounds has been proposed. By application of this study, 3'-deoxy-3'-fluorokanamycin B was prepared by treatment of 4",6"-O-cyclohexylidene-2'-deamino-3'-deoxy-3'-epi-6'-N-methoxycarbonyl- 1,3, 3"-tri-N-tosyl-2',3'-(N-tosylepimino)kanamycin B (21) with KHF2 as the key reaction. 3',4'-Dideoxy-3'-fluorokanamycin B was also prepared. Both compounds were active against resistant bacteria producing 3'-modifying enzymes.
Carbohydrate Sequence↗
Ion-pair partition chromatography in the analysis of drugs and biogenic substances in plasma and urine.
Liquid-liquid chromatography based on the ion-pair partition technique gives separation systems of high efficiency when silica micro-particles are used as the support for the stationary phase. With 10-mum particles, plate heights of the order of 40-70 mum have been achieved with a linear velocity of 0.25 cm/sec. The retention in ion-pair partition systems is determined by the nature and concentration of the counter ion, and the properties of the mobile phase also have a major influence. It is often possible to predict the selectivity, and this can be controlled by varying the composition of the mobile phase. This paper describes the application of ion-pair partition chromatography to the bioanalysis of drugs, drug metabolites and biogenic substances. Typical counter ions in the stationary phase were methanesulphonate and perchlorate for ammonium compounds and tetrabutylammonium for the separation of organic anions. Determinations by liquid chromatography were demonstrated for quinidine and dihydroquinidine, metanephrine and normetanephrine and for imipramine and its demethyl metabolite in plasma. A quaternary ammonium compound, QX-572, was determined in urine and chromatograms are shown for the isolation of indoleacetic and hydroxyindoleacetic acid in urine. The methods have been used in routine analysis. Ultraviolet detection has permitted the determination of highly absorbing compounds down to the 10-ng level in plasma and urine.
Absorption↗
Mass transfer in rectangular chromatographic channels.
Rectangular channels are explored nowadays for use in chromatographic and electrophoretic separations, especially after the possibilities of micromachining have become available to separation scientist. Expressions for plate heights expected for such experiments with an infinite channel width has been given by Giddings, while Golay derived the effect of finite channel width for unretained components. However, it remains unclear how the classical equations for plate height for retained components should be modified when the effect of finite channel width is taken into account. Also, the application of electroosmotic propulsion of the mobile phase leads to a flow profile different from the Poiseuille-type profile assumed in the above treatments, and no equations seem to be available for this situation. In this work, these problems have been addressed by an approach involving numerical Fourier transforms. Expressions for the plate height contribution from mobile phase mass transfer as a function of characteristic length dc (the height of the channel, or the diameter for open cylindrical systems, OT), mean mobile phase velocity, um, diffusion coefficient Dm, retention factor, k', and width-to-height ratio, phi, can always be written as: H = dc2um/DmF(k', phi). For cylindrical open systems, F(k', phi) equals 1/96 (1 + 6k' + 11k'2)/(1 + k')2, the well-known Golay equation. In the present work, this is taken as a reference point; results are cast in the form F(k', n) = (A + Bk' + Ck'2)/(1 + k')2, where A, B and C replace the factors 1/96, 6/96 and 11/96 of the Golay equation. Values of A, B and C are reported for various values of phi. This is done for a selection from the large variety of conditions that can be imagined: Coating on one, two or four walls of the channel, non-uniform or uniform coating, pressure-driven (Poiseuille-type) or electro-osmotically-driven flow, surface charge on one, two of four walls, etc. It is found that the effect of finite channel width is large for unretained solutes (plate height for a wide channel is nearly eight times larger than that predicted when the finite channel width is ignored), whereas the plate height increase with retention is in many cases influenced only slightly.
Algorithms↗
Micellar liquid chromatography for the analysis of nucleosides and bases.
A new high-performance liquid chromatographic method for the analysis of nucleosides and bases was developed in which a micellar mobile phase is used. Separation was achieved on a polyvinyl alcohol (PVA) column by isocratic elution with micellar sodium dodecyl sulfate (SDS) as the mobile phase. The retention behavior of the nucleosides and bases was significantly different from that obtained by reversed-phase chromatography. Effect of pH, temperature, and concentration of SDS and the counter ion (Na+) on retention behavior were investigated. With the PVA column, the best conditions for an isocratic separation were 0.01 M SDS (pH 3.4) and a flow-rate of 2 ml/min at ambient temperature. Mechanisms for the retention of the nucleosides and bases on the PVA column with a micellar mobile phase were proposed and an application of the separation was demonstrated by the analysis of human serum.
Chromatography, Liquid↗
Management of renal cell carcinoma with level III thrombus in the inferior vena cava.
PURPOSE: Level III thrombus in the inferior vena cava poses a challenge to the surgeon due to its relative inaccessibility. We introduce a new system to redefine level III thrombus in anatomical relation to the hepatic veins and describe a technique of safe resection of these tumors through a transabdominal approach without recourse to cardiopulmonary bypass. MATERIALS AND METHODS: From August 1997 to July 2001, 23 patients underwent resection of renal cell carcinoma with a level III thrombus. Intraoperative as well as postoperative variables such as operative time, estimated blood loss, number of transfusions, cardiopulmonary bypass, postoperative complications, pathological findings and survival were recorded. RESULTS: A total of 15 male and 8 female patients with a mean age of 62 years (range 25 to 83) underwent resection of a level III thrombus emanating from renal cell carcinoma. Patients were divided into groups IIIa-9 with an infrahepatic thrombus, IIIb-6 with a hepatic thrombus, IIIc-5 with a suprahepatic, infradiaphragmatic thrombus and IIId-3 with a suprahepatic, supradiaphragmatic, infra-atrial thrombus. Mean operative time was 5 hours 42 minutes (range 4 to 7.5 hours). The number of transfusions was 0 to 4. Estimated blood loss was 100 to 5,000 cc (mean 500). Neither cardiopulmonary bypass nor veno-venous bypass was required. Median followup was 25 months. Two patients (9%) died, including 1 in the immediate postoperative period and the other from metastasis 15 months after surgery. At the last followup 3 patients (13%) had metastasis and 18 (78%) were disease-free for overall and disease-free survival rates of 91% and 78%, respectively. CONCLUSIONS: An aggressive surgical approach remains the mainstay of treatment to achieve cure. We believe that the extent of dissection is different in each subgroup and, therefore, the need exists to redefine level III thrombus of the inferior vena cava. The application of liver transplant techniques for mobilizing the liver off of the inferior vena cava as well as the inferior vena cava off of the posterior abdominal wall contributes to excellent exposure and enables adequate vascular control of the inferior vena cava.
Adult↗
A new, one-stage pedicled scrotal skin graft urethroplasty.
A new 1-stage procedure with a pedicled scrotal flap for bulbomembranous urethral reconstruction is described. The scrotal septum used as a pedicle provides good mobility to the flap. Because of this mobility the method appears to be applicable for reconstruction anywhere along the urethra.
Adenocarcinoma↗
Beyond your resume: a nurse's professional "portfolio".
Explore the source record for details and available documents.
Career Mobility↗
Career guidance for student nurses: an unmet need.
Career guidance is important both organizationally and for the individual, especially at a time of re-emerging concerns about retention, and increasing complexity of nursing careers due to rapidly changing systems of health care provision. A questionnaire survey of 1015 newly qualified registered general nurses explored their experiences of career guidance whilst students, in relation to three areas: . applying for first post . taking post-basic courses . longer term plans. Findings revealed that few students were provided with guidance. Furthermore, a substantial unmet need was demonstrated, especially in relation to discussions about individual career planning.
Career Mobility↗
Cytokines at the research-clinical interface: potential applications.
Developments in the characterization of growth factors and the recognition of their potential for clinical use has advanced through a number of stages. The development of clonogenic haemopoietic colony assays in the 1960s led to the discovery of colony-stimulating activity in the conditioned medium produced by certain cell lines. This activity was then purified and the colony-stimulating factors were identified. With rapid progress in molecular biology techniques in the 1980s, many further growth factors were cloned and produced on an industrial scale. Although erythropoietin, interferons, G-CSF, GM-CSF and IL-2 were all introduced into clinical practice as single agents, cytokines have more recently been investigated for use either in combination, or sequentially. Clinical trials are currently in progress to examine the optimum combinations and timing of administration. Current clinical applications include optimization of methods for mobilization of peripheral blood progenitor cells and amelioration of cytopenias following chemotherapy and bone-marrow transplantation. In the future, cytokines will be employed to expand stem and progenitor cells ex vivo, to improve gene transduction strategies, possibly to protect the gastrointestinal epithelium and as immunomodulators, both in vivo and in vitro. This review will focus on recently characterized growth factors including c-kit ligand/stem cell factor, flt3 ligand, c-mpl ligand/thrombopoietin and interleukins-11, 4, 7, 10, 12 and 13.
Animals↗
Partial purification of a specific inhibitor of the insulin-like growth factors by reversed-phase high-performance liquid chromatography.
We report here preliminary data using reversed-phase high-performance liquid chromatography for the purification of a specific inhibitor (a molecular weight 16,000-18,000 protein) of the insulin-like growth factor (IGF) or somatomedin family. Crude inhibitor prepared from Cohn fraction IV-1 of human serum was first partially purified using an IGF/CH-Sepharose 4B affinity column. Following elution of the bound inhibitor and resuspension in 0.1% aqueous trifluoroacetic acid (mobile phase A), it was injected (100 microliter; 2.0 mg protein) onto a Brownlee Aquapore RP-300 column. Application of a linear gradient from 0% to 100% mobile phase B (45% isopropanol-0.1% trifluoroacetic acid) resulted in elution of two peaks of inhibitor activity between 31% and 34% isopropanol associated with a major homogeneous protein peak and a minor heterogeneous protein peak. No inhibitor was recovered when an acetonitrile gradient was used instead of isopropanol, indicating that the inhibitor is very hydrophobic. These data suggest that high-performance liquid chromatography offers a simple procedure for the potential purification of IGF inhibitor(s) from normal human serum.
Blood Proteins↗
The NMR-MOUSE: quality control of elastomers.
New applications of the NMR-MOUSE (mobile universal surface explorer) to non-destructive quality control of elastomers are reported. One example concern the thermal aging of fast clutches which was probed by measurements of 1H transverse relaxation time. Novel methodological developments show that 1H double-quantum filtered NMR signals can be generated in the inhomogeneous fields of the NMR-MOUSE for characterization of residual dipolar couplings. This technique was applied to characterize reference natural rubber samples with different crosslink density and carbon black and silica fillers.
Elastomers↗
Organic matter effects on phase partition of 1,3-dichloropropene in soil.
The fumigant 1,3-dichloropropene (1,3-D), in combination with chloropicrin, is considered a major replacement to methyl bromide (MeBr). This study was conducted to better understand phase partitioning of 1,3-D and the role of organic matter in its adsorption to soil. Partition of 1,3-D between air and water (K(H)), and between soil and water (K(f)), was determined by quantifying the concentration in both phases upon equilibrium. At 20 degrees C, the K(H) values of (Z)- and (E)-1,3-D were 0.052 and 0.033, respectively. In four California and Florida soils, the K(f) values of 1,3-D isomers ranged from 0.39 to 8.55, and the K(oc) values ranged from 18 to 60. The relatively high K(H) and low K(f) imply that 1,3-D is highly mobile in most soils after subsurface application. Adsorption of 1,3-D in native soils and soils amended with manure compost increased with increasing soil organic matter content. This suggests that organic wastes may be applied to soil to increase 1,3-D adsorption, thus reducing its potential for offsite movement.
Adsorption↗
Lemons into lemonade.
A booming economy can make layoffs in the biotechnology industry a blessing in disguise.
Biotechnology↗
Characterization of SU-8 for electrokinetic microfluidic applications.
The characterization of SU-8 microchannels for electrokinetic microfluidic applications is reported. The electroosmotic (EO) mobility in SU-8 microchannels was determined with respect to pH and ionic strength by the current monitoring method. Extensive electroosmotic flow (EOF), equal to that for glass microchannels, was observed at pH > or =4. The highest EO mobility was detected at pH > or =7 and was of the order of 5.8 x 10(-4) cm(2) V(-1) s(-1) in 10 mM phosphate buffer. At pH < or =3 the electroosmotic flow was shown to reverse towards the anode and to reach a magnitude of 1.8 x 10(-4) cm(2) V(-1) s(-1) in 10 mM phosphate buffer (pH 2). Also the zeta-potential on the SU-8 surface was determined, employing lithographically defined SU-8 microparticles for which a similar pH dependence was observed. SU-8 microchannels were shown to perform repeateably from day to day and no aging effects were observed in long-term use.
Journal Article↗
[The "other induction"--experiences and consequences in 281 deliveries following intravaginal administration of PGE2 tablets].
186 patients have been included prospectively in a study, aimed at analysing the course of birth after induction with 3 mg PGE2-tablets given intravaginally. These data are compared with those gained from a retrospective analysis of 95 patients using a dose of 2 mg. The total of the births within our clinic in 1986/87 functions as controls. Although in every case there has been an urgent need for the termination of pregnancy and there have been also unfavourable cervix findings in the 3 mg group, no differences could be observed in comparison to the control group concerning duration of cervical dilatation and expulsion, as well as foetal outcome parameters. When comparing the 2 mg and 3 mg groups, a certain superiority of the 3 mg dosage could be noted, leading to the opinion, that trial dosages of less than 3 mg should be abandoned. C-section rate was lowest and spontaneous birth rate was highest in the 3 mg group as compared to the 2 mg and the control groups. Permanent CTG-monitoring was not necessary. CTG-controls after 2 and 6 hours proved to be sufficient. Uterine hyperstimulation occurred in 2.1% of cases in both groups. In every case, prompt antagonization by means of high dose betamimetic therapy could be achieved. Due to reducing maternal and foetal side effects, the maximal mobility of the mother after tablet application, as well as, for the smooth congruence of cervical ripening and labour induction, the clinical use of the 3 mg tablet is a modern alternative to the classic oxytocin induction.
Administration, Intravaginal↗
Spontaneous nucleotide exchange in low molecular weight GTPases by fluorescently labeled gamma-phosphate-linked GTP analogs.
Regulated guanosine nucleotide exchange and hydrolysis constitute the fundamental activities of low molecular weight GTPases. We show that three guanosine 5'-triphosphate analogs with BODIPY fluorophores coupled via the gamma phosphate bind to the GTPases Cdc42, Rac1, RhoA, and Ras and displace guanosine 5'-diphosphate with high intrinsic exchange rates in the presence of Mg(2+) ions, thereby acting as synthetic, low molecular weight guanine nucleotide exchange factors. The accompanying large fluorescence enhancements (as high as 12-fold), caused by a reduction in guanine quenching of the environmentally sensitive BODIPY dye fluorescence on protein binding, allow for real-time monitoring of this spontaneous nucleotide exchange in the visible spectrum with high signal-to-noise ratios. Binding affinities increased with longer aliphatic linkers connecting the nucleotide and BODIPY fluorophore and were in the 10-100 nM range. Steady-state and time-resolved fluorescence spectroscopy showed an inverse relationship between linker length and fluorescence enhancement factors and differences in protein-bound fluorophore mobilities, providing optimization criteria for future applications of such compounds as efficient elicitors and reporters of nucleotide exchange. EDTA markedly enhanced nucleotide exchange, enabling rapid loading of GTPases with these probes. Differences in active site geometries, in the absence of Mg(2+), caused qualitatively different reporting of the bound state by the different analogs. The BODIPY analogs also prevented the interaction of Cdc42 with p21 activated kinase. Together, these results validate the use of these analogs as valuable tools for studying GTPase functions and for developing potent synthetic nucleotide exchange factors for this important class of signaling molecules.
Boron Compounds↗