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101.
Grancher D Jaussaud P Durix A Berthod A Fenet B Moulard Y Bonnaire Y Bony S 《Journal of chromatography. A》2004,1059(1-2):73-81
This paper describes a new method of purification of the Lolitrem B, a tremorgenic mycotoxin produced in planta by the endophytic fungus Neotyphodium lolii. The method is based on the large-scale isolation of the toxin by countercurrent chromatography (CCC). The lolitrem B content in endophyted ryegrass seed, 11 microg/g or 11 ppm, is extracted by stirring finely ground seeds with ethanol for 3 h at room temperature. The concentrated crude extract contains about 0.6 mg/g or 600 ppm of lolitrem B. It is then submitted to CCC purification with a biphasic four-solvent liquid system. A 160-fold enrichment was obtained in one step producing a raffinate containing 10% or 100 mg/g of the toxin. Further purifications were then performed by thin layer and low pressure liquid chromatography. Twenty-eight micrograms of lolitrem B with a 96% purity grade were obtained from 8 kg of seeds (yield 32%). 相似文献
102.
4-(4′-Dioctylaminocarbonylbiphenyloxy) phthalonitrile was synthesized from 4-(4′-carboxybiphenyloxy)phthalonitrile and dioctylamine
in the presence of Et3N. Metallophthalocyanines (Zn, Co and Cu) substituted with four dioctylaminocarbonyl biphenyloxy groups on the peripheral
positions were prepared from 4-(4′-dioctylaminocarbonylbiphenyloxy)phthalonitrile and the corresponding divalent metal salts
(Zn(CH3COO)2, CoCl2 and CuCl2). The new phthalocyanines are soluble in common organic solvents. These compounds were characterised by 1H-NMR, 13C-NMR, FT-IR, UV-Vis and mass spectroscopies. 相似文献
103.
Codée JD Litjens RE den Heeten R Overkleeft HS van Boom JH van der Marel GA 《Organic letters》2003,5(9):1519-1522
Diphenylsulfoxide in combination with triflic anhydride provides a very potent thiophilic glycosylation promotor system, capable of activating disarmed thioglycosides. The usefulness of this novel thiophilic activator is illustrated in a successful chemoselective glycosylation sequence in which the donor thioglycoside in the first condensation step may be either armed or disarmed. [reaction: see text] 相似文献
104.
The twelve tri-N-sulphonylhexahydro-1,3,5-triazines (R = alkyl or aryl) exhibit a common fragmentation pattern; most of the fragments are directly or indirectly generated from the [M ? RSO2]+ ion. Tri-N-Benzylsulphonylhexahydro-1,3,5-triazine (R = PhCH2) departs from the others mainly because the key ion [M ? RSO2]+ suffers a skeletal rearrangement with loss of SO2. The rationalizations presented are supported by metastable evidence, accurate mass measurements and deuterium labelling. 相似文献
105.
A new liquid chromatographic (LC)-chemometric approach was developed for the determination of sunset yellow (SUN) and tartrazine (TAR) in commercial preparations. This approach uses LC and chemometric calibration methods, i.e., classical least-squares (CLS), principal component regression (PCR), and partial-least squares (PLS), simultaneously. The combined LC-chemometric approaches, denoted as LC-CLS, LC-PCR, and LC-PLS, are based on photodiode array (PDA) detection at multiple wavelengths. Optimum chromatographic separation of SUN and TAR with allura red as the internal standard (IS) was obtained by using a Waters Symmetry C18 column, 5 microm, 4.6 x 250 mm, and 0.2 M acetate buffer (pH 5)-acetonitrile-methano-bidistilled water (55 + 20 + 15 + 10, v/v) as the mobile phase at a flow rate of 1.9 mL/min. The LC data sets consisting of the ratios of analyte peak areas to the IS peak area were obtained by using PDA detection at 5 wavelengths (465, 470, 475, 480, and 485 nm). LC-chemometric calibrations for SUN and TAR were separately constructed by using the relationship between the peak-area ratio and the training sets for each colorant. LC-chemometric approaches were tested for different synthetic mixtures containing SUN and TAR in the presence of the IS. These LC-chemometric calibrations were applied to a commercial preparation of the 2 colorants. The experimental results of the LC-chemometric approaches were compared with those obtained by a developed classical LC method using single-wavelength detection. 相似文献
106.
The processing and error analysis of signals in flow-injection systems were systematically studied by simulation and experimental measurements. The content includes an error analysis for peak-height and peak-area signal, a least-squares filtering procedure applied to the flow-injection curve and a peak recognition to remove interferences from air bubbles. Simulation results were obtained by statistical processing of peak-height and peak-area values from Gaussian curves to which noise had been added. The experimental measurements were done by an automatic flow-injection device to obtain detailed information for each individual point of a peak. 2-(2-Arsenophenylazo)-7-(2,6-dichlorophenylazo-4-sulphonic acid)-1,8-dihydroxynaphthalene-3,6-disulphonic acid (DCSA) was used for measuring physical dispersion alone, and Fe(II)-o-phenanthroline for the measurement of both physical dispersion and chemical reaction. The results from computer simulation and experiments agreed well. 相似文献
107.
108.
109.
Ivan Leban Boenna Golankiewicz Joanna Zeidler Gerald Giester Joe Kobe 《Acta Crystallographica. Section C, Structural Chemistry》2002,58(3):o133-o135
In the title compound, C13H13N5O4·H2O (4,5′‐cyclowyosine·H2O), the cyclization forces a syn arrangement of the aglycon with respect to the sugar moiety. The ribofuranose part of the molecule displays a β‐d configuration with an envelope C1′‐endo pucker. The molecules are arranged in columns along the short a axis and are linked to water molecules through O—H?O and O—H?N hydrogen bonds. 相似文献
110.
The 1,10-phenanthroline (phen) complexes of Co(II), Ni(II), Cu(II) and
Cd(II) orotates were synthesized and characterized by elemental analysis,
magnetic susceptibility, spectral methods (UV-vis and FTIR) and thermal analysis
techniques (TG, DTG and DTA). The Co(II), Ni(II), Cu(II) and Cd(II) ions in
diaquabis(1,10-phenanthroline)metal(II) diorotate octahedral complexes [M(H2O)2(phen)2](H2Or)2·nH2O
(M=Co(II), n=2.25; Ni(II), n=3;
Cu(II) and Cd(II), n=2) are coordinated
by two aqua ligands and two moles of phen molecules as chelating ligands through
their two nitrogen atoms. The monoanionic orotate behaves as a counter ion
in the complexes. On the basis of the first DTGmax,
the thermal stability of the hydrated complexes follows the order: Cd(II),
68°C 68°C 相似文献