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排序方式: 共有67条查询结果,搜索用时 15 毫秒
1.
A simple and highly selective method for the determination of piroxicam and pyridoxine (vitamin B6) in pharmaceutical formulations is presented. The approach is based on the combination of solid-phase extraction (SPE) and room-temperature fluorimetry (RTF). SPE under optimum pH conditions provides the separation between piroxicam and pyridoxine. The selectivity of analysis, the analytical figures of merit, and the accuracy of the method are demonstrated with the determination of piroxicam and pyridoxine in several pharmaceutical preparations. 相似文献
2.
Günther Snatzke Cristina Angeli Enio Decorte Flavio Moimas Biserka Koji-Prodi Ziva Ruzi-Toro Vitomir Sunji 《Helvetica chimica acta》1986,69(3):734-748
Hydrogenation of the ketone group in di-O-benzylderivative ( 8 ) of the known macrocyclic lactone zeralenone ( 7 ) using a novel chiral borane complex 3 . BH3, prepared in situ, proceeded at lower temperatures with moderate diastereoselectivity (~40%, d. e. at ?60°). Unsaturated diastereomers 9 and 10 were separated, and 9 converted into zeranol ( 11 ), a known anabolic agent. Restricted conformational mobility at lower temperatures is assumed for the intermediate 8 on the basis of the temperature-dependent CD spectra of its acetyl congeners 18 and 19 . X-Ray structure analysis of 7-O-acetylderivative ( 13 ) of 11 revealed the (R)-configuration at C(7). Two crystallographically independent H2O molecules are involved in the H-bonds, one of them (O(21)) rises the helices of the molecules of 13 along b. Small positive torsional angle [C(16)-]C(161)-C(1) [=O] (+19.3°), transoid(E) conformation of the lactone group, and nearly achiral arrangement of the C(11)-C(12) bond (torsional angle [C(11)-]C(12)-C(121)[C(161)] is ?93°) are the main conformational features that differentiate the macrocylic RAL (resorcinic-acid lactone) derivatives from the 6-membered lactone derivative 20 , studied earlier by CD. Consequently, the rules developed for the CD effects within conjugation band (around 270 nm), and n→π* band (around 255 nm) of the latter compound, cannot be applied the macrocyclic lactones. 相似文献
3.
Solid-surface room-temperature phosphorimetry (SSRTP) is proposed as an alternative detection technique for the liquid chromatographic determination of caffeine, theophylline and theobromine. The measurements are performed in a continuous mode with a two-nebulizer automated system for SSRTP detection. The analytical figures of merit obtained with the proposed detector are compared with those obtained by UV absorption detection. The SSRTP and UV chromatograms of spiked urine samples are compared, and the possibility of keeping the SSRTP substrates as permanent records of analyzed samples is discussed. 相似文献
4.
Eduardo Sommella Giacomo Pepe Francesco Pagano Gian Carlo Tenore Paola Dugo Michele Manfra Pietro Campiglia 《Journal of separation science》2013,36(20):3351-3355
We have developed a fast ultra HPLC with ion‐trap TOF‐MS method for the analysis of flavonoids in Citrus bergamia juice. With respect to the typical methods for the analysis of these matrices based on conventional HPLC techniques, a tenfold faster separation was attained. The use of a core–shell particle column ensured high resolution within the fast analysis time of only 5 min. Unambiguous determination of flavonoid identity was obtained by the employment of a hybrid ion‐trap TOF mass spectrometer with high mass accuracy (average error 1.69 ppm). The system showed good retention time and peak area repeatability, with maximum RSD% values of 0.36 and 3.86, respectively, as well as good linearity (R2 ≥ 0.99). Our results show that ultra HPLC can be a useful tool for ultra fast qualitative/quantitative analysis of flavonoid compounds in citrus fruit juices. 相似文献
5.
Hernández FE Yu S García M Campiglia AD 《The journal of physical chemistry. B》2005,109(19):9499-9504
We present for the first time experimental evidence of fluorescence lifetime enhancement of organic chromophores attached to metal nanospheres via radiative decay engineering. The hybrid system (HS) was a modified "diconjugated" molecular probe, 4-acetamido-4'-maleimidylstilbene-2,2'-dithiol (AMDT), covalently bound to the surface of 5-nm-diameter Au nanospheres by its two sulfur atoms, at a distance d < 1 nm and with its molecular axis parallel to the surface of the nanoparticle surface. We measured a fluorescence lifetime increase of a factor of 2 at room temperature (tau(AMDT) = (4.32 +/- 0.10) ns and tau(HS) = (8.73 +/- 0.23) ns) and a factor of 3.4 at 4.2 K (tau(AMDT) = (2.64 +/- 0.07) ns and tau(HS) = (7.96 +/- 0.14) ns). We also found that the fluorescence quantum yield of this hybrid system is not reduced, proof of a weak energy transfer between the molecular probe and the nanoparticle. These results demonstrate that a molecular dipole oriented parallel to the metal surface tends to be reduced by the coupling with its image. 相似文献
6.
This article presents the first application of gold nanoparticles deposited capillaries as pre-concentration devices for in-capillary microextraction CZE and their use for the analysis of monohydroxy-polycyclic aromatic hydrocarbons in synthetic urine samples. The successful separation of 1-hydroxypyrene, 9-hydroxyphenanthrene, 3-hydroxybenzo[a]pyrene (3-OHbap), 4-hydroxybenzo[a]pyrene and 5-hydroxybenzo[a]pyrene under a single set of electrophoretic conditions is demonstrated as well as the feasibility to obtain competitive ultraviolet absorption LOD with commercial instrumentation. Enrichment factors ranging from 87 (9-OHphe) to 100 (3-OHbap) made it possible to obtain LOD ranging from 9 ng/mL (9-OHphe and 3-OHbap) to 14 ng/mL (4-hydroxybenzo[a]pyrene). 相似文献
7.
Monitoring of high-molecular weight polycyclic aromatic hydrocarbons (HMW-PAH) via simple and cost effective methods still remains a challenge. In this article, we combine solid-phase nano-extraction (SPNE) and 4.2 K laser-excited time resolved Shpol'skii spectroscopy (LETRSS) into a valuable alternative for the water analysis of dibenzo[a,l]pyrene, dibenzo[a,h]pyrene, dibenzo[a,i]pyrene and naphtho[2,3-a]pyrene. In comparison to the original SPNE procedure, the present method improves PAH recoveries and reduces extraction time from 30 to 20 min per sample. Quantitative release of HMW-PAH into the Shpol'skii matrix (n-octane) is best accomplished with a mixture of 48 μL of methanol and 2 μL of 1-pentanethiol. Their migration into the 50 μL layer of n-octane provides highly resolved spectra with distinct fluorescence lifetimes for unambiguous isomer determination. Complete analysis takes less than 30 min per sample and consumes only 100 micro-liters of organic solvents. 500 μL of water are sufficient to obtain limits of detection ranging from 16 ng L(-1) (dibenzo[a,l]pyrene) to 55 ng L(-1) (dibenzo[a,i]pyrene), relative standard deviations better than 3% and analytical recoveries above 90%. Although a straightforward comparison to chromatographic methods is not possible because of the lack of analytical figures of merit on HMW-PAH, the excellent precision of measurements, limits of detection and overall recoveries makes SPNE-LETRSS an attractive approach to water analysis of HMW-PAH. 相似文献
8.
Let $G$ be a locally finite group which contains a non-cyclic subgroup $V$ of order four such that $C_{G}\left( V\right) $ is finite and $C_{G}\left( \phi \right)$ has finite exponent for some $\phi \in V$ . We show that $[G,\phi ]^{\prime }$ has finite exponent. This enables us to deduce that $G$ has a normal series $1\le G_1\le G_2\le G_3\le G$ such that $G_1$ and $G/G_2$ have finite exponents while $G_2/G_1$ is abelian. Moreover $G_3$ is hyperabelian and has finite index in $G$ . 相似文献
9.
Sabrina Castellano Marisabella Santoriello Pietro Campiglia Giovanna Cardillo Alessia Bertamino Isabel Gomez-Monterrey Ettore Novellino Gianluca Sbardella 《Tetrahedron letters》2009,50(49):6869-6871
An inexpensive and regioselective approach to dihydrothieno[3,2-g]quinoline-4,9-dione is reported. A combination of a mild version of Skraup reaction with a sequential substitution/Michael addition allowed the selective preparation in acceptable yield of a pharmacologically important quinone derivative, previously obtained only in trace and together with the other regioisomer. 相似文献
10.
Hussein Hijazi Thomas Langlinay Hermann Rothard Philippe Boduch Frédéric Ropars Amine Cassimi Lucio S. Farenzena Enio F. da Silveira 《The European Physical Journal D - Atomic, Molecular, Optical and Plasma Physics》2014,68(7):1-6
Electronic sputtering of lithium fluoride by swift heavy ions was studied as a function of electronic energy loss (dE/dx) e . The single crystal targets were irradiated with swift heavy ion beams (166Z P 692; 46E P /M P (MeV/u) 611). This allowed varying the deposited energy by a factor of 20 (1.86dE/dx (keV/nm) 632). The sputtered secondary ions were measured from well controlled LiF targets without surface contaminations, by means of the time-of-flight technique (TOF-SIMS). The mass spectrum reveals an important contribution of clusters (over single ions), which increases with (dE/dx) e . Another observation for the strongest perturbation at high dE/dx (>8 keV/nm) is that the secondary ion yields saturate: Y(dE/dx) = constant. In contrast, at lower dE/dx (<8 keV/nm) for weaker perturbation, the yield Y scales with (dE/dx)2. This quadratic increase would rather point towards a thermal evaporation-like mechanism leading to electronic sputtering, however, the origin of the yield saturation remains an open finding. 相似文献