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11.
This paper describes the investigation of the potential of a quadrupole orthogonal acceleration time-of-flight mass spectrometer (Q-TOF) equipped with an atmospheric pressure ionisation interface for quantitative measurements of small molecules separated by reversed phase liquid chromatography. To this end, the detection limits and linear dynamic range in particular were studied in an LC/MS/MS experiment using 3,4-methylenedioxymethamphetamine standards and 3,4-methylenedioxyethylamphetamine for internal standardisation. In a second phase, the experiment was repeated with real biological extracts (whole blood, serum, and vitreous humour). A calibration for 3,4-methylenedioxymethamphetamine and its metabolite 3,4-methylenedioxyamphetamine was prepared in each of these matrices again using 3,4-methylenedioxyethylamphetamine as internal standard. The resulting quantitative data were compared with those obtained by liquid chromatography with fluorescence detection for the same extracts. The Q-TOF results revealed excellent sensitivity and a linear dynamic range of nearly four decades (2-10 000 pg on-column, r(2) = 0.9998, 1/x weighting). Furthermore, all the calibration curves prepared in biological material were superimposable, LC/MS/MS and LC-fluorescence, and the quantitative results for actual samples compared very favourably. It was concluded that the Q-TOF achieves a linear dynamic range for quantitative LC/MS/MS work exceeding that of fluorescence detection and at much better absolute sensitivity. Copyright 1999 John Wiley & Sons, Ltd.  相似文献   
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Poly‐(L ‐lysine citramide) is a degradable drug carrier of the polyelectrolyte type that is composed of citric acid and L ‐lysine building blocks. In a previous work, poly‐(L ‐lysine citramide) was synthesized by the interfacial polycondensation of α‐hydroxy acid protected citryl dichloride with COOH‐protected lysine diamine. Because of head‐to‐head and head‐to‐tail and tail‐to‐tail linkages in the chains as well as various side reactions such as deprotection of the α‐hydroxy acid moieties and intramolecular imide ring formation, a very large family of degradable polyelectrolyte copolymers was obtained. All the members of this family hydrolytically degrade to the same end products. In this study, another route was explored based on the polycondensation of α‐hydroxy acid protected citric acid pentafluorophenyl diesters, namely, citrobenzal dipentafluorophenyl and citrochloral dipentafluorophenyl with NN′‐trimethylsilylated COOH‐protected L ‐lysine. The resulting polymers were characterized by IR, NMR, and size exclusion chromatographic analyses. The resulting chain structures and repeat units were identified from these characterizations and are discussed as compared with characteristics exhibited by analogous polymers resulting from interfacial polycondensation. Differences observed at the intermediate stage involving protected polymers were largely erased during the final deprotection stage because of imide formation during final hydrolysis under the selected conditions. © 2001 John Wiley & Sons, Inc. J Polym Sci Part A: Polym Chem 39: 3475–3484, 2001  相似文献   
14.
By means of a noncommutative differential calculus on function space of discrete Abelian groups and that of the regular lattice with equal spacing as well as the discrete symplectic geometry and a kind of classical mechanical systems with separable Hamiltonian of the type H(p, q) = T(p) + V(q) on regular lattice, we introduce the discrete symplectic algorithm, i.e., the phase-space discrete counterpart of the symplectic algorithm including original symplectic schemes and the jet-symplectic schemes in terms of the discrete time jet bundle formalism, on the regular lattice. We show some numerical calculation examples and compare the results of different schemes.  相似文献   
15.
Nano-objects and thin films displaying molecular spin-crossover phenomena have recently attracted much attention. However, the investigation of spin crossover at reduced sizes is still a big challenge. Here we demonstrate that surface plasmon polariton waves propagating along the interface between a metal and a dielectric layer can be used to detect the spin-state changes in the latter with high sensitivity, even at the nanometer scale.  相似文献   
16.
Enhanced second-harmonic generation (SHG) conversion efficiency was theoretically predicted in waveguide geometry with coupling to a one-dimensional grating photonic band gap (PBG). We report a series of experiments using samples made with lithium niobate. A waveguide was fabricated near the surface by applying the proton-exchange technique. The characteristics of waveguide modes were determined by several techniques: prism coupling, diffraction, and Cherenkov radiation. The WKB method was used to analyze the results. Ultraviolet laser lithography was applied to make PBG gratings on the sample. We further investigated Cherenkov second-harmonic generation (CSHG), i.e., SHG radiated into the substrate, under the condition of a band-edge PBG resonance in the waveguides. The SHG inside planar waveguides was also experimentally investigated. We fabricated waveguides with multiple pump modes and found that the second mode was more efficient in enhancing the second harmonic signal. This result is explained by our model. Several samples were investigated in detail; the highest conversion efficiency of CSHG with a PBG was enhanced around 50 times above the CSHG signal without a PBG. A numerical model was constructed with parameters calculated from our sample characterization data to interpret the experimental results.  相似文献   
17.
Summary Thermal analysis has been used in foundry applications to assess the quality of the melt before casting. The high-end thermal analysis techniques such as DSC or DTA are expensive and not suitable for foundry applications. The Computer-Aided Cooling Curve Analysis (CA-CCA) method based on one thermocouple has been widely used as a batch process with poor control over heat extraction and cooling rates during solidification. A heat pipe apparatus has been developed as a thermal analysis tool. The apparatus can assess the melt quality more accurately, as well as, allow for better control of heating and cooling rates. Moreover, the solidification process can be modeled more accurately, and thus the casting parameters affecting the casting quality can be closely simulated and consequently controlled. In this paper the principles of a heat-pipe assisted thermal analysis system are highlighted. The advantages of the new system are described and the possibility of its adoption in melt assessments is discussed.  相似文献   
18.
The influence of electromagnetic actuators (EMAs) on the frequency response of a harmonically excited cantilever beam is investigated analytically, numerically and experimentally in this paper. Specifically, the intensity of the current generating the EMAs force is varied and its effect on the dynamic behavior of the system is analyzed. Analytical treatment based on perturbation analysis is performed on a simplified equation modeling the one mode vibration of the cantilever beam. Results indicated that EMAs produce a softening behavior in the system. Further, it is shown that as the current intensity of EMAs increases, the resonance curve shifts toward smaller values of frequency and the non-linear characteristic of the system becomes softer. The analytical predictions have been verified numerically and confirmed experimentally using a test rig.  相似文献   
19.
In this work, we describe a simple method of Abel inversion for temperature measurement in a natural convection axisymmetric flow. The essence of the method is that the measured lateral fringe shift profile is fitted with a polynomial with only even powers and then Abel inverse integral is evaluated analytically. This technique is compared with recent existing methods to test the accuracy and error propagation using a simulated interferogram of natural convection flow below a downward-facing heated horizontal disk in air. For this comparison, lateral fringe profiles are simulated using temperature fields computed by solving Navier Stokes and energy equations. Through random-number generation, noise profile is artificially added to the simulated noise-free lateral fringe shift profile. The results showed that the proposed technique for Abel inversion leads to accurate temperature profiles when the lateral fringe shift profile is fitted with even-power polynomials having degrees ranging from 20 to 30.  相似文献   
20.
This paper discusses the results of a study related to natural convection cooling of a heat source located on the bottom wall of an inclined isosceles triangular enclosure filled with a Cu water-nanofluid. The right and left walls of the enclosure are both maintained cold at constant equal temperatures, while the remaining parts of the bottom wall are insulated. The study has been carried out for a Rayleigh number in the range 104 ≤ Ra ≤ 106, for a heat source length in the range 0.2 ≤ ε ≤0.8, for a solid volume fraction in the range 0 ≤ ?≤0.06 and for an inclination angle in the range 0° ≤ δ≤45°. Results are presented in the form of streamline contours, isotherms, maximum temperature at the heat source surface and average Nusselt number. It is noticed that the addition of Cu nanoparticles enhances the heat transfer rate and therefore cooling effectiveness for all values of Rayleigh number, especially at low values of Ra. The effect of the inclination angle becomes more noticeable as one increases the value of Ra. For high Rayleigh numbers, a critical value for the inclination angle of δ = 15° is found for which the heat source maximum temperature is highest.  相似文献   
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