A newly developed interface coupling a CHN combustion device (elemental analyser 'EA') to an isotope ratio mass spectrometer is described and evaluated. The purpose of the device is to extend the dynamic range of delta(13)C and delta(15)N analysis from less than 2 orders of magnitude to more than 3 orders of magnitude. Carbon isotope ratio measurements of atropine as a model compound have been performed analysing between 1 μg to 5 mg C with acceptable to excellent precision (0.6 to 0.06 per thousand, delta-notation). The correction due to the blank signal is critical for sample amounts smaller than 4 μg C. The maximum sample weight is determined by the combustion capacity of the EA. Larger sample amounts are measured using dilution of a small part of the EA effluent with helium. The dilution mechanism works virtually free of isotope fractionation. Copyright 1999 John Wiley & Sons, Ltd. 相似文献
Characterization and quantitative analysis of oxidation plays an important role in biopharmaceutical development. This study demonstrates an approach to the assessment of susceptible to oxidation methionine residues in monoclonal antibodies and recombinant proteins. A method for the determination of oxidation levels by peptide mapping with mass spectrometric (MS) detection is described and its advantages compared to the UV detection are presented. Good linearity and reproducibility for determination of oxidation with MS detection are demonstrated (R2 > 0.99; RSDs of 4-9%). Aspects of method transfer to quality control group (QC) are discussed. As well, a quick and easy flow injection/MS method is proposed to substitute for peptide map analysis. Peptide coverage, linearity, reproducibility, robustness, sensitivity and quantitative oxidation results are compared for the flow injection/MS and LC/MS approaches. 相似文献
We propose two variants of tailored finite point (TFP) methods for discretizing two dimensional singular perturbed eigenvalue (SPE) problems. A continuation
method and an iterative method are exploited for solving discretized systems of equations to obtain the eigen-pairs of the SPE. We study the analytical solutions of two
special cases of the SPE, and provide an asymptotic analysis for the solutions. The
theoretical results are verified in the numerical experiments. The numerical results
demonstrate that the proposed schemes effectively resolve the delta function like of
the eigenfunctions on relatively coarse grid. 相似文献
In this paper we present error estimates for the finite element approximation of linear elastic equations in an unbounded domain. The finite element approximation is formulated on a bounded computational domain using a nonlocal approximate artificial boundary condition or a local one. In fact there are a family of nonlocal approximate boundary conditions with increasing accuracy (and computational cost) and a family of local ones for a given artificial boundary. Our error estimates show how the errors of the finite element approximations depend on the mesh size, the terms used in the approximate artificial boundary condition, and the location of the artificial boundary. A numerical example for Navier equations outside a circle in the plane is presented. Numerical results demonstrate the performance of our error estimates.
In this paper, we formulate interface problem and Neumann elliptic boundary value problem into a form of linear operator equations with self-adjoint positive definite op- erators. We prove that in the discrete level the condition number of these operators is independent of the mesh size. Therefore, given a prescribed error tolerance, the classical conjugate gradient algorithm converges within a fixed number of iterations. The main computation task at each iteration is to solve a Dirichlet Poisson boundary value problem in a rectangular domain, which can be furnished with fast Poisson solver. The overall computational complexity is essentially of linear scaling. 相似文献