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  • 1
    Keywords: PROTEINS ; VELOCITY ; AGGREGATION ; BIOPHARMACEUTICALS ; FLUORESCENCE-DETECTED SEDIMENTATION ; SIZE-EXCLUSION CHROMATOGRAPHY ; FIELD-FLOW FRACTIONATION ; SPINCO ULTRACENTRIFUGE ; BEAD MODELS ; HYDRODYNAMICS
    Abstract: Analytical ultracentrifugation (AUC) is a first principles based method to determine absolute sedimentation coefficients and buoyant molar masses of macromolecules and their complexes, reporting on their size and shape in free solution. The purpose of this multi-laboratory study was to establish the precision and accuracy of basic data dimensions in AUC and validate previously proposed calibration techniques. Three kits of AUC cell assemblies containing radial and temperature calibration tools and a bovine serum albumin (BSA) reference sample were shared among 67 laboratories, generating 129 comprehensive data sets. These allowed for an assessment of many parameters of instrument performance, including accuracy of the reported scan time after the start of centrifugation, the accuracy of the temperature calibration, and the accuracy of the radial magnification. The range of sedimentation coefficients obtained for BSA monomer in different instruments and using different optical systems was from 3.655 S to 4.949 S, with a mean and standard deviation of (4.304 +/- 0.188) S (4.4%). After the combined application of correction factors derived from the external calibration references for elapsed time, scan velocity, temperature, and radial magnification, the range of s-values was reduced 7-fold with a mean of 4.325 S and a 6-fold reduced standard deviation of +/- 0.030 S (0.7%). In addition, the large data set provided an opportunity to determine the instrument-to-instrument variation of the absolute radial positions reported in the scan files, the precision of photometric or refractometric signal magnitudes, and the precision of the calculated apparent molar mass of BSA monomer and the fraction of BSA dimers. These results highlight the necessity and effectiveness of independent calibration of basic AUC data dimensions for reliable quantitative studies.
    Type of Publication: Journal article published
    PubMed ID: 25997164
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  • 2
    Electronic Resource
    Electronic Resource
    Copenhagen : International Union of Crystallography (IUCr)
    Acta crystallographica 57 (2001), S. o663-o665 
    ISSN: 1600-5368
    Source: Crystallography Journals Online : IUCR Backfile Archive 1948-2001
    Topics: Chemistry and Pharmacology , Geosciences , Physics
    Notes: The title compound, C10H10N2·C4H8N2O2, consists of hydrogen-bonded 2,3-dimethylquinoxaline and dimethylglyoxime molecules. Both dimethylglyoximes are located on an inversion centre and there are two half-molecules in the asymmetric unit. The dimethylglyoxime molecules are linked about inversion centres to the 2,3-dimethylquinoxaline moiety by O—H...N hydrogen bonds (O...N 2.898 and 2.805 Å) to form polymeric chains.
    Type of Medium: Electronic Resource
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