Josephson voltage standard at National Physical Laboratory,New Delhi

A C Josephson effect is now used by several countries as the reference standard for the unit of d.c. voltage. This paper describes the work done at the National Physical Laboratory (NPL), New Delhi in the realization of the unit of volt based on the a.c Josephson effect. A voltage standard at 1 mV level using a Nb-Nb point contact junction has been established and the as-maintained volt based on a bank of standard cells has been intercompared against it using a 1:1000 voltage divider. The experimental set-up used in this comparison and the results of recent measurements are described. The overall uncertainty in assigning the value of emf to a standard cell is about 1 ppm. The as-maintained volt has been found to agree with the Josephson voltage within overall uncertainty.     

Minor alkaloids of Tylophora asthmatica: Revised structure of tylophorinidine

The structure of the phenolic alkaloid tylophorinidine, isolated from Tylophora asthmatica, has been shown to be 2. Two other minor alkaloids isolated from the plant have been shown to be d-septicine (11) and d-isotylocrebrine (14).     

Crystal and molecular structure of sarcosine

The crystal structure of sarcosine in pure form has been determined at low temperature (135 K). The crystals are othorhombic, space group P2(1)2(1)2(1) with unit cell dimensions a = 6.687(2) A, b = 7.899(3) A, c = 8.607(3) A. On the basis of 988 reflections with intensities larger than 3 sigma (I) the structure was refined to a conventional R-factor of 0.034 to give e.s.d. in bond lengths of 0.002 A and 0.2 degrees in angles. The molecule is extended and exists in the zwitterionic form. There is a small deviation from planarity in the alpha-amino acid group as well as in the main chain.     

Direct in situ observation of increasing structural dimensionality during the hydrothermal formation of open-framework zinc phosphates

The first time-resolved in situ X-ray diffraction studies of the hydrothermal crystallisation of open-framework zinc phosphates reveal a pathway of sequential crystallisation involving formation of a metastable low dimensional chain phase before the growth of three-dimensional zeolitic architectures.     

The role of temperature on the structure and dimensionality of MOFs: an illustrative study of the formation of manganese oxy-bis(benzoate) structures

Three new manganese oxy-bis(benzoate) compounds, synthesized by increasing the reaction temperature, with increasing dimensionality and decreasing Mn-Mn distances, indicate a possible pathway through an entropy driven dehydration route.     

Self-assembly of fluorescent inclusion complexes in competitive media including the interior of living cells

Anthracene-containing tetralactam macrocycles are prepared and found to have an extremely high affinity for squaraine dyes in chloroform (log Ka = 5.2). Simply mixing the two components produces highly fluorescent, near-infrared inclusion complexes in quantitative yield. An X-ray crystal structure shows the expected hydrogen bonding between the squaraine oxygens and the macrocycle amide NH residues, and a high degree of cofacial aromatic stacking. The kinetics and thermodynamics of the assembly process are very sensitive to small structural changes in the binding partners. For example, a macrocycle containing two isophthalamide units associates with the squaraine dye in chloroform 400,000 times faster than an analogous macrocycle containing two 2,6-dicarboxamidopyridine units. Squaraine encapsulation also occurs in highly competitive media such as mixed aqueous/organic solutions, vesicle membranes, and the organelles within living cells. The highly fluorescent inclusion complexes possess emergent properties; that is, as compared to the building blocks, the complexes have improved chemical stabilities, red-shifted absorption/emission maxima, and different cell localization propensities. These are useful properties for new classes of near-infrared fluorescent imaging probes.     

A Series of Collaborations between Various Pharmaceutical Companies and Regulatory Authorities Concerning the Analysis of Biomolecules Using Capillary Electrophoresis: Additional Instruments/Buffer

An international project team (including members from US, Canada and UK) was formed from a number of interested biopharmaceutical companies and regulatory authorities to conduct a cross-organisation collaboration exercise. The results of the first comparison with eight different organisations that used instruments of the same equipment model, the same reagents, and the same methodology has been reported previously [1]. This report represents the addition of other instruments using a different run buffer. The relative migration times were different, as expected, prohibiting a direct comparison between companies. The within-organisation variability was low for both relative migration time (<0.34% RSD% for all companies save one) and the peak area (<5% RSD% for all companies save one) when measuring the purity of a representative IgG sample. The apparent molecular weight of bovine serum albumin was measured with good precision (less than 10% RSD% across all companies) to the theoretical value when all data is utilized (67.5 kDa compared to 66.4 kDa). For a representative IgG sample, the three main components, IgG Light Chain, IgG Non-glycosylated Heavy Chain, and IgG Heavy Chain, could not be separated, specifically the IgG Non-glycosylated Heavy Chain and IgG Heavy Chain. When the IgG Non-glycosylated Heavy Chain and IgG Heavy Chain were combined for all organisations, the fractional peak area for the IgG Light Chain and IgG Non-glycosylated Heavy Chain + IgG Heavy Chain peak also showed excellent agreement, with less than 7.5 and 3.5% RSD%, respectively. The value of this exercise is in demonstrating the reliability of CE for the determination of apparent size of biopharmaceutical proteins. This underpins the appropriate use of such CE data in support of regulatory submissions.