Radiohochspannungsionophoretische untersuchungen der isotopenaustauschreaktionen zwischen polythionaten und sulfit

The isotopic exchange of sulfur-35 between trithionate/sulfit and tetrathionate/pentathionate is examined. High voltage paper ionophoresis is applied for the separation of the reaction mixture. The amount of activity of the reaction products is determined at different times. This enables to calculate the kinetical data of those exchange systems.      

Cyclodextrin Derivatives in GC Separation of Racemic Mixtures of Volatiles. Part XIV: Some Applications of Thick-Film Wide-Bore Columns to Enantiomer GC Micropreparation

Representative examples of preparative GC isolation of pure enantiomers in amounts ranging from 0.5 to 2 mg, with thick-film wide-bore open tubular columns coated with cyclodextrin (CD) diluted in polysiloxanes, are described. Two 25 m×0.53 mm i.d. columns, coated with 3 μm of 30% 2,6-di-O-methyl-3-O-pentyl-β-CD/OV-1701 and 2 μm of 30% 2,3-di-O-acetyl-6-O-tert- butyldimethylsilyl-β-CD/PS-086 as stationary phases, were used. Methyl 3-hydroxyhexanoate, methyl 2-methylbutanoate, δ-hexalactone, δ-octalactone, and γ-decalactone (the latter from a nature-identical mango aroma), were submitted to automated micropreparative GC. Average yields of about 30% were achieved when amounts above 20 μg/μl were injected, and an enantiomeric purity above 90% was obtained.     

Full-field Thermal Deformation Measurements in a Scanning Electron Microscope by 2D Digital Image Correlation

Using recently developed methods for application of a nano-scale random pattern having high contrast during SEM imaging, baseline full-field thermal deformation experiments have been performed successfully in an FEI Quanta SEM using 2D-DIC methods. Employing a specially redesigned commercial heating plate and control system, with modified specimen attachment procedures to minimize unwanted image motions, recently developed distortion correction procedures were shown to be effective in removing both drift and spatial distortion fields under thermal heating. 2D-DIC results from heating experiments up to 125°C on an aluminum specimen indicate that (a) the fully corrected displacement components have nearly random variability and a standard deviation of 0.02 pixels (≈25 nm at 200× and ≈0.5 nm at 10,000×) in each displacement component and (b) the unbiased measured strain fields have a standard deviation ≈150 × 10⁻⁶ and a mean value that is in good agreement with independent measurements, confirming that the SEM-DIC based method can be used for both micro-scale and nano-scale thermal strain measurements.

2H/1H Ratio Analysis of Flavor Compounds by On‐Line Gas Chromatography Pyrolysis Isotope Ratio Mass Spectrometry (HRGC‐P‐IRMS): Benzaldehyde

Isotope ratio monitoring gas chromatography‐mass spectrometry of the ²H/¹H ratio by pyrolysis isotope ratio mass spectrometry (P‐IRMS) was used to analyze benzaldehyde originating from various sources. Based on the δ²H_SMOW value of an authentic reference sample determined with an elemental analyzer (EA), the range of reproducibility and linearity was checked. Correct (EA related) and reproducible data were obtained for sample amounts >0.6 μg benzaldehyde (on column). In another series of experiments, the influence of sample preparation, i. e. simultaneous distillation‐extraction (SDE) was found to be negligible. The following ranges of δ²H_SMOW values were determined for benzaldehyde using five types of samples, i. e. (i) synthetic (δ²H_SMOW –78 to –85‰, ex benzal chloride; +420 to +668‰, ex toluene) and ‘natural’ (including ‘ex‐cassia’) references (δ²H_SMOW –83 to –144‰); (ii) bitter almond oils (δ²H_SMOW –113 to –148‰); (iii) fruits (δ²H_SMOW –111 to –146‰); (iv) kernels (δ²H_SMOW –115 to –188‰); and (v) leaves (δ²H_SMOW –165 to –189‰).     

A Bioorthogonal Chemical Reporter of Viral Infection

Pathogen‐selective labeling was achieved by using the novel gemcitabine metabolite analogue 2′‐deoxy‐2′,2′‐difluoro‐5‐ethynyluridine (dF‐EdU) and click chemistry. Cells infected with Herpes Simplex Virus‐1 (HSV‐1), but not uninfected cells, exhibit nuclear staining upon the addition of dF‐EdU and a fluorescent azide. The incorporation of the dF‐EdU into DNA depends on its phosphorylation by a herpes virus thymidine kinase (TK). Crystallographic analyses revealed how dF‐EdU is well accommodated in the active site of HSV‐1 TK, but steric clashes prevent dF‐EdU from binding human TK. These results provide the first example of pathogen‐enzyme‐dependent incorporation and labeling of bioorthogonal functional groups in human cells.