Determination of caffeine in tea samples by Fourier transform infrared spectrometry

A sustainable and environmentally friendly procedure has been developed for the FTIR determination of caffeine in tea leaf samples. The method is based on the extraction with ammonia and CHCl3 and direct determination of caffeine on the chloroform extracts using peak height absorbance measurements at 1658.5 cm(-1) and external calibration. The method provides a sensitivity of 0.2142 absorbance units mg(-1) mL and a limit of detection of 1 mg L(-1), corresponding to 0.002% m/m caffeine in tea leaves. As compared with a reference procedure, based on UV absorbance measurement at 276 nm after low pressure column chromatography, the developed procedure reduces the consume of CHCl3 by a factor of 10, that of NH4OH by a factor of 20 and avoids the use of diethyl ether and Celite. The time required to do the analysis of a sample is 15 minutes as compared with the 6 hours for the reference one.     

Eisen(III)-Aluminium-Mischhydroxide und deren katalytisches Verhalten

Zusammenfassung Es wurden mechanische Gemenge sowie Gemeinschaftsfällungen von röntgenamorphen Eisen(III)-hydroxid und Aluminiumoxidhydrat untersucht, die sich röntgenographisch nicht, wohl aber in ihrem katalytischen Vorhalten voneinander unterscheiden.     

Bestimmung von Palladium mit Diphenylglyoxim

Ohne Zusammenfassung     

Unterschiede im katalytischen Verhalten geometrisch isomerer Verbindungen

Ohne Zusammenfassung     

Crystal and molecular structure of the (−)-N-hydroxyimide of (10-pinene-2-yl) succinimic acid

Two independent molecules in the unit cell are the same enantiomer of the title compound but possess slightly different conformations. Both conformers are joined by H-bonds to one water molecule. The configuration at C11 was established asR.Crystal data: C₁₄H₁₉O₃N×1/2H₂O; trigonal,P3₂;a=17.486(2),b=17.486(2),c=8.024(1)Å;V=2124.72(6)ų;Z=6; (CuK)=1.54178 Å;F(000)=834; finalR=0.0495 for 2376 reflections (of 2747 unique data).     

In situ isobaric lipid mapping by MALDI–ion mobility separation–mass spectrometry imaging

The highly diverse chemical structures of lipids make their analysis directly from biological tissue sections extremely challenging. Here, we report the in situ mapping and identification of lipids in a freshwater crustacean Gammarus fossarum using matrix‐assisted laser desorption/ionization (MALDI) mass spectrometry imaging (MSI) in combination with an additional separation dimension using ion mobility spectrometry (IMS). The high‐resolution trapped ion mobility spectrometry (TIMS) allowed efficient separation of isobaric/isomeric lipids showing distinct spatial distributions. The structures of the lipids were further characterized by MS/MS analysis. It is demonstrated that MALDI MSI with mobility separation is a powerful tool for distinguishing and localizing isobaric/isomeric lipids.     

Tracing the Photoaddition of Pharmaceutical Psoralens to DNA

The psoralens 8-methoxypsoralen (8-MOP), 4,5′,8-trimethylpsoralen (TMP) and 5-methoxypsoralen (5-MOP) find clinical application in PUVA (psoralen + UVA) therapy. PUVA treats skin diseases like psoriasis and atopic eczema. Psoralens target the DNA of cells. Upon photo-excitation psoralens bind to the DNA base thymine. This photo-binding was studied using steady-state UV/Vis and IR spectroscopy as well as nanosecond transient UV/Vis absorption. The experiments show that the photo-addition of 8-MOP and TMP involve the psoralen triplet state and a biradical intermediate. 5-MOP forms a structurally different photo-product. Its formation could not be traced by the present spectroscopic technique.     

Towards Reliable and Quantitative Surface‐Enhanced Raman Scattering (SERS): From Key Parameters to Good Analytical Practice

Experimental results obtained in different laboratories world‐wide by researchers using surface‐enhanced Raman scattering (SERS) can differ significantly. We, an international team of scientists with long‐standing expertise in SERS, address this issue from our perspective by presenting considerations on reliable and quantitative SERS. The central idea of this joint effort is to highlight key parameters and pitfalls that are often encountered in the literature. To that end, we provide here a series of recommendations on: a) the characterization of solid and colloidal SERS substrates by correlative electron and optical microscopy and spectroscopy, b) on the determination of the SERS enhancement factor (EF), including suitable Raman reporter/probe molecules, and finally on c) good analytical practice. We hope that both newcomers and specialists will benefit from these recommendations to increase the inter‐laboratory comparability of experimental SERS results and further establish SERS as an analytical tool.     

Selective bond breaking in beta-D-ribose by gas-phase electron attachment around 8 eV

Electron attachment experiments are carried out on the beta-d-ribose molecule in the gas phase for the energy region around 8 eV, and clear fragmentation products are observed for different mass values. A computational analysis of the relevant dynamics is also carried out for the beta-d-ribose in both the furanosic and pyranosic form as gaseous targets around that energy range. The quantum scattering attributes obtained from the calculations reveal in both systems the presence of transient negative ions (TNIs). An analysis of the spatial features of the excess resonant electron, together with the computation and characterization of the target molecular normal modes, suggests possible break-up pathways of the initial, metastable molecular species.