PubMed · 11146869
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R Wilkinson, E A Poppe, K Leidig, K Schirmer. 2000. Moulding problems: feed system too small.. https://pubmed.ncbi.nlm.nih.gov/11146869/
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NIR transflectance spectroscopy was used to determine polarimetric parameters (direct polarization, polarization after inversion, specific rotation in dry matter, and polarization due to nonmonosaccharides) and sucrose in honey. In total, 156 honey samples were collected during 1992 (45 samples), 1995 (56 samples), and 1996 (55 samples). Samples were analyzed by NIR spectroscopy and polarimetric methods. Calibration (118 samples) and validation (38 samples) sets were made up; honeys from the three years were included in both sets. Calibrations were performed by modified partial least-squares regression and scatter correction by standard normal variation and detrend methods. For direct polarization, polarization after inversion, specific rotation in dry matter, and polarization due to nonmonosaccharides, good statistics (bias, SEV, and R(2)) were obtained for the validation set, and no statistically (p = 0.05) significant differences were found between instrumental and polarimetric methods for these parameters. Statistical data for sucrose were not as good as those of the other parameters. Therefore, NIR spectroscopy is not an effective method for quantitative analysis of sucrose in these honey samples. However, NIR spectroscopy may be an acceptable method for semiquantitative evaluation of sucrose for honeys, such as those in our study, containing up to 3% of sucrose. Further work is necessary to validate the uncertainty at higher levels.
A highly hydrophilic poly(7-oxonorbornene-5,6-dicarboxylic acid-block-norbornene) [=poly-(ONDCA-b-NBE)]-coated silica was investigated for the liquid chromatographic (LC) determination of flavonoids in plant extracts of complex biological origin using UV absorbance and mass spectrometric (MS) detection. Compared to the most commonly used octadecyl derivatized silica this sorbent allowed fast separations even at extreme pH values. Furthermore, UV absorbance and MS detection were evaluated. As we found, UV detection at 254 nm allows the determination of flavonoids down to the ng range with a linearity of R2>0.9906. For the more selective characterization the validated LC system was coupled to a quadrupole ion trap mass spectrometer via an electrospray ionization (ESI) interface. MS detection showed high linearity (R2>0.9904) for all investigated flavonoids. Due to the relatively high flow-rate of 1 ml/min the limits of detection were found in the lower-microg range. Collision induced dissociation was applied to obtain characteristic fragmentation fingerprints. Finally, the validated LC-ESI-MS-MS method demonstrated that this poly-(ONDCA-b-NBE) stationary phase allows fast characterization and quantitation in onion, elderflower blossom, lime blossom, St. John's Wort and red wine.
A sensitive and simple method for the simultaneous determination of nutritionally important minerals in food samples is in great demand. Ion chromatography coupled with UV-vis detection is shown to be an appropriate technique for this objective. The method is based on the formation of mineral complexes by pyridine-2,6-dicarboxylic acid in the mobile phase. The complexes are then postcolumn derivatized with 4-(2-pyridylazo)resorcinol (PAR), resulting in mineral-PAR complexes that are detected by UV-vis absorption at 500 nm. This facilitates the simultaneous separation and quantification of minerals in one chromatographic run. Within 16 min, Cu, Ni, Zn, Co, Mn, and Fe are analyzed. When a 50 microL injection volume is used, the average detection limit is 5 ppb in the injection liquid. The detection limit makes it a superior alternative to AAS and, in several applications, also an alternative to ICP-MS techniques. Different sample treatments were evaluated. The concentration of acid in the treated sample varied with the sample treatment, which may cause a limitation for the injection volume. A crucial prerequisite to achieve the reported detection limits and to obtain reliable results is to completely exclude all contamination from instruments and materials.