A simple and efficient high-performance liquid chromatographic method was developed and validated for the separation and determination of capsaicin and its major dihydro- and homoderivatives in spice paprika products in 20 min with fluorescent and 35 min with mass-spectrometric detection. The separation was performed on reversed-phase chromatographic adsorbent of cross-linked endcapping with eluent consisting of 1:1 acetonitrile-water or acetonitrile-0.1% formic acid under isocratic conditions. Excellent separation of all the major and minor capsaicinoids with resolution index between 1.08 and 7.34 was achieved. The detection and quantification limits of capsaicinoids in standard material solutions were between 2 and 10 ng/mL. The lowest detectable amount of capsaicin, with fluorescent detection, was found to be <1 µg/g non-pungent spice paprika powder. The naturally occurring capsaicinoids could be distinguished from the non-capsaicinoids compounds appeared on liquid chromatography-fluorescence profile of extract from drastically processed paprika by applying mass spectroscopic detection. Hungarian spice paprika were evaluated as mild to very hot (capsaicinoid content: 334-1,660 µg/g) and chili products as very or extremely hot products (1,543-2,818 µg/g).
Remediation of areas contaminated by potentially toxic elements (PTE) requires the appropriate assessment of the environmental mobility of contaminants. The fractionation techniques developed for agrochemical and environmental purposes model the pathways of environmental mobilization mainly by sequential extraction procedures. In Europe mostly the simplified extraction scheme proposed by Community Bureau of Reference (BCR) in 1993 is widely used, why only to this certified sediment sample (BCR 701) is available, certified for fractionation of six elements (Cu, Cd, Cr, Ni, Pb, Zn). In the BCR extracts the reagentsolvents applied in leaching steps cause strong matrix interferences when for determination the PTE-contents of these solutions the multielemental capacity of inductively coupled plasma optical emission spectrometry (ICP-OES) should be utilized. Due to the different source of contamination the flexible multi-elemental ICP-OES method should be applied for analysis of the different BCR-extractant-solvent media which makes possible the reliable detection of all occurring PTE in the area. For this purpose as the most adequate solution the application of ICP-OES spectrometer with charge-coupled device (CCD)-detection was selected which is able to record the entire spectral range between 120-800 nm. On the basis of detailed study of BCR-solvent-matrix-and expected-analite-line interferences it was established that the sensitivities of the prominent lines of pollutant elements strongly depend on the type of extractants. For improving the accuracy of analytical results obtained for soils and environmental sediments, matrix matched calibration, internal standardization and robust plasma conditions were recommended and optimized. The successful application of this methodology is presented for a PTE-contamited lake sediment sample and for selected typical Hungarian soil samples stored in sample bank of Hungarian Soil Protection Information and Monitoring System.
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