PubMed · 15999440
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2005. AAMI advice on reprocessing instructions.. https://pubmed.ncbi.nlm.nih.gov/15999440/
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The FDA process analytical technology (PAT) initiative will materialize in a significant increase in the number of installations of spectroscopic instrumentation. However, to attain the greatest benefit from the data generated, there is a need for calibration procedures that extract the maximum information content. For example, in fermentation processes, the interpretation of the resulting spectra is challenging as a consequence of the large number of wavelengths recorded, the underlying correlation structure that is evident between the wavelengths and the impact of the measurement environment. Approaches to the development of calibration models have been based on the application of partial least squares (PLS) either to the full spectral signature or to a subset of wavelengths. This paper presents a new approach to calibration modeling that combines a wavelength selection procedure, spectral window selection (SWS), where windows of wavelengths are automatically selected which are subsequently used as the basis of the calibration model. However, due to the non-uniqueness of the windows selected when the algorithm is executed repeatedly, multiple models are constructed and these are then combined using stacking thereby increasing the robustness of the final calibration model. The methodology is applied to data generated during the monitoring of broth concentrations in an industrial fermentation process from on-line near-infrared (NIR) and mid-infrared (MIR) spectrometers. It is shown that the proposed calibration modeling procedure outperforms traditional calibration procedures, as well as enabling the identification of the critical regions of the spectra with regard to the fermentation process.
The concentrations of the polymethoxylated flavones (PMFs) in peels of selected citrus cultivars grown in Jamaica and Mexico were determined. The PMFs were extracted from sun-dried citrus peels with reagent-grade methanol. Analyses were carried out by reverse-phase HPLC and UV detection. The column used was a C(18) 5 microm (150 x 4.6 mm) Discovery column. Elution was in the gradient mode, using a ternary mobile phase. The results showed that all the citrus cultivars used contained at least three of the six major PMFs quantified. Ortanique peel contained the highest quantity of PMFs (34,393 +/- 272 ppm), followed by tangerine (28,389 +/- 343 ppm) and Mexican sweet orange (sample 1; 21,627 +/- 494 ppm). The major PMFs, i.e. sinensetin, nobiletin, tangeretin, heptamethoxyflavone, tetramethylscutellarein and hexamethyl-o-quercetagetin, present in the peels of 20 citrus cultivars, was quantified. The results were compared with those of Florida citrus peels. A large amount of citrus peels and byproducts are produced in the Caribbean which could provide a cheap and convenient source of PMFs.
A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of camboginol in the extract of fruit rinds of Garcinia cambogia has been developed. Separation was achieved isocratically on an RP C(18) column using a solvent system consisting of a mixture of acetonitrile-water (9:1) and methanol-acetic acid (99.5:0.5) in the ratio of 30:70 as mobile phase at a flow rate of 0.4 mL/min. A multiple reaction monitoring (MRM) method was developed for quantification of camboginol in the fruit rinds extract of G. cambogia using MRM transitions of m/z 601.4 --> m/z 176.7 and m/z 601.4 --> m/z 448.9, respectively. The calibration curve based on peak area against concentration was linear up to 50 ng/mL with a detection limit of 0.5 ng/mL. The method showed satisfactory reproducibility with a coefficient of variation of less than 6%. The method was successfully applied for quantification of camboginol in different Garcinia extracts.