Wellsroach8257

The investigation of the possibility to determine various characteristics of powder heparin (n = 115) was carried out with infrared spectroscopy. The evaluation of heparin samples included several parameters such as purity grade, distributing company, animal source as well as heparin species (i.e. Na-heparin, Ca-heparin, and heparinoids). Multivariate analysis using principal component analysis (PCA), soft independent modelling of class analogy (SIMCA), and partial least squares - discriminant analysis (PLS-DA) were applied for the modelling of spectral data. Different pre-processing methods were applied to IR spectral data; multiplicative scatter correction (MSC) was chosen as the most relevant. Obtained results were confirmed by nuclear magnetic resonance (NMR) spectroscopy. Good predictive ability of this approach demonstrates the potential of IR spectroscopy and chemometrics for screening of heparin quality. This approach, however, is designed as a screening tool and is not considered as a replacement for either of the methods required by USP and FDA.The detection of the abuse of pseudo-endogenous steroids in sport is articulated in two different levels an initial testing procedure, based on the longitudinal evaluation of the urinary androgenic steroid profile by gas-chromatography mass spectrometry (GC-MSn), and a confirmation analysis, based on the differentiation between the endogenous and exogenous origin of the pseudo-endogenous steroids by gas-chromatography coupled to isotopic ratio mass spectrometry (GC/C/IRMS). The abuse of pharmaceutical preparations displaying a carbon isotopic composition values within a range similar to those reported for endogenous urinary steroids makes more difficult the application of GC/C/IRMS technique. To overcome this limitation, the direct detection of an intact synthetic anabolic steroid ester in blood matrices (plasma and/or serum) could supply the unequivocal proof of exogenous administration of pseudo-endogenous steroids. Here we are presenting a liquid chromatography tandem mass spectrometry (LC-MS/MS) method fo (0.25-10 ng/mL). The LODs are between 0.03 and 0.30 ng/mL, the extraction recovery higher than 70 % for all esters and no remarkable matrix effect, expressed in terms of ion enhancement and ion suppression, was observed. Finally, the developed and validate method was applied in the analysis of serum samples collected after the administration of a single dose (40 mg, 1 capsule) of testosterone undecanoate (Andriol ®) demonstrating its applicability.Pyrazinamide (PZA), Rifampicin (RIF), Isoniazid (ISH) and Ethambutol (ETB) form the core for the treatment of Tuberculosis, today a devastating disease in low-income populations around the world. These drugs are usually administrated by fixed-dose combination (FDC) products, to favour the patient compliance and prevent bacterial resistance. PZA exists in four enantiotropically-related polymorphs (Forms α, δ, β and γ), but only Form α is considered suitable for pharmaceutical products due to its stability and bioavailability properties. The classical approaches to address solid-state (microscopy, X-ray diffraction and calorimetry) shows limitations for quantification of polymorphs in the presence of excipients and other active components, as in the case of FDC tablets. In this work, an overall strategy was developed using near infrared spectroscopy (NIR) coupled to partial least squares regression (PLS) to quantify Form α of PZA in drug substance (raw material) and PZA/RIF/ISH-FDC tablets. For this purpose, twgy could be applied to a different stage of the process (i.e premixed-powders or granulates). The suitability of the method was also verified when Form α was satisfactorily analysed in FDC fortified with Form δ and Form γ to reach 0.78, 0.88 and 0.98 w/w, Form α. TAS-102 Thymidylate Synthase inhibitor This strategy results in an excellent alternative to ensure the polymorphic purity of PZA throughout the overall pharmaceutical manufacturing process.Recently, several peptides are used as active ingredients in topical cosmetic formulations, few information are available on their dermal stability against proteases. In this study, it was developed a simple and reliable assay to evaluate the stability of cosmeceutical peptides in skin homogenates. The quantification of studied peptides was performed by liquid chromatography coupled with a triple quadrupole mass spectrometer operating in tandem mass spectrometry mode (LC-MS/MS) and the conditions were tuned through energy resolved MS/MS (ERMS) experiments. The sample preparation procedure was carried out on rat skin homogenates by employing pal-KTTKS (reference peptide and the parameters that may affect the assay results were evaluated, including substrate concentration, dilution of skin homogenate, protein concentration and batch-to-batch variation of the homogenate. The optimized conditions were applied to check the degradation profile of pal-KTTKS in human skin samples and the obtained results were compared. Finally, the degradation profiles of SA1-III and pamSA1-III, recently described as cosmeceutical peptides, in human skin homogenate were evaluated. The results showed that proposed peptides are stable toward proteases for up to 8 h of incubation. Thanks to this characteristic, these peptides can be considered very interesting candidates as active ingredients for creams intended for a daily application.In order to facilitate correlation calculation and matrix-based resolution in comprehensive two-dimensional gas chromatography - mass spectrometry (GC × GC-MS) data-set, an intelligent clustering of modulation peaks (ICMP) algorithm was developed in this paper. ICMP is start with the second -dimension (2D) peak restriction, then conducting the peak shape restriction in the first dimension (1D), finally end with the eigenvalues calculation against mass spectra in moving sub-windows. After this three-tier restriction, multi-component spectral correlative chromatography (MSCC) was applied in peak clustering result from a row-wise augmented "two-dimension (2D) slice" set. Then the component similarities and differences were distinguished rapidly/ accurately in chemical fingerprints from ChaiHu Shugan San and Cyperus rotundus. Faced with co-eluted phenomenon, matrix-based resolution was made in the representative sub-matrices that have been locked in ICMP procedure. From the example data shows that ICMP- multivariate curve resolution (MCR) can served as a good complement to (non) trilinear decomposition.