Home-made cider brandy (Calvados): analysis of distillation fractions by gas chromatography-mass spectrometry method

In this study, the distillation fractions of cider brandy produced illegally in Lithuania using gas chromatographic-mass spectrometry method were investigated. The conditions of gas chromatography-mass spectrometry were firstly optimized. A qualitative analysis of three distillation fractions was performed and estimated. The first fraction (initial) of distillation products was collected for 0.5 h, the second one (intermediate) was collected for the next 1.5 h and the third (main) fraction for the next 5 h. A method of the quantitative analysis of different volatile analytes such as acetaldehyde, methanol, ethanol, 1-propanol, isobutanol, 1-butanol, isoamyl alcohol and benzyl alcohol in the distillation products was also developed. The concentration of ethanol decreased significantly in the main fraction in comparison with those of the initial and intermediate fractions. The concentration of 1-propanol, isobutanol, 1-butanol and isoamyl alcohol in the last fraction decreased drastically as well.

Development and Validation of a Diethyl Phosphite Content in Foscarnet Sodium USP by GC MS Technique

A simple, rapid, selective, and reproducible Gas chromatographic mass spectrometry (GC-MS) method has been developed and validated for the estimation of Diethyl Phosphite content in Foscarnet Sodium USP Drug substance. The drugs were estimated using HP-5, Length-30 M, Internal diameter 0.32 mm; Film thickness 1 μ at a total flow rate of 11.9 ml/min, and column flow of 1.49 ml/min was used for the separation. Flow control mode was pressure. Column oven temperature 70°C and injector temperature 220°C. Oven program modified for proper elution of peak. The linearity range used was 0.025-0.120µg/ml and (Rt) was 6.7 min. The correlation coefficient values were found to be 0.997. Precession studies showed % RSD values less than 15.0% for all the selected concentrations. The percentage recovery of Diethyl phosphite from LOQ to 150% was found in range of 100.7 -116.7%. The content results of Phophite content were within the limits of less than 0.12 ppm. The method was validated as per the International Conference on Harmonization (ICH) guidelines. The developed method was successfully used for the quantitative analysis of commercially available dosage forms.

An efficient urine peptidomics workflow identifies chemically defined dietary gluten peptides from patients with celiac disease

Celiac disease (CeD) is a common autoimmune disorder induced by consuming gluten proteins found in wheat, barley, and rye. Glutens resist breakdown by gastrointestinal proteases, ultimately resulting in peptides with chemical structures that elicit inflammation in patients with CeD. Despite well-established connections between digestion-resistant glutens and CeD, chemically defined, bioavailable peptides produced from dietary proteins have never been identified from humans in an unbiased manner. This is largely attributable to technical challenges, which have impeded our knowledge of potentially diverse peptide species that encounter the immune system. Here, we developed a novel liquid chromatographic-mass spectrometric workflow for untargeted sequence analysis of the urinary peptidome. Using this protocol, we detected 679 distinct dietary peptides, of which ~35% have a CeD-relevant T cell epitope and 5% are known to stimulate innate immune responses. Remarkably, gluten peptides from patients with CeD qualitatively and quantitatively differed from control subjects. Our urinary peptidomic workflow provides new foundations for understanding gluten immunogenicity and enhancing CeD management. Additionally, it should promote new understandings of the uncharacterized dietary and urinary peptidomes.

New insights into the composition of historical remedies and pharmaceutical formulations: the identification of natural resins and balsams by gas chromatographic-mass spectrometric investigations

The present paper reports one of the first studies on the identification of natural resins and balsams in modern era drug formulations. Gas chromatography coupled with mass spectrometry (GC-MS) was applied to investigate the composition of ancient remedies and pharmaceutical formulations coming from the Spezieria di Santa Maria della Scala in Rome, founded at the end of the seventeenth century by the Discalced Carmelites. The obtained results highlight the presence of complex mixtures containing resinaceous and lipidic-based compounds. Thanks to the detection of characteristic markers, it was possible to identify several natural resins, such as guaiacum resin, ladano resin and scammony resin. Balsamic and aromatic compounds characteristic of essential oils were identified as well. In addition, an anti-inflammatory ointment, composed by mixing Venetian turpentine, a Pinaceae resin and a triterpene resin exudate of a plant from South America, was found among the analysed formulations. Combining the analytical results, the historical research and the botanical composition, it was possible to formulate compositional hypotheses of this historical medicine and provided some indications about their use in health. The study of historical drugs is not only important to know the practices handed down by apothecaries in the past, but also fundamental to reconstruct historical recipes that can inspire new dermatological, cosmetic, hygienic and current curative products.