The Development and Application of Novel IR and NMR-Based Model for the Evaluation of Carminative Effect of Artemisia judaica L. Essential Oil

Artemisia judaica L. is a medicinal plant that is traditionally used to relieve abdominal pains through its carminative activity. In this study, spectroscopic analysis was employed to investigate the carminative activity associated with A. judaica. Using infrared spectroscopy, the carminative activity was evaluated based on the first derivative of IR-characteristic stretching signal of CO2. Our results indicate that A. judaica oil effectively reduced the response of CO2 signal equivalent to thymol standard. Additionally, 1H-NMR spectroscopy was utilized to assess surface activity of A. judaica crude oil through the reduction of interfacial tension in a D2O/CDCl3 system. Apparently, 10 mg of the oil was able to solubilize water in a chloroform layer up to 4.3% (w/w). In order to correlate the observed surface activity of the oil to its actual composition, GC-MS and GC-FID structural analysis were undertaken. The results revealed that the oil composition consists of oxygenated terpenes which might be responsible for the carminative effect. Furthermore, owing to its sensitivity, our model provides a fundamental basis for the pharmacological assessment of trace amounts of oils with high precision and accuracy

Comparison of different water-miscible solvents for the preparation of plasma and urine samples in metabolic profiling studies

The Lowry method and a capillary electrophoresis method were used to analyse protein residues in the supernatant after solvent deproteination of plasma. Acetonitrile and acetone were much more effective than methanol and ethanol at reducing the levels of proteins in plasma. The ability of different solvents to decrease levels of phospholipids in plasma samples was assessed using electrospray ionisation mass spectrometry (MS). Phospholipid signals can obscure differences between samples in general metabolite profiling (i.e. non-target compound) studies. Acetonitrile was much more effective than methanol in reducing the MS signal due to phospholipids in plasma which is a consequence of the poor solubility of phospholipids in acetonitrile. The capability of the solvents at reducing salts in urine samples was also studied by using an amperometric method. Using this approach little difference was detected between methanol, ethanol, acetonitrile and acetone in their ability to desalt urine samples

Response to drug treatment in newly diagnosed epilepsy: a pilot study of 1H NMR- and MS-based metabonomic analysis

Understanding the biological basis of drug resistance and developing techniques which facilitate prediction of outcome have the potential to revolutionise the pharmacotherapy of epilepsy.We have performed a pilot study of metabonomic analysis using nuclear magnetic resonance(NMR) spectroscopy and mass spectrometry (MS) in an effort to identify metabolic biomarkers of response to antiepileptic drug treatment. Pretreatment serum samples were obtained from 125 patients with newly diagnosed epilepsy who were taking part in a randomized monotherapy trial. Outcome (responder, nonresponder) was assessed at 6 weeks, 6 months, and 12 months after starting treatment. Serum samples were subject to investigation by both NMR and MS and the resulting data interrogated by principal component analysis. There was no clear distinction in the metabolic profile, acquired by either NMR or MS, of responders and nonresponders to AED treatment at any of the three clinical end points investigated, suggesting that pretreatment serum samples do not contain any prominent biomarkers of responsiveness to initial treatment in new-onset epilepsy. Metabonomic analysis is undoubtedly applicable to the search for biological predictors of response to drug treatment in epilepsy, but future studies should employ larger patient cohorts, more discriminatory analyses, and a less equivocal clinical phenotype

Stability determination for cyclized 2,4-dinitrophenyl hydrazone derivative of glucose

Abstract Background The most well established tactic for the analysis of monosaccharaides, such as glucose, relies on derivatization procedures, using reagents as 2,4-dinitrophenylhydrazine (DNPH). Usually, the instability of the formed imine product deteriorates the detection of trace amounts of the sugar; rendering the spectrophotometric analysis of monosaccharaides extremely challenging. Methods In this study, we propose a modified derivatization procedure, reliant on the formation of a stable DNPH-glucose derivative, to aid in the spectrophotometric analysis of glucose. The derivatization procedure was customized to perform the product work-up step under acidic conditions. Results The proton rich media resulted in direct reduction of the Schiff’s base with concomitant intramolecular rearrangement of the product to yield a stable cyclized DNPH-glucose derivative. The annealed structure of the titled compound was verified by 1NMR, 13C-NMR, HMBC and X-ray crystallography. Conclusions The derivative revealed extended stability in spiked plasma samples which suggests a potential to employ the described procedure for glucose analysis and detection in biological samples

7-(3-Chlorophenylamino)-1-cyclopropyl-6-fluoro-8-nitro-4-oxo-1,4-dihydroquinoline-3-carboxylic Acid

7-(3-Chlorophenylamino)-1-cyclopropyl-6-fluoro-8-nitro-4-oxo-1,4-dihydro-quinoline-3-carboxylic acid (2) was prepared and fully characterized by NMR, IR, and MS. Compound 2 exhibited good antibacterial activity against gram-positive standard and resistant strains