Phenolic-compound-extraction systems for fruit and vegetable samples.

This paper reviews the phenolic-compound-extraction systems used to analyse fruit and vegetable samples over the last 10 years. Phenolic compounds are naturally occurring antioxidants, usually found in fruits and vegetables. Sample preparation for analytical studies is necessary to determine the polyphenolic composition in these matrices. The most widely used extraction system is liquid-liquid extraction (LLE), which is an inexpensive method since it involves the use of organic solvents, but it requires long extraction times, giving rise to possible extract degradation. Likewise, solid-phase extraction (SPE) can be used in liquid samples. Modern techniques, which have been replacing conventional ones, include: supercritical fluid extraction (SFE), pressurized liquid extraction (PLE), microwave-assisted extraction (MAE) and ultrasound-assisted extraction (UAE). These alternative techniques reduce considerably the use of solvents and accelerate the extraction process.

Potential of RP-UHPLC-DAD-MS for the qualitative and quantitative analysis of sofosbuvir in film coated tablets and profiling degradants.

Sofosbuvir is one of the new direct-acting antiviral drugs against hepatitis C virus (HCV) infection. This drug has recently been launched into the market, and generic versions of the medication are expected to be produced by local drug producers in some countries. Therefore, new methods are required to control sofosbuvir in pharmaceuticals. In the present study, a new method based on reversed phase (RP)-ultra-high performance liquid chromatography (UHPLC) coupled to diode array detection (DAD) and mass spectrometry (MS) was developed to facilitate the qualitative and quantitative analysis of sofosbuvir in film coated tablets. A wavelength of 260 nm was selected to perform a cost-effective quantification and the method showed adequate linearity, with an R2 value of 0.9998, and acceptable values of accuracy (75%-102%) and precision (residual standard deviation <5%). The detection and quantification limits were 0.07 µg/mL and 0.36 µg/mL, respectively. Furthermore, the use of high-resolution MS enabled us to ensure the specificity, check impurities and better sensitivity. Therefore, this methodology promises to be suitable not only for the routine analysis of sofosbuvir in pharmaceutical dosage forms, but also for potential degradants.

Identification of active compounds in vegetal extracts based on correlation between activity and HPLC-MS data.

We propose a method identifying candidates for active compounds in vegetal extracts. From a collection of samples, the method requires, for each sample, a HPLC-MS analysis and a measurement of the activity. By applying a correlation analysis between the activity and the chromatographic area for each interval of elution time and m/z ratio, the peaks corresponding to candidates for active compounds can be identified. Additionally, when peaks are identified, a model can be estimated to predict the activity in new samples. Both methods are evaluated in one experiment involving the phenolic extract (PE) from 22 samples of extra virgin olive oil (EVOO) where the activity is a cytotoxicity index against JIMT-1 breast cancer cells. In this experiment, the samples were separated into two disjunct partitions: one was used for training (identification of candidates and estimation of prediction model), while the other was used for validation (by comparing the predicted and the measured activities). Three compounds were identified as candidates to be responsible for the cytotoxicity of the EVOO-PE against JIMT-1 cells. The prediction model provided an accurate estimation of the activity.

Correlation between the antibacterial activity and the composition of extracts derived from various Spanish Cistus species.

Cistaceae is a large family of shrubs commonly distributed in the Mediterranean ecosystem. The aim of this study was to explore the potential antimicrobial properties against Escherichia coli and/or Staphylococcus aureus of different extracts obtained from four Cistaceae species that are especially abundant in Spanish semi-arid regions. MIC50 values of the extracts of C. salviifolius exhibited potent bacteriostatic effects against S. aureus compared with the other Cistus species tested. Spray-drying had less impact on the antimicrobial activities and polyphenolic contents than did evaporation followed by freeze-drying. When C. salviifolius extract was concentrated and the polar fraction was removed, its bacteriostatic and bactericidal activities against both strains were significantly enhanced. Seasonal influences on the composition have also been found. Up to 48 compounds were found in the aqueous extract of C. salviifolius using RRLC-ESI-TOF-MS. The analysis of the composition of the extracts revealed that the inhibitory activity against E. coli may be related to the presence of galloylated flavanols and specific flavonols, whereas the inhibitory capacity against S. aureus may be related primarily to polar compounds and to other flavonols. Potential synergistic effects among polyphenols may deserve further studies. These extracts may serve as an alternative source of antimicrobial ingredients focused on medical devices or cosmetics.