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Extra virgin olive oil (EVOO) is well known for containing relevant amounts of healthy phenolic compounds. The European Food Safety Authority (EFSA) allowed a health claim for labelling olive oils containing a minimum amount of hydroxytyrosol (OHTyr) and its derivatives, including tyrosol (Tyr). Therefore, harmonized and standardized analytical protocols are required in support of an effective application of the health claim. Acid hydrolysis performed after extraction and before chromatographic analysis has been shown to be a feasible approach. Nevertheless, other fast, green, and easy methods could be useful for on-site screening and monitoring applications. In the present research, a natural deep eutectic solvent (NADES) composed of lactic acid and glucose was used to perform a liquid/liquid extraction on EVOO samples, followed by UV-spectrophotometric analysis. The spectral features of the extracts were related with the content of total OHTyr and Tyr, determined by the acid hydrolysis method. The second derivative of spectra allowed focusing on three single wavelengths (i.e., 299 nm, 290 nm, and 282 nm) significantly related with total OHTyr, total Tyr, and their sum, respectively. In particular, the sum of OHTyr and Tyr could be determined with a root mean square error of prediction of 29.5 mg kg−1, while the limits of quantitation and detection were respectively 11.8 and 4.9 mg kg−1. The proposed method, therefore, represents an easy screening tool, with the use of a green, food-derived solvent, and could be considered as an attempt to pave the way for food grade analytical chemistry.

Compounded therapeutic mAbs used in a hospital require quality control (QC). In our hospital, analytical QC process intended to mAbs identification and quantification is based on flow injection analysis associated with second-derivative UV spectroscopy and matching method algorithm. We studied the influence of degraded mAbs after compounding on this validated QC. Three forced stress conditions including mechanical, thermal, and freeze-thawing stresses were studied to yield degraded mAbs from 2 model compounds, that is, bevacizumab (IgG1) and nivolumab (IgG4). Different degraded mAbs were generated and were analyzed in terms of turbidity, the percentage of aggregation, size distribution, and changes in tertiary structure. Stresses showed to be mAb-dependent in terms of aggregation. Tertiary structural changes were observed in most of the stressed samples by principal component analysis of the UV second-derivative data. The structural and physicochemical modifications conducted to mismatch depending on the nature of the stress. The mismatch ranged from 17% to 72% for the mAbs, except for freeze-thawed bevacizumab for which a perfect match (100%) was reached. The quantification with an unfulfilled relative error of the concentration (i.e., > ±15%) was detected only for mechanically stressed mAbs. In conclusion, the study revealed that the influence of the mAbs and the type of stress impact on the QC of compounded mAbs. [ABSTRACT FROM AUTHOR]

Abstract The need for high-throughput quality control of pharmaceuticals after compounding is often required before the treatment of the patients. Ultra-fast analysis using flow injection analysis coupled to UV spectroscopy and least square matching was assessed for the simultaneous quantification and identification of three therapeutic taxanes after dilution in physiological saline (cabazitaxel, docetaxel, and paclitaxel). In-depth preliminary analysis of the zero and first order UV spectra of the taxanes using principal component analysis (PCA) allowed us focusing on relevant spectral range with very low formulation influence. Least square-matching algorithm available on basic HPLC software was applied to these spectra yielding very high match scores (>999) with significant difference ( P < 0.0001). The approach was qualitatively assessed through specificity and sensitivity which were excellent for the three taxanes (100%, n = 378), irrespective of their formulation. In terms of quantification, satisfactory linearity and accuracy were achieved for each of the taxanes according to their therapeutic range (0.05 to 1.02 mg·mL−1). The RSD (%) of the precision was satisfactory (<3%). Finally, the suitability of the approach for the taxanes QC has been demonstrated under routine application. Graphical abstract Unlabelled Image [ABSTRACT FROM AUTHOR]

• Five spectrophotometric methods for determination of masitinib were developed. • Derivative ratio method and log-A derivative method were used for identification. • Masitinib was determined in bulk and in pharmaceutical preparation. • Assessment of the masitinib stability in aqueous acidic solution was carried out. • UV spectra were used to extract both qualitative and quantitative information. Masitinib is an orally administered selective tyrosine kinase inhibitor. It has emerged as a promising drug for multiple diseases including cancer and inflammation in either human or veterinary medicine. Five new and simple UV spectrophotometric methods were developed for its determination in bulk and in pharmaceutical tablets. These methods are based on measuring the absorbance of masitinib in either zero order or first, second, third or fourth derivative spectra. Measurements are optimized so as to minimize excipients' interferences. The methods are suitable for micro-analysis of masitinib. The proposed methods were validated according to the ICH-Q2(R1) guidelines and was successfully applied for determination of masitinib in laboratory prepared tablet. The presented methods are simple, fast, cost‐effective and suitable for routine pharmaceutical analysis. Moreover, two derivative spectrophotometric-based methods were developed for identification of masitinib, the derivative ratio method and log-A derivative method. The impact of the developed methods on the environment was assessed by both analytical Eco-Sale and the Green Analytical Procedure Index (GAPI). The present work proves how derivative spectrophotometry could greatly extract qualitative and quantitative information from UV spectra. [ABSTRACT FROM AUTHOR]

Extra virgin olive oil (EVOO) is well known for containing relevant amounts of healthy phenolic compounds. The European Food Safety Authority (EFSA) allowed a health claim for labelling olive oils containing a minimum amount of hydroxytyrosol (OHTyr) and its derivatives, including tyrosol (Tyr). Therefore, harmonized and standardized analytical protocols are required in support of an effective application of the health claim. Acid hydrolysis performed after extraction and before chromatographic analysis has been shown to be a feasible approach. Nevertheless, other fast, green, and easy methods could be useful for on-site screening and monitoring applications. In the present research, a natural deep eutectic solvent (NADES) composed of lactic acid and glucose was used to perform a liquid/liquid extraction on EVOO samples, followed by UV-spectrophotometric analysis. The spectral features of the extracts were related with the content of total OHTyr and Tyr, determined by the acid hydrolysis method. The second derivative of spectra allowed focusing on three single wavelengths (i.e., 299 nm, 290 nm, and 282 nm) significantly related with total OHTyr, total Tyr, and their sum, respectively. In particular, the sum of OHTyr and Tyr could be determined with a root mean square error of prediction of 29.5 mg kg−1, while the limits of quantitation and detection were respectively 11.8 and 4.9 mg kg−1. The proposed method, therefore, represents an easy screening tool, with the use of a green, food-derived solvent, and could be considered as an attempt to pave the way for food grade analytical chemistry. [ABSTRACT FROM AUTHOR]