Analytical tools for urocanic acid determination in human samples: A review

Urocanic acid is a chromophore found in the skin that has been identified as an important immunosuppressant and carcinogenesis mediator through its photoisomerization from trans to cis form induced by ultraviolet radiation. Research on analytical methods that explore urocanic acid isomerization is indispensable to fully understand the deleterious effects mediated by this biomarker. In this context, the current relevant analytical methods for determination of these isomers in human samples are summarized in this review. The methods presented here are applicable to human samples collected by noninvasive methods (or minimally invasive), encompassing an array of analytical techniques, including high‐performance capillary electrophoresis, confocal Raman spectroscopy, gas chromatography, high‐performance liquid chromatography, and mass spectrometry, among others. Developed high‐performance liquid chromatography methods have proven to be advantageous, allowing noninvasive collections for in vivo analysis and the confocal Raman, specially, for real‐time analysis. Among all these methods, high‐performance liquid chromatography is the most investigated one with mass spectrometry or ultraviolet detector, and the mass spectrometry detector being the most studied in the last years, demonstrating high sensitivity, very low detection limits, and accurate identification, especially for clinical investigations.     

Development and Validation of a Stability-Indicating LC Method for the Determination of Rupatadine in Pharmaceutical Formulations

A reversed-phase liquid chromatography (RP-LC) method was validated for the determination of rupatadine in pharmaceutical dosage forms. The LC method was carried out on a Gemini C₁₈ column (150 mm × 4.6 mm I.D.), maintained at 30 °C. The mobile phase consisted of ammonium acetate buffer (pH 3.0; 0.01 M) with 0.05% of 1-heptanesulfonic acid–acetonitrile (71.5:28.5, v/v), run at a flow rate of 1.0 mL min⁻¹ and using photodiode array (PDA) detection at 242 nm. The chromatographic separation was obtained with retention time of 5.15 min, and was linear in the range of 0.5–400 μg mL⁻¹ (r ² = 0.9999). The specificity and stability-indicating capability of the method was proven through the degradation studies and showing also, that there was no interference of the excipients. The accuracy was 100.39% with bias lower than 0.58%. The limits of detection and quantitation were 0.01 and 0.5 μg mL⁻¹, respectively. Moreover, method validation demonstrated acceptable results for precision, sensitivity and robustness. The proposed method was applied for the analysis of pharmaceutical dosage forms assuring the therapeutic efficacy.

     

Development and Validation of a Stability-Indicating LC Method for Determination of Ebastine in Tablet and Syrup

A simple stability-indicating reversed-phase liquid chromatographic method with diode-array detection was developed and validated for the quantitative determination of ebastine in tablets and syrup. The LC method was carried out on a C₁₈ column with acetonitrile:phosphoric acid 0.1% pH 3.0 (55:45, v/v) as mobile phase, at a flow rate of 1.2 mL min⁻¹. Ultraviolet detection of ebastine was at 254 nm. A linear response (r = 0.9999) was observed in the range of 10–80 μg mL⁻¹. The RSD values for intra- and inter-day precision studies showed good results (RSD < 2%) and accuracy was greater than 98%. Validation parameters such as specificity and robustness were also determined. The method was found to be stability-indicating and can be applied to quantitative determination of ebastine in tablets and syrup.

     

Numerical simulation of the vertical flow in a gas-solid system based on nuclear techniques

The conservation equations for particulate systems were utilized to investigate the fluid-dynamic behavior of a gas-solid mixture flowing along a vertical tube (riser) in a simplified model of a pilot catalytic cracking unit. Nuclear techniques were utilized for the determination of the flow parameters along the riser. The results show a satisfactory agreement between the theoretical data and those obtained by experimental tests.     

Characterization of Collagen from Three Genetic Lines (Gray,Red and F1) of Oreochromis niloticus (Tilapia) Skin in Young and Old Adults

From tilapia (Oreochromis niloticus) farming, the by-products have been identified as a source of collagen that could be used for the development of dermocosmetics or pharmaceutical products. However, the characteristics of collagen related to a specific strain or culture must be well defined prior to its application. Collagen was extracted from the skin of three strains of tilapia: red YY males (YY: two Y-type sex chromosomes), XX gray females, and the F1: offspring of crossing red YY males with XX gray females; at different ages in the adult phase, using acetic acid and pepsin enzyme. The characteristics of acid-soluble collagen (ASC) and pepsin-soluble collagen (PSC) were shown by SDS-PAGE band profiles to be similar to bovine collagen type I (SIGMA), the PSC of gray tilapia being more fragile to temperature changes, consistent with the results of fractional viscosity. The characteristics of the F1 progeny were prioritized for being a commercially productive and sustainable source for the extraction of collagen, and the ASC form, being the one with the greatest stability and advantage over PSC, of importance to our investigations, leads to a controlled digestion as in the case of peptide induction, and also in the development of natural products in the pharmaceutical and/or dermocosmetic industry. Evaluations of the triple helix structure by FT-IR, X-ray diffraction and UV–visible spectroscopy give similar results between the strains: red, gray, and F1, and between ages in the adult form F1 (15, 24, and 36 months of age). Consequently, the skin of tilapia in adult form is recommended sustainably for up to 24 months of age where the collagen is obtained with the use of acetic acid without enzymatic treatment.     

A New Electrochemical Sensor Based on Carbon Black Modified With Palladium Nanoparticles for Direct Determination of 17α-Ethinylestradiol in Real Samples

Electrochemical sensors to quantify concentrations of emerging pollutants have attracted great attention from the industry and scientific community. Nanomaterials such as carbon black have been applied in sensors to identify substances that are toxic to the environment and human health due to their excellent electroanalytical properties. The aim of the study was to develop a novel electrochemical sensor for the endocrine disruptor hormone determination. To our knowledge, for the first time the synthesis of material based on carbon black containing immobilized palladium nanoparticles, with the application for the hormone ethinylestradiol, is reported in the literature. The material was synthesized, characterized, and applied to the determination in tap water and human urine of the synthetic hormone 17α-ethinylestradiol (EE2), which is currently considered an emerging pollutant. The morphology, structure and electrochemical performance of the sensors were characterized by scanning electron microscopy (SEM) and cyclic voltammetry (CV). Differential pulse voltammetry (DPV) in sodium phosphate buffer solution at pH 5.0 allowed the generation of a method to quantify the concentration of 17α-ethinylestradiol in a linear range of 0.5–119.0 μmol L⁻¹, obtaining 81.0 nmol L⁻¹ of calculated limit of detection (LOD). The system was efficient in detecting 17α-ethinylestradiol in real urine samples and showed no interferences for ascorbic acid, uric acid, progesterone, and dopamine. It is noteworthy that the results obtained showed good recovery values, considering that the urine samples were not previously treated or pre-concentrated, which suggests the development of an electrochemical sensor that works in situ and in real time to monitor relevant substances in the control clinical and environmental, with the possibility of point-of-care analyses.     

Development and Validation of a Stability-Indicating LC Method for Determination of Ebastine in Tablet and Syrup

A simple stability-indicating reversed-phase liquid chromatographic method with diode-array detection was developed and validated for the quantitative determination of ebastine in tablets and syrup. The LC method was carried out on a C₁₈ column with acetonitrile:phosphoric acid 0.1% pH 3.0 (55:45, v/v) as mobile phase, at a flow rate of 1.2 mL min⁻¹. Ultraviolet detection of ebastine was at 254 nm. A linear response (r = 0.9999) was observed in the range of 10–80 μg mL⁻¹. The RSD values for intra- and inter-day precision studies showed good results (RSD < 2%) and accuracy was greater than 98%. Validation parameters such as specificity and robustness were also determined. The method was found to be stability-indicating and can be applied to quantitative determination of ebastine in tablets and syrup.