Amino acids (AAs) are considered as the building blocks of life. Unlike nonessential AAs, the human body cannot synthesize essential AAs and should be supplied in food or dietary supplements. The aim of the work is simultaneous HPLC-UV determination of 10 structurally related AAs without pre- or postderivatization in powdered dietary supplements (PDSs). This was challenging, especially because PDS has no standardized procedures for its quality control. HPLC-UV chromatograms of the 10 AAs were recorded using a gradient elution of the mobile phase on a CLC-C18 column at 225 nm. The elution started with 100% of phosphate buffer (pH 7.4, 10 mM) for 10 min; then, the concentration of acetonitrile increased linearly to reach 50% for another 15 min at room temperature. Good separation was achieved within a 25 min run time without pre- or postderivatization. The method was carefully validated according to the ICH guidelines over the linearity range of 100-200, 50-200, 20-150, 50-400, 20-250, 75-175, 50-250, 50-250, 50-300, and 5-100 μg/mL for l-lysine, l-threonine, l-histidine, l-valine, l-methionine, l-isoleucine, l-leucine, l-tyrosine, l-phenylalanine, and l-tryptophan, respectively, with mean recoveries ranges between 98.91 and 100.77. The method was found to be precise, and the relative standard deviation (RSD) was found to be between 0.28 and 1.92 with recoveries between 97.91 and 101.11. The method was found to be robust that resists deliberate changes in pH, flow rate, and mobile-phase percentages. It was successfully applied for the analysis of PDSs. The proposed method could be very useful for the quality control of the 10 structurally related AAs during their synthesis and for testing raw materials and pharmaceutical preparations.

A simple, cheap, sensitive, and time-saving square wave voltammetric (SWV) procedure using a carbon paste electrode modified with aluminum oxide nanoparticle decorated multi-walled carbon nanoparticles (Al₂O₃-NPs/MWCNTs/CPE) is presented for the ultra-sensitive determination of tamsulosin (TAM) and solifenacin (SOL), one of the most prescribed pharmaceutical combinations in urology. Characterization of the developed electrode was performed using scanning electron microscopy (SEM), X-ray diffraction (XRD) patterns, energy dispersive X-ray analysis (EDX), transmission electron microscopy (TEM) and FT-IR spectrophotometry. The voltammetric behavior of TAM/SOL was evaluated using Al₂O₃-NPs in different content and electrode compositions. The use of Al₂O₃ functionalized MWCNTs as a CPE modifier increased the process of electron transfer as well as improved the electrode active surface area therefore, ultra-sensitive results were acquired with a linear range of 10–100 and 12–125 ng ml⁻¹ for TAM and SOL respectively, and a limit of the detection value of 2.69 and 3.25 ng ml⁻¹ for TAM and SOL, respectively. Interestingly, the proposed method succeeded in quantifying TAM and SOL with acceptable percentage recoveries in dosage forms having diverged concentration ranges and in the biological fluids with very low peak plasma concentration (C_max). Furthermore, the proposed method was validated, according to the ICH criteria, and shown to be accurate and reproducible.

Milk is one of the most important multicomponent superfoods owing to its rich macronutrient composition. It requires quality control at all the production stages from the farm to the finished products. A localized surface plasmon resonance optical sensor based on a citrate-capped silver nanoparticle (Cit-AgNP)–coated glass substrate was developed. The fabrication of such sensors involved a single-step synthesis of Cit-AgNPs followed by surface modification of glass slides to be coated with the nanoparticles. The scanning electron microscope micrographs demonstrated that the nanoparticles formed monolayer islands on glass slides. The developed surface-enhanced infrared absorption spectroscopy (SEIRA) sensor was coupled to artificial neural networking (ANN) for the qualitative differentiation between cow, camel, goat, buffalo, and infants’ formula powdered milk types. Moreover, it can be used for the quantitative determination of the main milk components such as fat, casein, urea, and lactose in each milk type. The qualitative results showed that the obtained FTIR spectra of cow and buffalo milk have high similarity, whereas camel milk resembled infant formula powdered milk. The most difference in FTIR characteristics was evidenced in the case of goat milk. The developed sensor adds several advantages over the traditional techniques of milk analysis using MilkoScan™ such as less generated waste, elimination of pre-treatment steps, minimal sample volume, low operation time, and on-site analysis. Graphical abstract