Chemoselective Synthesis of β‐Amino Ester or β‐Lactam via Sonochemical Reformatsky Reaction

A series of β‐amino esters were synthesized by the reaction of N‐tosyl aldimine or N‐hydroxy aldimine with bromoacetate by sonochemical Reformatsky reaction. The β‐N‐hydroxyamino ester was obtained and the formed sensitive hydroxylamino functionality was resistant under the reaction condition. The β‐lactam also was synthesized by the reaction of N‐p‐methoxy aldimine as reacting substrate under this sonochemical Reformatsky reaction condition.     

Solvent‐Free Sonochemical Synthesis and Antifungal Activity of 1‐Alkyl‐3‐Methylimidazolium Bromide [RMIM]Br Ionic Liquids

In view of the continuous threat of opportunistic fungal infections to human health and the emerging importance of ionic liquids in therapeutic applications, we report the efficient one‐pot synthesis of a series of 1‐alkyl‐3‐methylimidazolium bromide [RMIM]Br ionic liquids through an ultrasound‐assisted reaction of 1‐methylimidazole and alkyl bromides (RBr) under solvent‐free conditions. High product yields were obtained for all syntheses (>95%) under mild conditions (2‐5 hours at 20‐40 °C). The success of the synthetic method was confirmed through ¹H‐NMR, ¹³C‐NMR and FT‐IR spectroscopy. All products exhibited activity against the fungus C. albicans with clotrimazole and water as positive and negative controls, respectively. At a concentration of 1%, [OMIM]Br IL exhibited an antimycotic activity with an index of 1.5 which is comparable to that of 1% clotrimazole having an antimicrobial index of 1.3, signifying the potential of the product as a fungal growth inhibitor. Structure‐Activity Relationship (SAR) studies showed that an increase in the alkyl chain length corresponds to an increase in the antifungal activity of the ionic liquids.     

Solid state and sonochemical syntheses of nano lead(II) chloride and bromide coordination polymers from its nitrate analog via mechanochemical crystal to crystal transformations

Reversible crystal-to-crystal transformations of 3D lead(II) coordination polymers with the ligand 2,5-bis(4-pyridyl)-3,4-diaza-2,4-hexadiene (4-bpdh), from nitrate analoge [Pb(4-bpdh)(NO₃)₂(H₂O)]_n (1) to [Pb(4-bpdh)(NO₃)(Br)]_n (2), [Pb(4-bpdh)(Br)₂]_n (3), [Pb(4-bpdh)(NO₃)(Cl)]_n (4) and [Pb(4-bpdh)(Cl)₂]_n (5) by solid state anion-replacement processes under mechanochemical reactions, have been studied. The reversible solid state structural transformations of compounds 1–5, by anion-replacement processes under mechanochemical reaction, have been verified by PXRD measurements. Nanoparticles of compounds were synthesized by sonochemical process and characterized by scanning electron microscopy (SEM), powder X-ray diffraction, IR spectroscopy and elemental analyses. The SEM images showed that morphology change occurs during solid state anion-replacements of nanocrystals.     

Alteration of volatile compounds profile of brewers’ spent grain by bath-ultrasonication and its combination with conventional water-bath and autoclave treatment

The study aimed to investigate the capability of bath-ultrasonication and its combination with conventional water-bath and autoclave treatment in modifying the volatile composition of brewers’ spent grain (BSG). It was hypothesized that the treatments modified the volatile composition of BSG due to the sonochemical modification. The results demonstrated that the treatments intensified the desirable odor and removed the undesirable one which might allow the possibility of masking and renewing the odor perception of BSG. Besides the influence on odor perception related compounds, it is worth to highlight that the treatments eliminated herbicidal compounds such as (E,E)-2,4-heptadienal and (E)-2-hexenal which might be present from herbicidal treatment. Combination of bath-ultrasonication with autoclave treatment modified the volatile aldehydes while its combination with conventional water-bath generated the same profile as it was in untreated BSG. Time elevation on bath-ultrasonication had no significant impact on the amount of ketones and alkanes, while the fluctuation occurred as an impact of thermal exposures. Moreover, the treatment reduced the amount of alcohol and increased the fatty acids. In conclusion, bath-ultrasonication and its combination with thermal exposure modified the volatile compositions of BSG.     

Sonochemical synthesis and fabrication of perovskite type calcium titanate interfacial nanostructure supported on graphene oxide sheets as a highly efficient electrocatalyst for electrochemical detection of chemotherapeutic drug

In green approaches for electrocatalyst synthesis, sonochemical methods play a powerful role in delivering the abundant surface areas and nano-crystalline properties that are advantageous to electrocatalytic detection. In this article, we proposed the sphere-like and perovskite type of bimetal oxides which are synthesized through an uncomplicated sonochemical procedure. As a yield, the novel calcium titanate (orthorhombic nature) nanoparticles (CaTiO₃ NPs) decorated graphene oxide sheets (GOS) were obtained through simple ultrasonic irradiation by a high-intensity ultrasonic probe (Titanium horn; 50 kHz and 60 W). The GOS/CaTiO₃ NC were characterized morphologically and chemically through the analytical methods (SEM, XRD, and EDS). Besides, as-prepared nanocomposites were modified on a GCE (glassy carbon electrode) and applied towards electrocatalytic and electrochemical sensing of chemotherapeutic drug flutamide (FD). Notably, FD is a crucial anticancer drug and also a non-steroidal anti-androgen chemical. Mainly, the designed and modified sensor has shown a wide linear range (0.015–1184 µM). A limit of detection was calculated as nanomolar level (5.7 nM) and sensitivity of the electrode is 1.073 μA μM⁻¹ cm⁻². The GOS/CaTiO₃ modified electrodes have been tested in human blood and urine samples towards anticancer drug detection.     

Ultrasonication and hydrothermal assisted synthesis of cloud-like zinc molybdate nanospheres for enhanced detection of flutamide

Ultrasonication is one of the emerging probes for nanoparticles synthesis as well as promoting the material property by treasuring the precious time during a chemical reaction. In this present work, we successfully designed a cloud-like α-ZnMoO₄ nanospheres (ZMNS) using ultrasound assistance (bath sonication with the power of 60 W and frequency of 37/80 kHz) hydrothermal method for catalyzing the effective electrochemical determination of anti-androgen drug candidate flutamide (FLT). The crystallinity and phase purity were investigated using powder X-ray diffractometric analysis. The FTIR and Raman spectra information were compared to detect the possible bonding in ZMNS. The texture and surface morphology were studied using Field emission scanning electron microscope and High-resolution Transmission electron microscope images. The presence of the elements (Zn, Mo and O) and the absence of any other impurities were monitored and confirmed using EDAX analysis. The fabrication of ZMNS modified GCE was performed carefully. Additionally, the ZMNS modified glassy carbon electrode (GCE) exhibits superior electrocatalytic activity by means of higher cathodic peak current towards the detection of FLT. The fashioned electrode attained two wide linear response ranges (0.1 to 73 µM; 111 to 1026 µM) with a lower detection limit of about 33 nM correspondingly. Furthermore, the fabricated sensor displayed excellent sensitivity of 1.095 µA µM⁻¹ cm⁻² and good selectivity for FLT sensing even in the existence of similar interfering compounds and biomolecules. Along with that, the designed sensor executed noticeable reproducibility, repeatability, and enduring stability.     

Single-step sonochemical synthesis of Cu2O-CeO2 nanocomposites with enhanced photocatalytic oxidative desulfurization

In this paper, for the first time, composite nanostructures of Cu₂O-CeO₂ were prepared by a facile and single-step sonochemical method for thiophene photocatalytic oxidative desulfurization. Sonication was performed utilizing a high-intensity ultrasonic probe with a maximum output power of 80 Wcm⁻³ and operating frequency at 20 kHz. The direct effect of ultrasonic waves on the composition and morphology of the obtained products was also evaluated and it was found that under ultrasonic irradiation, Cu₂O-CeO₂ can be produced while the main product in the absence of ultrasonic waves is CuO-CeO₂. Cu₂O-CeO₂ exhibits much higher photocatalytic efficiency (84%) than CuO-CeO₂ (39%) due to its higher light absorption and electron synergistic effect. The effect of Ce:Cu on photocatalytic efficiency was examined by considering the ratios of 1:0.25, 1:1, 0.5:1, and 0.25:1 and yields of 64, 81, 84, and 76% were obtained, respectively. This indicates that there is an optimal value for the Ce:Cu ratio in the Cu₂O-CeO₂ nanocomposite.     

Facile synthesis of copper ferrite nanoparticles with chitosan composite for high-performance electrochemical sensor

Herein, the synthesis of copper ferrite nanoparticles (CuFe₂O₄ NPs)/chitosan have been prepared by sonochemical route under ultrasonic irradiation bath at 40 kHz and 50 W. A high sensitive and stable modified electrochemical sensor was developed using a composition of copper ferrite nanoparticles coordinated with biopolymer through a facile ultrasound approach. Besides, power and frequency parameters are highly important for sonochemical synthesis and specifically structure, and size of the nanomaterials development during the ultrasonic irradiation time. In this work, ultrasonic bath was used to synthesis of CuFe₂O₄ nanomaterial at 40 kHz with 1 h. CuFe₂O₄/chitosan was characterized by FESEM, EDX, XRD and electrochemical methods. Furthermore, 8-hydroxyguanine is one of biomarker by oxidative stress. The concentrations of 8-hydroxyguanine within a cell are a measurement of oxidative stress in human body. Consequently, the measurement of 8-hydroxyguanine in blood serum samples with high specificity is of greatest importance. The CuFe₂O₄/chitosan modified electrode is displayed a low detection limit of 8.6 nM and long linear range (0.025–697.175 µM).     

Ultrasonic assisted fabrication of silver tungstate encrusted polypyrrole nanocomposite for effective photocatalytic and electrocatalytic applications

Ultrasonication is an emerging and evergreen technique for the efficient synthesis of the catalytically active heterostructured materials. In-situ one-pot ultrasonic-assisted synthesis method was demonstrated in this work for the fabrication of silver tungstate encrusted polypyrrole nanocomposite using semi-automatic ultrasonic probe maintained at 34°C/50 kHz ultrasonic frequency and at 150 W ultrasonic power. This material retains enhanced optical, electrical, morphological properties, photocatalytic behavior in photodegradation of congo red dye, tetracycline drug and its electrochemical sensing potential for the effective determination of a broad spectrum of antibacterial drug, nitrofurazone. Optical properties were investigated using UltraViolet–Visible diffuse reflectance spectral (UV–VIS DRS) data along with Tauc’s bandgap energy calculations. The morphological properties were examined using FESEM and TEM micrographs. All the PXRD and XPS details prove the effective distribution of PPy on the surface of Ag₂WO₄ rods with the help of powerful ultrasonic assistance. PPy acted as a support for nucleation and growth of Ag₂WO₄ and an inhibitor of phase transformations. Ag₂WO₄/PPy exhibits great photocatalytic behavior while comparing with pure PPy and Ag₂WO₄ in the degradation of carcinogenic dye congo red and antibiotic drug tetracycline. In addition to that, Ag₂WO₄/PPy modified GCE exposed a widespread linear range from 0.1 to 107 µM along with a very low detection limit of 12 nM and huge sensitivity of 1.74 µA µM⁻¹cm⁻² in the electrochemical determination of nitrofurazone.     

Sonochemical approach to the synthesis of metal tungstate/nafion composite with electrocatalytic properties and its electrochemical sensing performance

High-intensity ultrasound can be used to produce novel materials, offering an atypical pathway to recognized products without high bulk temperatures, high pressures, or long reaction times. A highly sensitive and selective robust modified sensor was developed using a composition of electrochemically active strontium metal (Sr) based tungstate interconnected with nafion polymer through a facile sonochemical approach. In addition, multiple parameters are important for sonochemical methods and specifically nanomaterial or electrocatalyst development during the ultrasonic irradiation. Moreover, high-intensity ultrasonic probe (Ti-horn) was used to synthesis of nanomaterial at 50 kHz and 200 W. The SrWO₄/nafion was characterized via FESEM, EDX and XRD methods. 8-HD-guanosine (8-hydroxydeoxyguanosine) is one of the major byproduct of deoxyribonucleic acid (DNA) oxidation. The concentrations of 8-HD-guanosine within a cell are a measurement of oxidative stress in body and however its excess level in body causes carcinogenic threats. Therefore, the quantification of 8-HD-guanosine in biological samples with high sensitivity is of great significance. The SrWO₄/nafion modified sensor displayed low detection of 14.36 nM and wide linear range (0.025–398.6 µM), compare to previous reports.