Efficient Removal of Hexavalent Chromium (Cr(VI)) from Wastewater Using Amide-Modified Biochar.

The utilization of biochar, derived from agricultural waste, has garnered attention as a valuable material for enhancing soil properties and serving as a substitute adsorbent for the elimination of hazardous heavy metals and organic contaminants from wastewater. In the present investigation, amide-modified biochar was synthesized via low-temperature pyrolysis of rice husk and was harnessed for the removal of Cr(VI) from wastewater. The resultant biochar was treated with 1-[3-(trimethoxysilyl) propyl] urea to incorporate an amide group. The amide-modified biochar was characterized by employing Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM), and X-ray diffraction (XRD) techniques. During batch experiments, the effect of various parameters, such as adsorbent dosage, metal concentration, time duration, and pH, on Cr(VI) removal was investigated. The optimal conditions for achieving maximum adsorption of Cr(VI) were observed at a pH 2, an adsorbent time of 60 min, an adsorbent dosage of 2 g/L, and a metal concentration of 100 mg/L. The percent removal efficiency of 97% was recorded for the removal of Cr(VI) under optimal conditions using amide-modified biochar. Freundlich, Langmuir, and Temkin isotherm models were utilized to calculate the adsorption data and determine the optimal fitting model. It was found that the adsorption data fitted well with the Langmuir isotherm model. A kinetics study revealed that the Cr(VI) adsorption onto ABC followed a pseudo-second-order kinetic model. The findings of this study indicate that amide-functionalized biochar has the potential to serve as an economically viable substitute adsorbent for the efficient removal of Cr(VI) from wastewater.

Improving the Energy Storage of Supercapattery Devices through Electrolyte Optimization for Mg(NbAgS)x(SO4)y Electrode Materials.

Electrolytes are one of the most influential aspects determining the efficiency of electrochemical supercapacitors. Therefore, in this paper, we investigate the effect of introducing co-solvents of ester into ethylene carbonate (EC). The use of ester co-solvents in ethylene carbonate (EC) as an electrolyte for supercapacitors improves conductivity, electrochemical properties, and stability, allowing greater energy storage capacity and increased device durability. We synthesized extremely thin nanosheets of niobium silver sulfide using a hydrothermal process and mixed them with magnesium sulfate in different wt% ratios to produce Mg(NbAgS)x)(SO4)y. The synergistic effect of MgSO4 and NbS2 increased the storage capacity and energy density of the supercapattery. Multivalent ion storage in Mg(NbAgS)x(SO4)y enables the storage of a number of ions. The Mg(NbAgS)x)(SO4)y was directly deposited on a nickel foam substrate using a simple and innovative electrodeposition approach. The synthesized silver Mg(NbAgS)x)(SO4)y provided a maximum specific capacity of 2087 C/g at 2.0 A/g current density because of its substantial electrochemically active surface area and linked nanosheet channels which aid in ion transportation. The supercapattery was designed with Mg(NbAgS)x)(SO4)y and activated carbon (AC) achieved a high energy density of 79 Wh/kg in addition to its high power density of 420 W/kg. The supercapattery (Mg(NbAgS)x)(SO4)y//AC) was subjected to 15,000 consecutive cycles. The Coulombic efficiency of the device was 81% after 15,000 consecutive cycles while retaining a 78% capacity retention. This study reveals that the use of this novel electrode material (Mg(NbAgS)x(SO4)y) in ester-based electrolytes has great potential in supercapattery applications.

Mirtazapine attenuated cadmium-induced neuronal intoxication by regulating Nrf2 and NF-κB/TLR4 signals.

Cadmium (Cd) is one of the most hazardous metals to the environment and human health. Neurotoxicity is of the most serious hazards caused by Cd. Mirtazapine (MZP) is a central presynaptic α2 receptor antagonist used effectively in treating several neurological disorders. This study investigated the anti-inflammatory and antioxidant activity of MZP against Cd-induced neurotoxicity. In this study, rats were randomly divided into five groups: control, MZP (30 mg/kg), Cd (6.5 mg/kg/day; i.p), Cd + MZP (15 mg/kg), and Cd + MZP (30 mg/kg). Histopathological examination, oxidative stress biomarkers, inflammatory cytokines, and the impact of Nrf2 and NF-κB/TLR4 signals were assessed in our study. Compared to Cd control rats, MZP attenuated histological abrasions in the cerebral cortex and CA1 and CA3 regions of the hippocampus as well as the dentate gyrus. MZP attenuated oxidative injury by upregulating Nrf2. In addition, MZP suppressed the inflammatory response by decreasing TNF-α, IL-1ß, and IL-6 mediated by downregulating TLR4 and NF-κB. It is noteworthy that MZP's neuroprotective actions were dose-dependent. Collectively, MZP is a promising therapeutic strategy for attenuating Cd-induced neurotoxicity by regulating Nrf2, and NF-κB/TLR4 signals, pending further study in clinical settings.

Isolation, Characterization and Anticancer Activity of Two Bioactive Compounds from Arisaema flavum (Forssk.) Schott.

Medicinal plants play important role in the public health sector worldwide. Natural products from medicinal plants are sources of unlimited opportunities for new drug leads because of their unique chemical diversity. Researchers have focused on exploring herbal products as potential sources for the treatment of cancer, cardiac and infectious diseases. Arisaema flavum (Forssk.) is an important medicinal plant found in the northwest Himalayan regions of Pakistan. It is a poisonous plant and is used as a remedy against snake bites and scorpion stings. In this study, two bioactive compounds were isolated from Arisaema flavum (Forssk.) and their anticancer activity was evaluated against human breast cancer cell line MCF-7 using an MTT assay. The crude extract of Arisaema flavum (Forssk.) was subjected to fractionation using different organic solvents in increasing order of polarity. The fraction indicating maximum activity was then taken for isolation of bioactive compounds using various chromatographic and spectroscopic techniques such as column chromatography, thin-layer chromatography (TLC), gas chromatography−mass spectrometry (GC-MS), Fourier transform infrared spectroscopy (FTIR) and nuclear magnetic resonance spectroscopy (NMR). Crude extract of Arisaema flavum (Forssk.), as well as various fractions extracted in different solvents such as n-hexane, chloroform and ethyl acetate, were tested against human breast cancer cell line MCF-7 using an MTT assay. The crude extract exhibited significant dose-dependent anticancer activity with a maximum activity of 78.6% at 500 µg/mL concentration. Two compounds, hexadecanoic acid ethyl ester with molecular formula C18H36O7 and molar mass 284 and 5-Oxo-19 propyl-docosanoic acid methyl ester with molecular formula C26H50O3 and molecular mass 410, were isolated from chloroform fraction. These compounds were tested against the MCF-7cell line for cytotoxic activity and exhibited a significant (p < 0.00l) decrease in cell numbers for MCF-7 cells with IC50 of 25 µM after 48 h of treatment. Results indicated that Arisaema flavum (Forssk.) possesses compounds with cytotoxic activity that can further be exploited to develop anticancer formulations.

Evaluation of the Anti-Cancer Potential of Rosa damascena Mill. Callus Extracts against the Human Colorectal Adenocarcinoma Cell Line.

Chemotherapy is an aggressive form of chemical drug therapy aiming to destroy cancer cells. Adjuvant therapy may reduce hazards of chemotherapy and help in destroying these cells when obtained from natural products, such as medical plants. In this study, the potential therapeutic effect of Rosa damascena callus crude extract produced in vitamin-enhanced media is investigated on colorectal cancer cell line Caco-2. Two elicitors, i.e., L-ascorbic acid and citric acid at a concentration of 0.5 g/L were added to the callus induction medium. Callus extraction and the GC-MS analysis of methanolic crude extracts were also determined. Cytotoxicity, clonogenicity, proliferation and migration of Caco-2 colorectal cancer cells were investigated using MTT cytotoxicity, colony-forming, Ki-67 flow cytometry proliferation and Migration Scratch assays, respectively. Our results indicated that L-ascorbic acid treatment enhanced callus growth parameters and improved secondary metabolite contents. It showed the least IC50 value of 137 ug/mL compared to 237 ug/mL and 180 ug/mL in the citric acid-treated and control group. We can conclude that R. damascena callus elicited by L-ascorbic acid improved growth and secondary metabolite contents as well as having an efficient antiproliferative, anti-clonogenic and anti-migratory effect on Caco-2 cancer cells, thus, can be used as an adjuvant anti-cancer therapy.

Graphene oxide-octadecylsilane incorporated monolithic nano-columns with 50 µm id and 100 µm id for small molecule and protein separation by nano-liquid chromatography.

In this study, graphene oxide-octadecylsilane incorporated monolithic nano-columns were developed for protein analysis by nano liquid chromatography (nano LC). The monolithic column with 100 µm id was first prepared by an in situ polymerization using ethylene dimethacrylate (EDMA), 3-chloro-2-hydroxypropylmethacrylate (HPMA-Cl), and methacryloyl graphene oxide nanoparticles (MGONPs). MGONPs were synthesized by the treatment of 3-(trimethoxysilyl)propylmethacrylate (TMSPM) and GO. Tetrahydrofuran (THF) and dodecanol were used as the porogenic solvent. The resulting column was functionalized by dimethyloctadecylch lorosilane (DODCS) for the enhancement of hydrophobicity. The functionalization greatly improved the baseline separation of hydrophobic compounds such as polyaromatic hydrocarbons (PAHs). The optimized monolith with respect to total polymerization mixture was characterized by using Fourier-transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) X-ray diffraction (XRD) and chromatographic analyses. The blank monoliths without functionalization exhibited poor separation while a good separation performance of MGONPs functionalized monoliths was achieved. The monolith with 100 µm id was evaluated in protein separation in nano LC using RNase A, Cytochrome C, Lysozyme, Trypsin, and Ca isozyme II as the test proteins. It was shown that protein separation mechanism was based on large π-system of GO and hydrophobicity of the monolithic structure. Theoretical plates number up to 57 600 plates were achieved. The nano-column with 50 µm id was also prepared using the same polymerization mixture under the same chemical conditions. These nano-columns were employed for protein separation by nano LC, and the dependence of both nano-column performance on the internal diameter was also discussed.

Efficient Removal of Pb(II) from Aqueous Medium Using Chemically Modified Silica Monolith.

The adsorptive removal of lead (II) from aqueous medium was carried out by chemically modified silica monolith particles. Porous silica monolith particles were prepared by the sol-gel method and their surface modification was carried out using trimethoxy silyl propyl urea (TSPU) to prepare inorganic-organic hybrid adsorbent. The resultant adsorbent was evaluated for the removal of lead (Pb) from aqueous medium. The effect of pH, adsorbent dose, metal ion concentration and adsorption time was determined. It was found that the optimum conditions for adsorption of lead (Pb) were pH 5, adsorbent dose of 0.4 g/L, Pb(II) ions concentration of 500 mg/L and adsorption time of 1 h. The adsorbent chemically modified SM was characterized by scanning electron microscopy (SEM), BET/BJH and thermo gravimetric analysis (TGA). The percent adsorption of Pb(II) onto chemically modified silica monolith particles was 98%. An isotherm study showed that the adsorption data of Pb(II) onto chemically modified SM was fully fitted with the Freundlich and Langmuir isotherm models. It was found from kinetic study that the adsorption of Pb(II) followed a pseudo second-order model. Moreover, thermodynamic study suggests that the adsorption of Pb(II) is spontaneous and exothermic. The adsorption capacity of chemically modified SM for Pb(II) ions was 792 mg/g which is quite high as compared to the traditional adsorbents. The adsorbent chemically modified SM was regenerated, used again three times for the adsorption of Pb(II) ions and it was found that the adsorption capacity of the regenerated adsorbent was only dropped by 7%. Due to high adsorption capacity chemically modified silica monolith particles could be used as an effective adsorbent for the removal of heavy metals from wastewater.

Various Strategies in Post-Polymerization Functionalization of Organic Polymer-Based Monoliths Used in Liquid Phase Separation Techniques.

This review article is aimed at summarizing the various strategies that have been developed so far for post-polymerization functionalization (PPF) of organic polymer-based monoliths used in liquid phase separation techniques, namely HPLC at all scales and capillary electrochromatography (CEC). The reader will find the organic reactions performed on monolithic columns for grafting the chromatographic ligands needed for solving the separation problems on hand. This process involves therefore the fabrication of template monoliths that carry reactive functional groups to which chromatographic ligands can be covalently attached in a post-polymerization kind of approach. That is, the template monolith that has been optimized in terms of pore structure and other morphology can be readily modified and tailor made on column to fit a particular separation. The review article will not only cover the various strategies developed so far but also describe their separation applications. To the best of our knowledge, this review article will be the first of its kind.

Development and Validation of Novel HPLC Methods for Quantitative Determination of Vitamin D3 in Tablet Dosage Form.

In the present work, an efficient isocratic HPLC method was developed for the precise and accurate estimation of vitamin D3 in tablet form. The chromatographic conditions comprised an L3 silica column (5 µm in particle size, 4.6 mm × 250 mm) with a mobile phase n-hexane/ethyl acetate (85:15 v/v) with a flow rate of 2.0 mL/min and a detection wavelength of 292 nm. The new methodology was validated for accuracy, precision, specificity, robustness, and quantification limits according to an official monograph of USP/BP and ICH guidelines. The peak areas of the six replicates of the homogeneous sample were recorded. The mean value obtained was 67,301, and the relative standard deviation (RSD) was 0.1741. The linearity and range were in the acceptable bounds, i.e., 0.999, which was calculated using regression line analysis. The results show that the method is truly acceptable as the RSD, as the flow rate was 0.81%, while for the mobile phase composition, it was 0.72%, which lies in the acceptable range. The limit of detection (LOD) and the limit of quantification (LOQ) values were 0.0539 µg/mL and 0.1633 µg/mL, respectively. The % RSD of the intra and inter-day precision of the method was deemed acceptable according to the international commission for harmonization guidelines. The developed method has potential to be used for the detection and quantification of vitamin D3 during routine analysis for tablets in dosage form.

Ultrathin optically transparent carbon electrodes produced from layers of adsorbed proteins.

This work describes a simple, versatile, and inexpensive procedure to prepare optically transparent carbon electrodes, using proteins as precursors. Upon adsorption, the protein-coated substrates were pyrolyzed under reductive conditions (5% H2) to form ultrathin, conductive electrodes. Because proteins spontaneously adsorb to interfaces forming uniform layers, the proposed method does not require a precise control of the preparation conditions, specialized instrumentation, or expensive precursors. The resulting electrodes were characterized by a combination of electrochemical, optical, and spectroscopic means. As a proof-of-concept, the optically transparent electrodes were also used as substrate for the development of an electrochemical glucose biosensor. The proposed films represent a convenient alternative to more sophisticated, and less available, carbon-based nanomaterials. Furthermore, these films could be formed on a variety of substrates, without classical limitations of size or shape.

Nano-liquid chromatography with monolithic stationary phase based on naphthyl monomer for proteomics analysis.

Monolithic poly(2-vinylnaphthalene-co-divinylbenzene) columns were introduced, for the first time, and were evaluated as the separation media for nano-liquid chromatography (nano-LC). These columns were prepared by in-situ polymerization of 2-vinylnaphthalene (2-VNA) as the functional monomer and divinylbenzene (DVB) as the crosslinker in a fused silica capillary column of 50 µm i.d. Various porogenic solvents, including tetrahydrofuran (THF), dodecanol and toluene were used for morphology optimization. Final monolithic column (referred to as VNA column) was characterized by using scanning electron microscopy (SEM) and chromatographic analyses. Alkylbenzenes (ABs), and polyaromatic hydrocarbons (PAHs) were separated using the VNA column while the column offered excellent hydrophobic and π-π interactions under reversed-phase conditions. Theoretical plates number up to 41,200 plates/m in isocratic mode for ethylbenzene could be achieved. The potential of the final VNA column was demonstrated with a gradient elution in the  separation of six intact proteins, including ribonuclease A (RNase A), cytochrome C (Cyt C), lysozyme (Lys), ß-lactoglobulin (ß-lac), myoglobin (My) and α-chymotrypsinogen (α-chym) in nano LC system. The column was then applied to the peptide analysis of trypsin digested cytochrome C, allowing a high peak capacity up to 1440 and the further proteomics analysis of COS-7 cell line was attempted applying the final monolithic column in nano-LC UV system.

Juglans regia Linn.: A Natural Repository of Vital Phytochemical and Pharmacological Compounds.

Juglans regia Linn. is a valuable medicinal plant that possesses the therapeutic potential to treat a wide range of diseases in humans. It has been known to have significant nutritional and curative properties since ancient times, and almost all parts of this plant have been utilized to cure numerous fungal and bacterial disorders. The separation and identification of the active ingredients in J. regia as well as the testing of those active compounds for pharmacological properties are currently of great interest. Recently, the naphthoquinones extracted from walnut have been observed to inhibit the enzymes essential for viral protein synthesis in the SARS-CoV-2. Anticancer characteristics have been observed in the synthetic triazole analogue derivatives of juglone, and the unique modifications in the parent derivative of juglone have paved the way for further synthetic research in this area. Though there are some research articles available on the pharmacological importance of J. regia, a comprehensive review article to summarize these findings is still required. The current review, therefore, abridges the most recent scientific findings about antimicrobial, antioxidant, anti-fungal, and anticancer properties of various discovered and separated chemical compounds from different solvents and different parts of J. regia.

Synergistic redox enhancement: silver phosphate augmentation for optimizing magnesium copper phosphate in efficient energy storage devices and oxygen evolution reaction.

The implementation of battery-like electrode materials with complicated hollow structures, large surface areas, and excellent redox properties is an attractive strategy to improve the performance of hybrid supercapacitors. The efficiency of a supercapattery is determined by its energy density, rate capabilities, and electrode reliability. In this study, a magnesium copper phosphate nanocomposite (MgCuPO4) was synthesized using a hydrothermal technique, and silver phosphate (Ag3PO4) was decorated on its surface using a sonochemical technique. Morphological analyses demonstrated that Ag3PO4 was closely bound to the surface of amorphous MgCuPO4. The MgCuPO4 nanocomposite electrode showed a 1138 C g-1 capacity at 2 A g-1 with considerably improved capacity retention of 59% at 3.2 A g-1. The increased capacity retention was due to the fast movement of electrons and the presence of an excess of active sites for the diffusion of ions from the porous Ag3PO4 surface. The MgCuPO4-Ag3PO4//AC supercapattery showed 49.4 W h kg-1 energy density at 550 W kg-1 power density and outstanding capacity retention (92% after 5000 cycles). The experimental findings for the oxygen evolution reaction reveal that the initial increase in potential required for MgCuPO4-Ag3PO4 is 142 mV, indicating a clear Tafel slope of 49 mV dec-1.

Effect of Cr-Doping on the Structural and Magnetic Properties of Mechanically Alloyed FeCoNiAlMn1-xCrx High-Entropy Alloy Powder.

In this work, the new compositions of FeCoNiAlMn1-xCrx, (0.0 ≤ x ≤ 1.0), a high-entropy alloy powder (HEAP), are prepared by mechanical alloying (MA). The influence of Cr doping on the phase structure, microstructure, and magnetic properties is thoroughly investigated through X-ray diffraction (XRD), scanning electron microscopy (SEM), and vibrating sample magnetometry. It is found that this alloy has formed a simple body-centered cubic structure with a minute face-centered cubic structure for Mn to Cr replacement with heat treatment. The lattice parameter, average crystallite size, and grain size decrease by replacing Cr with Mn. The SEM analysis of FeCoNiAlMn showed no grain boundary formation, depicting a single-phase microstructure after MA, similar to XRD. The saturation magnetization first increases (68 emu/g) up to x = 0.6 and then decreases with complete substitution of Cr. Magnetic properties are related to crystallite size. FeCoNiAlMn0.4Cr0.6 HEAP has shown optimum results with better saturation magnetization and coercivity as a soft magnet.

Application of ZnO-NRs@Ni-foam substrate for electrochemical fingerprint of arsenic detection in water.

Arsenic (As3+) is the most carcinogenic and abundantly available heavy metal present in the environment. Vertically aligned ZnO nanorod (ZnO-NR) growth was achieved on metallic nickel foam substrate via a wet chemical route and it was used as an electrochemical sensor towards As(iii) detection in polluted water. Crystal structure confirmation, surface morphology observation and elemental analysis of ZnO-NRs were conducted using X-ray diffraction, field-emission scanning electron microscopy and energy-dispersive X-ray spectroscopy, respectively. Electrochemical sensing performance of ZnO-NRs@Ni-foam electrode/substrate was investigated via linear sweep voltammetry, cyclic voltammetry and electrochemical impedance spectroscopy in a carbonate buffer solution of pH = 9 and at different As(iii) molar concentrations in solution. Under optimum conditions, the anodic peak current was found proportional to the arsenite concentration from 0.1 µM to 1.0 µM. The achieved values for limit of detection and limit of quantification were 0.046 ppm and 0.14 ppm, respectively, which are far lower than the recommended limits for As(iii) detection in drinking water as suggested by the World Health Organization. This suggests that ZnO-NRs@Ni-foam electrode/substrate can be effectively utilized in terms of its electrocatalytic activity towards As3+ detection in drinking water.

Investigating the Physical Properties of Thallium-Based Ternary TlXF3 (X = Be, Sr) Fluoroperovskite Compounds for Prospective Applications.

In the present work, several properties of fluoroperovskites are computed and examined through the approximations of trans- and blaha-modified Becke-Johnson (TB-mBJ) and generalized gradient approximation of Perdew-Burke-Ernzerhof (GGA-PBE) integrated within density functional theory (DFT). The lattice parameters for cubic TlXF3 (X = Be, Sr) ternary fluoroperovskite compounds at an optimized state are examined and their values are used to calculate the fundamental physical properties. TlXF3 (X = Be and Sr) cubic fluoroperovskite compounds contain no inversion symmetry and are thus a non-centrosymmetric system. The phonon dispersion spectra confirm the thermodynamic stability of these compounds. The results of electronic properties clarify that both the compounds possess a 4.3 eV of indirect band gap from M-X for TlBeF3 and a direct band gap of 6.03 eV from X-X for TlSrF3, which display that both compounds are insulators. Furthermore, the dielectric function is considered to explore optical properties like reflectivity, refractive index, absorption coefficient, etc., and the different types of transitions between the bands were investigated by using the imaginary part of the dielectric function. Mechanically, the compounds of interest are computed to be stable and possess high bulk modulus values, and the ratio of "G/B" is higher than "1", which indicates the strong and ductile nature of the compound. Based on our computations for the selected materials, we deem an efficient application of these compounds in an industrial application, which will provide a reference for future work.

Open tubular nano-liquid chromatography with a new polylysine grafted on graphene oxide stationary phase for the separation and determination of casein protein variants in milk.

In this study, a novel narrow capillary (i.e., 20 µm i.d.) coating procedure was reported for the preparation and application of open-tubular (OT) column for the separation of casein (CN) protein variants in milk. Based on this approach, a new poly-L-lysine (PLL) grafted on graphene oxide stationary phase was developed for OT nano-liquid chromatography (OT-nano LC). In this preparation, methacryloyl graphene oxide nanoparticles (MGONPs) were synthesized and used as reactive monomer. Fused silica capillaries with 20 µm i.d. were used for the preparation of OT column. After silanization of the capillary column, the stationary phase was prepared by MGONPs graft polymerization and PLL modification. It was shown that the use of MGONPs amount was important for the capillary coating. A column without PLL modification was also prepared for comparing the effect of PLL. SEM images of the column showed that MGONPs were bound to the surface of capillary in a dense monolayer. Alkylbenzenes (ABs) were used for the chromatographic characterization of the OT column. The results showed that the modification was successfully performed and allowed satisfactory separation of ABs. The developed OT column in the ProFlow nano-LC was applied to the separation of casein (CN) protein variants, including αs1-CN, αs2-CN, ß-CN and Ƙ-CN. Results indicated that the column provided a promising separation of casein protein variants due to both hydrophobic interactions and repulsive electrostatic interactions. Run-to-run and column-to-column reproducibilities were satisfactory (i.e., ≤3.12%). Real sample application of the OT column was demonstrated using a milk sample. Several isoforms of αs1-CN could be detected. All results demonstrated that the developed OT column with a novel coating procedure was promising for advanced nano-liquid chromatographic separations.

Efficient Synthetic Access to Novel Indolo[2,3-b]Quinoxaline-based Heterocycles.

BACKGROUND: This paper showed the synthetic capability of the indolo[2,3-b]quinoxaline nucleus to be provided as an excellent precursor for the synthesis of various heterocyclic compounds. These synthetic routes proceed via the formation of 3-(6H-indolo[2,3-b]quinoxalin-6-yl) propane hydrazide (2). The carbohydrazide 2 and its reactions with different reagents give five and six-membered rings, such as 1,3,4-thiadiazole, 1,3,4- oxadiazole, 1,2,4-triazole, and 1,2,4-triazine. METHODS: All chemicals used in the current study were of analytical grade. Melting points were determined using an APP Digital ST 15 melting point apparatus and were uncorrected. FT-IR spectra were recorded on a Pye- Unicam SP3-100 and Shimadzu-408 spectrophotometers in KBr pellets and given in (cm-1) KBr. The NMR spectra were detected by a Bruker AV-400 spectrometer (400 MHz for 1H, 100 MHz for 1C and 40.55 MHz for 15N), Institute of Organic Chemistry, Karlsruhe, Germany. Chemical shifts were expressed as δ (ppm) with TMS as an internal reference. Mass spectrometry was provided on a Varian MAT 312 instrument in EI mode (70 eV). RESULTS: The target compounds were obtained, and their structures were completely elucidated by various spectral and elemental analyses (Ft-IR, 1H-NMR, 13;C-NMR, and mass spectrometry). CONCLUSION: The current work showed a view of the reactivity of the carbohydrazide group. The carbohydrazide 2 was obtained from the hydrazinolysis of carboethoxy compound 1 and exploited as a key intermediate to synthesize heterocyclic compounds with different rings.

Development of Narrow-Bore C18 Column for Fast Separation of Peptides and Proteins in High-Performance Liquid Chromatography.

Separation with high efficiency and good resolution is constantly in demand in the pharmaceutical industry. The fast and efficient separation of complex samples such as peptides and proteins is a challenging task. To achieve high efficiency with good resolution, chromatographers are moving towards small particles packed into narrow-bore columns. Silica monolith particles (sub-2 µm) were derivatized with chlorodimethyl octadecyl silane (C18) and packed into stainless steel columns (100 mm × 1.8 mm i.d) by a slurry-packing method. The developed columns were used for the separation of peptides and proteins. A separation efficiency (N) of 40,000 plates/column (400,000 plates/m) was achieved for the mixture of five peptides. Similarly, the fast separation of the peptides was carried out using a high flow rate, and the separation of the five peptides was achieved in one minute with high efficiency (N ≅ 240,000 plates/m). The limit of detection (DL) and the limit of quantification (QL) for each analyte were determined by developing a linear regression curve with relatively very low concentrations of the target compound. The average values of the QL for the peptide and proteins were 0.55 ng and 0.48 ng, respectively, using short C18 column (1.8 mm × 100 mm) UV (at 214 nm). The fast analysis of peptides and proteins with such high efficiency and good resolution has not been reported in the literature yet. Owing to high efficiency, these home-made columns could be used as an alternative to the expensive commercial columns for peptide and protein separation.

Preparation of mixed-mode stationary phase for separation of peptides and proteins in high performance liquid chromatography.

Porous silica particles were prepared by sol-gel method with some modification to get wide-pore particles. These particles were derivatized with N-phenylmaleimide-methylvinylisocyanate (PMI) and styrene by reversible addition fragmentation chain transfer (RAFT) polymerization to prepare N-phenylmaleimide embedded polystyrene (PMP) stationary phases. Narrow bore stainless steel column (100 × 1.8 mm i.d) was packed by slurry packing method. The chromatographic performance of PMP column was evaluated for the separation of synthetic peptides mixture composed of five peptides (Gly-Tyr, Gly-Leu-Tyr, Gly-Gly-Tyr-Arg, Tyr-Ile-Gly-Ser-Arg, Leucine enkephalin) and tryptic digest of human serum albumin (HAS) respectively. Number of theoretical plates as high as 280,000 plates/m were obtained for peptides mixture at optimum elution condition. Separation performance of the developed column was compared with commercial Ascentis Express RP-Amide column and it was observed that separation performance of PMP column was better than commercial column in terms of separation efficiency and resolution.