Arfana Mallah

Quantitative separation of oxytocin, norfloxacin and diclofenac sodium in milk samples using capillary electrophoresis.

A simple, sensitive and rapid method has been developed for simultaneous separation and quantification of three different drugs: oxytocin (OT), norfloxacin (NOR) and diclofenac (DIC) sodium in milk samples using capillary electrophoresis (CE) with UV detection at 220 nm. Factors affecting the separation were pH, concentration of buffer and applied voltage. Separation was obtained in less than 9 min with sodium tetraborate buffer of pH 10.0 and applied voltage 30 kV. The separation was carried out from uncoated fused silica capillary with effective length of 50 cm with 75 microm i.d. The carrier electrolyte gave reproducible separation with calibration plots linear over 0.15-4.0 microg/mL for OT, 5-1000 microg/mL for NOR and 3-125 microg/mL for DIC. The lower limits of detection (LOD) were found to be 50 ng/mL for OT, and 1 microg/mL for NOR and DIC. The method was validated for the analysis of drugs in milk samples and pharmaceutical preparations with recovery of drugs within the range 96-100% with RSD 0.9-2.8%.

A Robust, Enzyme-Free Glucose Sensor Based on Lysine-Assisted CuO Nanostructures

The production of a nanomaterial with enhanced and desirable electrocatalytic properties is of prime importance, and the commercialization of devices containing these materials is a challenging task. In this study, unique cupric oxide (CuO) nanostructures were synthesized using lysine as a soft template for the evolution of morphology via a rapid and boiled hydrothermal method. The morphology and structure of the synthesized CuO nanomaterial were characterized using scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. The prepared CuO nanostructures showed high potential for use in the electrocatalytic oxidation of glucose in an alkaline medium. The proposed enzyme-free glucose sensor demonstrated a robust response to glucose with a wide linear range and high sensitivity, selectivity, stability, and reproducibility. To explore its practical feasibility, the glucose content of serum samples was successfully determined using the enzyme-free sensor. An analytical recovery method was used to measure the actual glucose from the serum samples, and the results were satisfactory. Moreover, the presented glucose sensor has high chemical stability and can be reused for repetitive measurements. This study introduces an enzyme-free glucose sensor as an alternative tool for clinical glucose quantification.

A MEKC method for naringenin from natural and biological samples

The work reported describes the development of a micellar electrokinetic chromatographic (MEKC) method for the determination of naringenin in real samples including grapefruit juice and human blood serum using a PDA detector. The effects of different CE parameters such as concentration and pH of the running buffer, voltage, injection time and concentration of sodium dodecyl sulfate (SDS) were optimized. Under the optimized conditions, naringenin could be well determined within 6 min using 40 mM borate buffer, 40 mM SDS at pH 9.0, at an applied voltage of 25 kV. For the quantitative determination of naringenin (flavonoid aglycone) in grapefruit juice, the naringin (flavonoid glycoside) was hydrolysed and the resulting aglycone was identified and quantified. The calibration curve was linear in the studied concentration range of 0.1 to 50 μg mL−1 (R2 = 0.995). The detection limit and the limit of quantification were found to be 0.05 and 0.19 μg mL−1, respectively.

Schiff Bases as Chelating Reagents for Metal Ions Analysis

The Schiff bases are formed by condensation of different -diketones, salicylaldehydes or 2hydroxyacetophenes with various amines. These bases react with metal and oxo-metal cations to form stable metal chelates which absorb/fluoresce in UV or visible region of light. The Schiff bases have been used in the determination of metal ions by spectrophotometry, spectrofluorimetry, gas chromatography, liquid chromatography and capillary electrophoresis. Ion-selective electrodes using Schiff’s bases is an emerging area for metal ion analysis. This review covers brief synthesis, chelation properties and analytical applications of Schiff bases.

Cathodic stripping voltammetry of pipemidic acid and ofloxacin in pharmaceutical dosages and human urine

Sensitive cathodic stripping voltammetric methods have been developed for two quinolone antibacterial drugs, pipemidic acid (PIP) and ofloxacin (OFL) using hanging mercury drop electrode as working electrode vs. Ag/AgCl reference electrode. The methods were developed for the determination of drugs individually as well as simultaneously. 0.1 M and 0.01 M hydrochloric acid was used as medium for PIP and OFL, respectively, 0.1 M potassium chloride was used as base electrolyte. Reduction waves were observed for PIP within −700 mV to −800 mV and for OFL within −1100 mV to −1200 mV. Linear calibration ranges for PIP and OFL were observed within 10–100 μg ml−1 with detection limits of 50 ng ml−1 and 1 μg ml−1, respectively. Relative standard deviations (RSD) for the analysis of 10 gµg ml−1 of PIP and OFL (n = 6) were 0.5% and 1.4%, respectively. The presence of glucose, lactose, sorbitol, gum arabic, starch, magnesium stearate, methylparaben and propylparaben did not affect the determinations of both PIP and OFL. The methods were used for the analysis of pharmaceutical preparations and the results indicated relative deviation of 0.5–5.5% from labeled values with RSD within 0.49–2.5%. PIP and OFL could also be determined simultaneously, and were determined from spiked human urine.

Quantitative separation of hesperidin, chrysin, epicatechin, epigallocatechin gallate, and morin using ionic liquid as a buffer additive in capillary electrophoresis

Recently, an increasing interest has been observed in ionic liquids (ILs) due to their potentialities in various chemical processes. ILs have some unique properties making them excellent additives in CE. In this work a simple, rapid, and reliable CZE method has been developed and validated using 1‐butyl‐3‐methyl imidazolium hexafluorophosphate (BMIM‐PF6) ionic liquid as a buffer additive for the determination/separation of five flavonoids including hesperedin, epicatechin (EC), epigallocatechin gallate (EGCG), and morin using photodiode array (PDA) detector. The effect of several parameters such as concentration and pH of the running buffer, applied voltage, and concentration of ionic liquid were optimized. CZE at 25°C with 25 mM borate buffer of pH 9.0 at an applied voltage of 17 kV by adding 17.5 mM of IL was found to be suitable for the separation/determination of all five analytes within 08 min. Validation of the method was performed in terms of linearity, accuracy, precision, and limit of detection and quantification. The calibration curves were plotted in the concentration range of 1–200 μg/mL for all five analytes. The response was linear with R2 = 0.990 for EC, chrysin, and hesperidin, 0.992 for morin, and 0.988 for EGCG. LOD and LOQ were obtained within the range of 0.4–0.5 and 1.4–1.7 μg/mL, respectively. The proposed method showed good reproducibility with RSD of less than 3% for both migration time and peak height. The method was successfully applied for the determination of flavonoids from citrus fruits and tea samples.

Reversed-Phase Liquid Chromatographic Separation and Determination of Ni(II), Cu(II), Pd(II), and Ag(I) Using 2-Pyrrolecarboxaldehyde-4-phenylsemicarbazone as a Complexing Reagent

This paper reports the utilization of 2-pyrrolecarboxaldehyde-4-phenylsemicarbazone (PPS) as a complexing reagent for the simultaneous determination and separation of Ni(II), Cu(II), Pd(II), and Ag(I) by reversed-phase high-performance liquid chromatography with UV detector. A good separation was achieved using Microsorb C18 column (150 × 4.6 mm i.d.) with a mobile phase consisted of methanol : acetonitrile : water : sodium acetate (1 mM) (68 : 6.5 : 25 : 0.5 v/v/v/v) at a flow rate of 1 mL/min. The detection was performed at 280 nm. The linear calibration range was 2–10 μg/mL for all metal ions. The detection limits (S/N = 3) were 80 pg/mL for Ni(II), 0.8 ng/mL for Cu(II), 0.16 ng/mL for Pd(II), and 0.8 ng/mL for Ag(I). The applicability and the accuracy of the developed method were estimated by the analysis of Ni(II) in hydrogenated oil (ghee) samples and Pd(II) in palladium charcoal.

A Novel Micellar Electrokinetic Chromatographic Method for Separation of Metal-DDTC Complexes

Micellar electrokinetic chromatography (MEKC) was examined for the separation and determination of Mo(VI), Cr(VI), Ni(II), Pd(II), and Co(III) as diethyl dithiocarbamate (DDTC) chelates. The separation was achieved from fused silica capillary (52 cm × 75 μm id) with effective length 40 cm, background electrolyte (BGE) borate buffer pH 9.1 (25 mM), CTAB 30% (100 mM), and 1% butanol in methanol (70 : 30 : 5 v/v/v) with applied voltage of -10 kV using reverse polarity. The photodiode array detection was achieved at 225 nm. The linear calibration for each of the element was obtained within 0.16-10 μg/mL with a limit of detection (LOD) 0.005-0.0167 μg/mL. The separation and determination was repeatable with relative standard deviation (RSD) within 2.4-3.3% (n = 4) in terms of migration time and peak height/peak area. The method was applied for the determination of Mo(VI) from potatoes and almond, Ni(II) from hydrogenated vegetable oil, and Co(III) from pharmaceutical preparations with RSD within 3.9%. The results obtained were checked by standard addition and rechecked by atomic absorption spectrometry.

Synthesis of Heart/Dumbbell-Like CuO Functional Nanostructures for the Development of Uric Acid Biosensor

It is always demanded to prepare a nanostructured material with prominent functional properties for the development of a new generation of devices. This study is focused on the synthesis of heart/dumbbell-like CuO nanostructures using a low-temperature aqueous chemical growth method with vitamin B12 as a soft template and growth directing agent. CuO nanostructures are characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), and X-ray photoelectron spectroscopy (XPS) techniques. CuO nanostructures are heart/dumbbell like in shape, exhibit high crystalline quality as demonstrated by XRD, and have no impurity as confirmed by XPS. Apparently, CuO material seems to be porous in structure, which can easily carry large amount of enzyme molecules, thus enhanced performance is shown for the determination of uric acid. The working linear range of the biosensor is 0.001 mM to 10 mM with a detection limit of 0.0005 mM and a sensitivity of 61.88 mV/decade. The presented uric acid biosensor is highly stable, repeatable, and reproducible. The analytical practicality of the proposed uric acid biosensor is also monitored. The fabrication methodology is inexpensive, simple, and scalable, which ensures the capitalization of the developed uric acid biosensor for commercialization. Also, CuO material can be used for various applications such as solar cells, lithium ion batteries, and supercapacitors.