A simple and highly sensitive cloud point extraction process was suggested for preconcentration of micrograms amount of isoxsuprine hydrochloride (ISX) in pure and pharmaceutical samples. After diazotization coupling of ISX with diazotized sulfadimidine in alkaline medium, the azo-dye product quantitatively extracted into the Triton X-114 rich phase, dissolved in ethanol and determined spectrophotometrically at 490 nm. The suggested reaction was studied with and without extraction and simple comparison between the batch and CPE methods was achieved. Analytical variables including concentrations of reagent, Triton X-114 and base, incubated temperature, and time were carefully studied. Under the selected optimum conditions, the linearity ranges of calibration curves were 1-9 and 0.5-8 µg/mL with detection limits of 0.26 and 0.09 µg/mL of ISX for batch and CPE methods respectively. A relative standard deviation (RSD %) best than 1.98 and 2.67 % with the percentage recoveries range 100.14 and 99.63 % were obtained for both methods respectively. The proposed methods were successfully used in routine analysis of ISX in pharmaceutical forms with high accuracy and reproducibility.
The UV−VIS absorption spectroscopy technique was used to study the formation of a new complex of charge transfer (CT) between bioactive organic molecules as (Nystatin) containing both a π-electrons from a conjugated system and lone-pair of electrons (amine) with Tetrachloro-1,4 benzoquinone (TCBQ) as a π-acceptor in which the transferred electron goes into its vacant anti-bonding molecular orbitals. The Tyrian purple-colored complex formed was quantitatively measured at 544 nm. This complex shows obeying Beer's law within the concentration range of (10-90) μg.ml-1The stoichiometry of the formed complex between the (Nys.) and (TCBQ) was found 1:2 as evaluated by continuous variation (Job's method) and mole ratio method The value of mola
... Show MoreSeparation of Trigonelline, the major alkaloid in fenugreek seeds, is difficult because the extract of these seeds usually contains Trigonelline, choline, mucilage, and steroidal saponins, in addition to some other substances. This study amis to isolate the quaternary ammonium alkaloid (Trigonelline) and choline from fenugreek seeds (Trigonella-foenum graecum L.) which have similar physiochemical properties by modifying of the classical method. Seeds were defatted and then extracted with methanol. The presence of alkaloids was detected by using Mayer's and Dragendorff's reagents. In this work, trigonilline was isolated with traces of choline by subsequent processes of purification using analytical and preparative TLC techniques.
... Show MoreA new spectrophotometric method for individual and simultaneous determination of cefixime and cephalexin depending on the first and second derivative mode techniques. The first and second derivative spectra of these compounds permitted individual and simultaneous determination of cefixime and cephalexin in concentration interval of (4– 24μg.ml-1 ) by measuring the amplitude of peak-to-base line, pea to peak at certain wavelengths and the area under peak at selected spectrum intervals. The methods showed reasonable precision and accuracy and have been applied to determine cefixime and cephalexin in two different pharmaceutical preparations.
ABSTRACT
Naproxen(NPX) imprinted liquid electrodes of polymers are built using polymerization precipitation. The molecularly imprinted (MIP) and non imprinted (NIP) polymers were synthesized using NPX as a template. In the polymerization precipitation involved, styrene(STY) was used as monomer, N,N-methylenediacrylamide (N,N-MDAM) as a cross-linker and benzoyl peroxide (BPO) as an initiator. The molecularly imprinted membranes and the non-imprinted membranes were prepared using acetophenone(AOPH) and di octylphathalate(DOP)as plasticizers in PVC matrix. The slopes and detection limits of the liquid electrodes ranged from)-18.1,-17.72 (mV/decade and )4.0 x 10-
... Show MoreLiquid membrane electrodes for the determination iron(III) were constructed based on chloramphenicol sodium succinate and iron(III) CPSS-Fe(III) as ion pair complex, with four plasticizers Di-butyl phosphate (DBP); Di-butyl phthalate (DBPH); Di-octyl phthalate (DOP); Tri-butyl phosphate (TBP); in PVC matrix . These electrodes give Nernstian and sub-Nernstian slopes (19.79, 24.60, 16.01 and 13.82mV/decade) and linear ranges from (1x10-5-1x10-2 M, 1x10-5-1x10-2 M, 1x10-6-1x10-2 M and 1x10-5-1x10-2 M) respectively. The best electrode was based on DBP plasticizer which gave a slope 19.79 mV/decade, correlation coefficient 0.9999, detection limit of 9×10-6 M, lifetime 37 day displayed good stability and reproducibility and used to determine
... Show MoreThe aim of this study is to evaluate the levels of trace elements Magnesium (Mg), Zinc (Zn), Copper (Cu), and Selenium (Se) in blood sera of asthmatic patients by Atomic Absorption Spectrophotometry (AAS). The concentrations of Mg, Cu, and Zn have been determined by Flame Atomic Absorption spectrophotometry (FAAS), and Se with flameless Graphite Furnace Atomic Absorption Spectrophotometry (GFAAS). The study involves (55) asthmatic patients as study group and (28) subjects as control from both genders. Serum levels of Mg, Cu, and Se were significantly higher (p<0.001 for all) in patients when compared with healthy subjects, while Zn level was relatively significant (p<0.05). Our observations confirm the efficacy and applicability of (AAS) in
... Show MoreSimple and sensitive batch and Flow-injection spectrophotometric methods for the determination of Procaine HCl in pure form and in injections were proposed. These methods were based on a diazotization reaction of procaine HCl with sodium nitrite and hydrochloric acid to form diazonium salt, which is coupled with chromatropic acid in alkaline medium to form an intense pink water-soluble dye that is stable and has a maximum absorption at 508 nm. A graphs of absorbance versus concentration show that Beer’s law is obeyed over the concentration range of 1-40 and 5-400 µg.ml-1 of Procaine HCl, with detection limits of 0.874 and 3.75 µg.ml-1 of Procaine HCl for batch and FIA methods respectively. The FIA average sample throughput was 70 h-1. A
... Show MoreA new method for construction ion-selective electrode (ISE) by heating reaction of methyl orange with ammonium reineckate using PVC as plasticizer for determination methyl orange and determination Amitriptyline Hydrochloried drug by formation ion-pair on electrode surface . The characteristics of the electrode and it response as following : internal solution 10-4M , pH (2.5-5) ,temperature (20-30) and response time 2 sec. Calibration response for methyl orange over the concentrationrange 10-3 -10-9 M with R=0.9989 , RSD%=0.1052, D.O.L=0.315X10-9 MEre%=(-0.877- -2.76) , Rec%.=(97.230 -101.711) .