The present work establishes and validates HILIC strategies simple, accurate, exact and precise in pure form and inpharmaceutical dosage for separating and determining theophylline. These methods are developed on HILIC theophyllineseparation in columns ZIC2 and ZIC3. The eluent was prepared by mixing buffer (20% sodium acetate-40 mM, pH 5.5), 80%acetonitrile. The flow rate is 0.8 mL/min, with gradient elution and UV detection at 270 nm. In the ZIC2 and ZIC3 columns oftheophylline determining, the concentration range was 0.01-4μg.ml-1. The lower limit of detection and quantification fortheophylline were determined as 0.130, 0.190 μg.ml-1 and accuracy were 99.70%, 99.58% on ZIC2 and ZIC3, respectively. TheHILIC methods developed and validated and statistical analysis indicate that the methods for estimating theophylline can bereplicated and chosen.
Two methods have been applied for the spectrophotometric determination of atropine, in
bulk sample and in dosage form. The methods are accurate, simple, rapid, inexpensive and
sensitive. The first method depending on the extraction of the formed ion-pair complex with
bromphenol blue (BPB) as a chromogenic reagent in chloroform, use phthalate buffer of pH
3.0; which showed absorbance maxima at 413 nm against reagent blank. The calibration
graph is linear in the ranges of 0.5-40 µg.mL
-1
with detection limit of 0.363µg.mL
-1
. The
second method depending on the measure of the absorbance maxima of the formed charge-transfer complex with 2,3-dichloro-5,6-dicyano-p-benzoquinone (DDQ) at 457 nm against
Phenytoin selective electrodes were constructed based on penytoin-phosphotungstate (Ph-PT) complex with different plasticizers; di-butyl phosphate (DBP), tri-butyl phosphate (TBP), di-butyl phthalate (DBPH),and o-nitro phenyl octyl ether (NPOE) phthalate. The electrodes based on DBPH, ONPOE plasticizers gave Narnistain slope which are, 56.4 and 55.3mV/decade with detection limit of 1.9x10-5 M , 1.8x10-5 and concentration range 10-1 to 10-4 M and pH range 3.0 – 8.0. The electrodes based on TBP and DBP showed non-Nernistain slopes, 40.2,40.5 mV/decade for both plasticizers. Interfering of some cations was investigated and shows no interfering with electrodes response. Potentiometric methods were used for measuring phenytion in
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Liquid 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
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Two simple and sensitive spectrophotometric methods are proposed for the determination of amitriptyline in its pure form and in tablets. The first method is based on the formation of charge- transfer complex between amitriptyline as n-donor and tetracyano-ethylene (TCNE) as πacceptor. The product exhibit absorbance maximum at 470 nm in acetonitrile solvent (pH =9.0 ) . In the second method the absorbance of the ion- pair complex, which is formed between the soughted drug and bromocresol green (BCG), was measured at 415 nm at ( pH=3.5) . In addition to classical univariate optimization, modified simplex method (MSM) was applied in the optimization of the variable affecting the color producing reaction by a geometric simple
... Show MoreA new colorimetric-flow injection method has been developed and validated for the detection of Cefotaxime sodium in pharmaceutical formulations. This method stands out for its rapid and sensitive nature. The formation of a brown-colored complex between Cefotaxime sodium and the Biuret reagent in a highly alkaline environment serves as the basis for the detection. The intensity of this colored complex is measured using a custom-built Continuous Flow Injection Analyzer, enabling accurate quantification of Cefotaxime sodium. Optimization studies of the chemical and physical parameters such as dilution of Biuret reagent, effect of the medium basicity, flow rate, sample loop and others have been investigated. The calibration gra
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New chlropheniramine maleate (CPM) selective electrochemical membranes were prepared by using chlropheniramine maleate -molecularly imprinted polymers. MIP was prepared by bulk polymerization using 2-hydroxyethyl methacrylate (2-HEMA) as monomer, ethylene glycol dimethacrylate (EGDMA) as a cross-linker and a benzoyl peroxide (BPO) as an initiator at 600C. Three CPM-MIP electrodes were constructed by using tri-tolyl Phosphate (ToCP), tris (2- ethyl hexyl) Phosphate (TEHP) and tributyl Phosphate (TBP) as plasticizers in PVC matrix.Electrode parameters including slopes, working concentrations ph. The interference effect in the presence of (Na+, Mg+2, Al+3, Glycine, Alanine, Arginine and Phenylalanine) was studied using the separated a
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PVC membrane sensor for the selective determination of Mefenamic acid (MFA) was constructed. The sensor is based on ion association of MFA with Dodecaphospho molybdic acid (PMA) and Dodeca–Tungstophosphoric acid(PTA) as ion pairs. Nitro benzene (NB) and di-butyl phthalate (DBPH) were used as plasticizing agents in PVC matrix membranes. The specification of sensor based on PMA showed a linear response of a concentration range 1.0 × 10–2 –1.0 × 10–5 M, Nernstian slopes of 17.1-18.86 mV/ decade, detection limit of 7 × 10-5 -9.5 × 10 -7M, pH range 3 – 8 , with correlation coefficients lying between 0.9992 and 0.9976, respectively. By using the ionphore based on PTA gives a concentration range of 1.0 × 10–4 –1.0 × 10–5 M,
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