Batch and Flow-Injection Spectrophotometric Determination of Thymol Using Procaine Hydrochloride as a New Chromogenic Reagent

New, simple and sensitive batch and Flow-injecton spectrophotometric methods for the determination of Thymol in pure form and in mouth wash preparations have been proposed in this study. These methods were based on a diazotization and coupling reaction between Thymol and diazotized procaine HCl in alkaline medium to form an intense orange-red water-soluble dye that is stable and has a maximum absorption at 474 nm. A graphs of absorbance versus concentration show that Beer’s law is obeyed over the concentration range of 0.4-4.8 and 4-80 µg.ml-1 of Thymol, with detection limits of 0.072 and 1.807 µg.ml-1 of Thymol for batch and FIA methods respectively. The FIA procedure sample throughput was 80 h-1. All different chemical and physical experimental parameters that affecting on the development and stability of the colored product were carefully studied and the proposed methods were successfully applied to the determination of Thymol in mouth wash preparations

Flow Injection Spectrophotometric Determination of Thymol using 4-Aminoantipyrine and Copper(II) Nitrate

Flow-injection (FI) spectrophotometric method has been developed for the analysis of thymol in pharmaceutical preparations. The method is based on organic coupling reaction between thymol and 4-amino antipyrine in the presence of alkaline medium to form an intense stable red color complex with copper nitrate that has a maximum absorption at 490 nm. Optimum conditions for determination of the drug was investigated .The calibration graph was linear over the range of 5-500 µg.ml-1 of thymol . The limit of detection (LOD) and limit of quantification (LOQ) were 1.81 ?g mL-1 and 3.60 ?g mL-1 respectively .The proposed method was applied satisfactorily to the determination of thymol in mouth wash preparations. The procedure is characterized by its simplicity, accuracy and precision

Spectrophotometric determination of Phenylephrine hydrochloride and Salbutamol sulphate drugs in pharmaceutical preparations using diazotized Metoclopramide hydrochloride

A spectrophotometric method has been proposed for the determination of two drugs containing phenol group [phenylephrine hydrochloride (PHP) and salbutamol sulphate (SLB)] in pharmaceutical dosage forms. The method is based on the diazotization reaction of metoclopramide hydrochloride (MCP) and coupling of the diazotized reagent with drugs in alkaline medium to give intense orange colored product (?max at 470 nm for each of PHP and SLB). Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. Under the proposed optimum condition, Beer’s law was obeyed in the concentration range of 1-32 and 1-14 ?g mL-1 for PHP and SLB, respectively. The limit of detection (LOD) and limit of quantification (LOQ) for each of PHP and SLB were 0.60, 0.52 ?g mL-1 and 2.02, 1.72 ?g mL-1, respectively. No interference was observed from common excipients present in pharmaceutical preparations. The good correlation coefficients and low relative standard deviation assert the applicability of this method. The suggested method was further applied for the determinations of drugs in commercial pharmaceutical preparations, which was compared statistically with reference methods by means of t- test and F- test and were found not to differ significantly at 95% confidence level. The procedure was characterized by its simplicity with accuracy and precision

Batch and Flow-Injection Spectrophotometric Determination of Procaine HCl in Pharmaceutical Preparations Via Using Diazotization and Coupling Reaction

Simple 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. All different chemical and physical experimental parameters that affecting on the development and stability of the colored product were carefully studied and the proposed methods were applied satisfactorily for the determination of Procaine HCl in an injections samples using the standard addition method

Spectrophotometric Analysis of Vancomycin Hydrochloride in Pure and Pharmaceutical Injections via Batch and Cloud Point Extraction Techniques

تم تطوير تفاعل بسيط وحساس لتقدير هيدروكلوريد الفانكومايسين باستخدام طرائق الدفعة واستخلاص نقطة الغيمة (CPE)   وتعتمد الطريقة الأولى على تكوين صبغة الآزو الناتجة عن تفاعل اقتران الدابسون المؤزوت مع هيدروكلوريد الفانكومايسين في الوسط القاعدي وتم تطوير حساسية هذا التفاعل باستخدام المادة الفعالة غير الأيونية (Triton X-114) وبتقنية نقطة الغيمة. تمت إذابة صبغة الآزو المستخلصة في الطور الغني بمادة الشد السطحي في الإيثانول وقياسها طيفيًا عند الطول الموجي الاعظم 440 نانومتر. تم تقدير التفاعل باستخدام كل من الطرائق الدفعة وطريقةCPE  (أي مع الاستخلاص وبدونه) وتم إجراء مقارنة بسيطة بين الطريقتين. وقد درست جميع الظروف الكيميائية والفيزيائية لطريقتي الدُفعة والاستخلاص بنقطة الغيمة بعناية في ظل الظروف المثلى ، كانت مديات الخطية من 3 إلى 50 و 0.5-25 ميكروغرام. مل-1 لهيدروكلوريد الفانكومايسين بينما كانت حدود الكشف 0.806 و 0.462 ميكروغرام.مل-1 لطريقتي الدفعة و التحليل بالاستخلاص بنقطة الغيمة على التوالي. تمت مقارنة قيم الاستعادية التي تم الحصول عليها مع تلك التي تم الحصول عليها من تطبيق طريقة الأشعة فوق البنفسجية. استخدمت التفنيات المقترحة بفعالية عالية في تقدير الفانكومايسين في الحقن الصيدلانية.  Development of a precise and delicate reaction has been acquired for the determination of vancomycin hydrochloride using batch and cloud point extraction (CPE) methods. The first method is based on the formation of azo dye as a result of diazotized dapsone coupled with vancomycin HCl (VAN) in a basic medium. The sensitivity of this reaction was enhanced by utilizing a nonionic surfactant (Triton X-114) and the cloud point extraction technique (second method). The azo dye formed was extracted into the surfactant-rich phase, dissolved in ethanol and detected at λmax 440 nm spectrophotometrically. The reaction was investigated using both batch and CPE methods (with and without extraction), and a simple comparison between the two developed methods was made. The conditions that affect the extraction process and the sensitivity of the methods have been carefully examined. The linearity of the calibration curves was in the range of 3-50 and 0.5- 25 µg.mL-1 with limits of detection of 0.806 and 0.462 µg.mL-1 for VAN in both batch and CPE procedures, respectively. The percentage of relative standard deviation (R.S.D.%) for the two methods was better than 2.54% and 2.83%, respectively. The recommended procedures have been effectively used to assay VAN in commercial injections

Synthesis and structure determination of new pharmaceutical cocrystals

Pharmaceutical cocrystals have an important and influential role in the pharmaceutical industry through the formation of substitutional crystalline material to obtain the optimum physical properties of an active pharmaceutical ingredient (API) without changing its chemical properties. Pyrazinamide is anti-bacterial drug which is used to treat tuberculosis that infects the lung tissues. In this thesis, the ability of pyrazinamide to form co-crystals with different di-carboxylic acids through the formation of strong hydrogen bonds to form motifs is investigated. Pyrazinamide cocrystals were synthesised through different methods using a variety of different solvents and different starting stoichiometric ratios. New cocrystals were formed between pyrazinamide and glutaric acid (1:1), pyrazinamide and adipic acid (4:1), pyrazinamide and pimelic acid (1:1), and pyrazinamide and sebacic acid (2:1). In all cases, X-ray powder diffraction and NMR were used to characterise the new material formed with the crystal structures of these materials determined through single crystal X-ray diffraction. The crystal structure of a polymorph of azelaic acid was also determined through single crystal X-ray diffraction analysis following attempted synthesis of a pyrazinamide:azelaic acid cocrystal. Other new products were characterised through X-ray powder diffraction, although further structural analysis was not carried out. These include adducts based on pyrazinamide:oxalic acid, pyrazinamide:malonic acid, pyrazinamide:maleic acid, pyrazinamide:isonicotinamide, nicotinamide:isonicotinamide and isonicotinamide:fumaric acid. Attempts to prepare adducts between pyrazinamide with histidine and nicotinamide only resulted in a mixture, as did the combination of L-dopamaine with succinic acid

The Spectrophotometric Determination of Famotidine Drug via Coupling with Diazotized Metochlopramide Hydrochloride

A new, simple and sensitive spectrophotometric method was described for the determination of famotidine (FAM) as a pure material and in pharmaceutical formulation. This method was based on diazotization and coupling reaction between famotidine and diazotized solution of metochlopramide hydrochloride (DMPH) in the presence of phosphate buffer solution to give a compound of azo dye having orange color soluble in water with high absorptivity at a wave length of 478 nm. The data shows that FAM and DMPH combine in the molar ratio of 1:1 at PH 7.0 .The method obeys Beer's law over concentration range of 1-40 ?g.ml-1 of famotidine with a correlation coefficient of 0.9955 and a detection limit of 0.10 ?g.ml-1. The apparent molar absorptivity referred to famotidine has been found to be 2.0 x 104 L. mol-1cm. -1. The proposed method was applied successfully to the assay of famotidine in pharmaceutical preparation

Spectrophotometric Determination of Nitrazepam in Pharmaceutical Tablets by Oxidative Coupling Reaction with Pyrocatechol

A simple and sensitive spectrophotometric method was developed for the determination of nitrazepam (NZP) in pharmaceutical tablets. The method was based on oxidative coupling organic reaction of reduced NZP with pyrocatechol in the presence of ferric sulfate to form red water soluble product with maximum absorbance at 510 nm. The reaction conditions were studied and optimized. The linear range for the determination of NZP, and the detection limit were 1 – 24 ىg mL-1 and 0.698 ىg mL-1, respectively. The proposed method has been applied successfully for the determination of NZP in pharmaceutical tablets. A statistical comparison of these results with those obtained by the British pharmacopoeia procedure using the Student t-test and variance ratio F-test shows a good agreement and indicates no significant difference in accuracy and precision at the 95% confidence

DETERMINATION CADMIUM, LEAD AND ZINC IN HUMAN HAIR BY USING FLAME ATOMIC ABSORPTION SPECTROMETRY (FAAS)

The heavy metals mean serious hazard in environmental pollution. Some of them are vital for many organisms in a low concentration, however the others ought to be poisonous at low concentrations, too. This paper gives an example for the correlation of the attention in human hair and in the environment of different heavy metals. Human hair (n=50) Volunteers (35 males and 15 females) of different age groups between 1 to 57 years samples were collected in Al – Ajailat, Libya. Hair samples were analyzed for heavy metals (Cd, Pb and Zn) by Flame Atomic Absorption Spectrophotometric technique (FAAS). The results showed that the samples concentrations ranged between 0.0001 and 0.3840 mg.kg−1 for cadmium, followed by zinc between 68.99 mg kg−1 and 225mg. kg−1while lead was between 0.632 mg kg−1 and 7.708mg. Kg−1. The results indicated that metal concentrations in male samples varied based on age, such that age group 33-43 years had the highest zinc concentration (206.2±11.6 mg/kg), and age group 1-10 years had the highest Cd (0.384±0.01 mg/kg) and Pb (1.929±0.05 mg/kg) concentrations. while, the cadmium and lead contents in children’s hair samples of both sexes was higher than compared to the values available in some countries. The difference between male and female concentration could be due to individual differences in exposure to heavy metal load as a result of habitual or environmental factors

Four Generations: SUSY and SUSY Breaking

We revisit four generations within the context of supersymmetry. We compute the perturbativity limits for the fourth generation Yukawa couplings and show that if the masses of the fourth generation lie within reasonable limits of their present experimental lower bounds, it is possible to have perturbativity only up to scales around 1000 TeV. Such low scales are ideally suited to incorporate gauge mediated supersymmetry breaking, where the mediation scale can be as low as 10-20 TeV. The minimal messenger model, however, is highly constrained. While lack of electroweak symmetry breaking rules out a large part of the parameter space, a small region exists, where the fourth generation stau is tachyonic. General gauge mediation with its broader set of boundary conditions is better suited to accommodate the fourth generation.Comment: 27 pages, 5 figure