Simple Spectrophotometric Method Research Articles

A Highly Selective and Simple Spectrophotometric Method for the Determination of Zinc at Nano-trace Levels in Some Environmental, Biological, Food, and Pharmaceutical Samples Using 2-hydroxynaphthaldehydebenzoylhydrazone

A simple, ultra-sensitive, and highly selective spectrophotometric method has been established for the trace quantification of zinc (Zn), using 2-hydroxynaphthaldehyde benzoylhydrazone (HNABH). Zn forms a pale yellowish-green complex (maximum absorption at 426 nm) with HNABH (1:1, v:v) in a marginally acidic solution (0.00005-0.00023 M H2SO4). The average molar absorption coefficient and Sandell’s sensitivity were found: 2.87×105 L/mol.cm and 12 ng/cm2 of Zn, respectively. The observed linearity range for Zn was 0.01-50 mg/Lwith a detection limit of 1 µg/L. The analysis of biological, food, and vegetable samples using the suggested method were found to be in tremendous accord with those acquired by Atomic Absorption Spectroscopy (AAS) and Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES). The method has high precision and accuracy (s = ±0.01 for 0.5 mg/L). The limit of quantification of the proposed method was 10 µg/L.

SPECTROPHOTOMETRIC DETERMINATION OF CEFPIROME IN PHARMACEUTICAL PREPARATION

Objective: A simple, sensitive and precise visible spectrophotometric method has been proposed for the determination of cefpirome (CFM) in pure and oral injectable dosage form.
 Methods: A spectrophotometric method is based on the formation of stable red color product by oxidation of drugs by ferric nitrate and subsequent complexation with 1, 10 – phenanthroline with maximum absorption at 515 nm.
 Result: The red color complex was formed between Fe (II) and 1, 10 – phenanthroline after reduction of Fe (III) to Fe (II) in the presence of CFM drug. The phosphoric acid solution was used only for quenching the complex formation reaction. Several parameters such as the maximum wavelength of absorption, the volume of reagents, sequence of addition and effect of temperature and time of heating were optimized to achieve high sensitivity, stability and reproducible results. Under the optimum conditions, linear relationship with good correlation coefficient (0.994) was found over the concentration range from 0.20 to 6.00 μg/mL with a molar extinction coefficient 7.7813 × 104 L/mol/cm, limit of detection 0.2026 and limit of quantification 0.6141 μg/mL, respectively.
 Conclusion: The proposed method was evaluated statistically for linearity, accuracy, and precision in terms of standard deviation, percentage recovery, percentage error and relative standard deviation. The proposed method can be applied for the routine estimation of CFM in the laboratory.

Estimation of In-vitro Plasma Protein Binding of Ampicillin in Horses Based on Spectrophotometric Method

Estimation of plasma protein binding (PPB) is of paramount importance in the pharmacokinetics characterization of drugs, as it can cause significant change in volume of distribution, clearance and half-life of the drug. Ampicillin (α-amino benzyl penicillin) is most commonly used drug in equine practice. This study was conducted to determine the extent of PPB of ampicillin in apparently healthy horses (n=6). A simple spectrophotometric method was applied for the determination of ampicillin at 320 nm wavelength, based on acid degradation product of penicillin at 75°C in presence of citrate buffer (pH 5.2) and traces of copper salt. In the study, it was observed that this method permits the detection of ampicillin to a level not beyond 1.0 μg/ml. Various concentrations of ampicillin (3.125, 6.25, 12.5, 25, 50, 100 μg/ml) were prepared in triplicate in pooled plasma collected from healthy animals. In vitro binding of ampicillin to plasma proteins was determined by employing the equilibrium dialysis technique. The study revealed that the plasma protein binding of ampicillin was to the extent of 12.8 ± 0.07%. Binding capacity of ampicillin to plasma protein (βi) and dissociation rate constant of protein-drug complex (Kβ) in the present study were 0.34 × 10−6 ± 0.02 × 10−6 mol.gm−1 and 0.003 × 10−9 ± 0.0003 × 10−9 mol, respectively in horses. Hence, the study concluded that usage of spectrophotometric method helps in quick, cost effective and efficient results in estimation of PPB for ampicillin.

An innovative spectrophotometric method for determination of polidocanol in pharmaceutical ampoules using phase equilibrium measurements

A simple spectrophotometric method was developed for determination of the challenging surface active non-chromophoric pharmaceutical product; polidocanol (PD). The assay principle depends on the ability of PD to form a ternary complex with the tetrahedral cobalt (II)-thiocyanate blue complex, due to the poly(ethylene oxide) group. The hydrophobic chain in PD allows the formed ternary complex to be extracted in the dichloromethane layer, which turns blue after addition of PD and shaking. The absorbance of the extracted ternary complex can be monitored to measure the concentration of PD. The proposed method was found selective and suitable for determination of PD in pharmaceutical dosage forms, with no interference from excipients. The different factors that may affect the method sensitivity were studied, including the type of extractant, the wavelength, the complex concentration, the mixing and the extraction time. The maximum sensitivity was attained when the absorbance was measured at 320 nm using dichloromethane as an extractant, and 3 M of ammonium thiocyanate mixed with PD for 2 min and extracted for 2 min. The developed method was validated according to the ICH guidelines, the calibration curve was constructed with a correlation coefficient of 0.999 in a concentration range of 50–400 µg/mL. The method was able to specifically detect and quantify PD in bulk with a %recovery 100.55% ± 0.29 and in its commercial dosage form with a %recovery of 100.30 ± 1.04.

Determination of Rhodamine B and Rhodamine 6G dyes in Various Ink Samples by Zero Crossing Method: First Derivative Spectrophotometry

A simple spectrophotometric method has been developed for resolving binary mixtures of Rhodamine B and Rhodamine 6G dyes of red ballpoint pen ink using the first-derivative spectra with measurements at zero-crossing wavelengths. Calibration graphs were linear up to 8 mg L-1 for Rhodamine B and 10 mg L-1 for Rhodamine 6G. This method was successfully applied for the quantitative determination of dyes having overlapping spectra in their bi-component mixtures. The applied derivative method is practical, simple, rapid, inexpensive and suitable for quantitative analysis of bi-component dye solutions in the ballpoint pen ink.

UV-SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION FOR ESTIMATION OF IPRATROPIUM BROMIDE IN API AND PHARMACEUTICAL DOSAGE FORM

Objective: The current work intended towards the developed and validated by using Simple, rapid, sensitive, precise and specific method UV Spectrophotometric method for the estimation of Ipratropium bromide in API and pharmaceutical formulation.
 Methods: Water used as a solvent and the absorbance of the drug was measured at the absorbance’s maxima of Ipratropium bromide λmax is 214 nm.
 Result: Calibration curve plotted in concentration range 20-120µg/ml exhibit the linearity relationship with line equation y=0.0062x+0.3161 and r2=0.995. The Accuracy was found to be 99.5-100.1%, the precision %RSD= 0.12888-0.30533, and the LOD and LOQ is 8.78266-28.5881. The method was found to comply with all the validation parameters as per ICH guidelines indicating the sensitivity of the method towards analyte.
 Conclusion: The method can be used satisfactory for the routine analysis of Ipratropium Bromide present in API and Pharmaceutical dosage form.

Rapid and Simple Spectrophotometric Method for the Determination of Antiviral and Anti-Parkinsonism Drugs

A rapid and sensitive spectrophotometric method has been developed for the quantitative analysis of three antiviral, anti-parkinsonism drugs, namely, amantadine (AMA), memantine (MET), and rimantadine (RIM). The method is based on the usage of 1,3-indandione (IDO) as a chromogenic reagent to form charge transfer complexes with the studied drugs and produce colored reaction products with an absorbance maximum at 522 nm, allowing quantitative analysis of these drugs. In addition, the study was validated according to the official guidelines that permits usage in quality control laboratories. Many factors (reagent volume, diluting solvent, temperature, reaction and stability time) influencing the reactions were studied and optimized. The results showed that this method is able to detect AMA, MET, or RIM over a linear range between 10–140 μg/mL with high selectivity and robustness. Furthermore, the study results were applied to analyze the drugs in their pharmaceutical preparations with acceptable accuracy and precision.

A simple spectrophotometric method for rapid quantitative screening of arsenic bio-transforming bacteria

Abstract A simple spectrophotometric technique for inorganic arsenic speciation of known total arsenic has been developed for application in quantitative screening of arsenite-oxidizing and arsenate-reducing bacteria from the wide range of environmental isolates. The technique is based on the spectrophotometric absorbance measurement of the color intensity in the arsenic and potassium permanganate mixture. Since arsenate does not react with potassium permanganate, the intensity of color decreases proportionately with the increasing concentration of arsenite in the total arsenic. The speciation method can be used over a pH range of 4–9. The validity of the results obtained from this spectrophotometric method was confirmed with the Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry (LC-ICP-MS). This method has great potential for the screening of arsenite-oxidizing bacteria.

A Simple Spectrophotometric Method for Determination of Glyoxylic Acid in Its Synthesis Mixture.

A new simple and reliable spectrophotometric method is described to determine glyoxylic acid in its synthesis reaction mixture containing oxalic acid, glycolic acid, acetic acid, glyoxal, and ethylene glycol by means of a modified Hopkins–Cole reaction between glyoxylic acid and tryptophan in presence of ferric chloride and concentrated sulphuric acid. The linear range of glyoxylic acid concentration is 0–0.028 M. The limits of detection (LOD) and quantitation (LOQ) are 0.0019 M and 0.00577 M, respectively. The LOD, LOQ, standard deviation, relative standard deviation, and recovery ratio of the proposed method are comparable with a selected HPLC reference method. Both methods displayed same precision and credibility. Reaction stoichiometry between tryptophan and glyoxylic acid is assumed to be 2 : 3. Reaction mechanism has been postulated based on identified molar ratios of reactants. Glyoxal gave a negative test with tryptophan although it is a dialdehyde.

DEVELOPMENT AND VALIDATION OF UV SPECTROPHOTOMETRICMETHOD FOR QUANTITATIVE ESTIMATION OF GLIPIZIDEIN PHARMACEUTICAL DOSAGE FORM

Objective: The present work is aimed to develop a simple, rapid, selective and economical UV spectrophotometric method for quantitative determination of Glipizideinbulk and pharmaceutical dosage form.
 Methods: In this method Dimethyl Form amide (DMF) was used as solvent, the absorption maxima was found to be275 nm in DMF. The developed method was validated for linearity, accuracy, precision, ruggedness, robustness, LOD and LOQ in accordance with the requirements of ICH guideline.
 Results: The linearity was found to be 10-60 µg/ml having linear equation y=0.017x-0.006 with correlation coefficient of 0.997. The% recovery was found to be in the range of 98.7-100%. The % RSD for intra-day and inter-day precision was found to be 0.569923 and 0.40169 respectively. The limit of detection (LOD) and limit of quantification (LOQ) was found to be3.06 µg/ml and 9.27 µg/ml respectively.
 Conclusion: The developed method was validated as per ICH Q2(R1) guidelines. The novel method is applicable for the analysis of bulk drug in its pharmaceutical dosage form.

VISIBLE SPECTROPHOTOMETRIC METHOD DEVELOPMENT AND VALIDATION OF IMATINIB IN BULK AND FORMULATION

Objective: A new, simple, sensitive, precise and reproducible UV visible spectrophotometric method was developed for the determination of Imatinib in pharmaceutical formulations with alizarin.
 Methods: The method is based on formation of yellow-colored complex. The UV spectrum of Imatinib in methanol showed λ max at 431 nm. Beer’s law is valid in the concentration range of 10-70 μg/ml. This method was validated for linearity, accuracy, precision, ruggedness and robustness.
 Results: The method has demonstrated excellent linearity over the range of 10-70 μg/ml with regression equation y =0.013x-0.017 and regression correlation coefficient r2= 0.997. Moreover, the method was found to be highly sensitive with LOD (4.3μg/ml) and LOQ (13.07μg/ml).
 Conclusion: Based on results the proposed method can be successfully applied for the assay of Imatinib in various pharmaceutical dosage forms.

A novel spectrophotometric method for simultaneous estimation of dibenzothiophene and 2-hydroxybiphenyl in their mixed spectrum and its application in screening of specific biodesulfurizing microbes.

The desulfurization of fuel is currently enforced to meet environmental legislation and prevent pollution. The use of specific biodesulfurizing microbes with a unique 4S pathway allows the desulfurization without compromising the quality of fuel. These specific microbes can be screened by the detection of 2-hydroxybiphenol (2-HBP) in desulfurizing mixture of dibenzothiophene (DBT). At present, colorimetric Gibb's assay is the most commonly employed screening method which requires a specific reagent, i.e., 2,6-dichloroquninone-4-chloramide. In the present study, a novel and simple spectrophotometric method was developed for the detection of 2-HBP for screening purpose based on dual wavelength method. The developed method facilitates the simultaneous analysis of DBT desulfurization and 2-HBP production in a sample by merely measuring the absorbance differences at two specified wavelengths, i.e., ΔA (λ 320-λ 247) for DBT and ΔA (λ 286-λ 324) for 2-HBP. The developed method was used to screen 57 microbes and two specific desulfurizing microbes Bacillus flexus MS-5 and Bacillus cereus BR-31 were selected based on 2-HBP production. The outcomes of developed method were validated by HPLC analysis. The strains MS-5 and BR-31 were employed in biodesulfurization and resulted in 54.88 ± 1.12% and 55.72 ± 1.32% desulfurization of 1.0mM DBT, respectively. The developed method for screening of specific desulfurizing microbes does not require any specific reagent or sophisticated instrument in spite of being quick and reliable. The microbes selected by developed method exhibited excellent potential for biodesulfurization of fuel.

A simple spectrophotometric method to determine phytic acid in poultry wastewater without acid digestion

ABSTRACT Frequently, wastewater from treatment plants associated with animal husbandry, mainly animal feeding operations, are used to irrigate near agricultural lands based on nitrogen requirements. To avoid soil phosphorus accumulation owing to its long-term application, it is necessary to achieve lower levels of total phosphorus; one of the methods involve eliminating dissolved organic phosphorus (DOP) in treatment systems. The DOP in effluents and manure wastewater streams is commonly quantified without the identification of individual phosphorus species. Nevertheless, characterisation of the DOP is particularly important, because removal techniques, as well as soil sorption capacity and phosphorus transfer in the runoff to water bodies, differ for different DOP compounds. Particularly, phytic acid (PA), the main DOP compound in animal wastes, can strongly bind to soils making it unavailable for plant uptake. This work evaluates the application of a simple analytical procedure to the determination of the PA concentration in manure wastewater. The method does not require a prior acid digestion stage; in addition, sample colour removal, as well as the removal of potentially interfering compounds are not required. The results are in agreement with results obtained using 31P NMR. PA recoveries ranged between 87% and 97%, relative standard deviation was <8.5%, while the limits of detection and quantification for phosphorus as PA were 0.18 mg·L−1 and 0.55 mg·L−1 respectively.

New simple spectrophotometric method for the specification of silver (i) in oil-water samples

A simple, highly selective and non-extractive spectrophotometric method for the specification of trace amounts silver (I) has been developed. In the water media 2,2’-di (2,3,4-trihydroxy-phenylazo) biphenyl reacts with the silver to give a highly absorbent greenish-yellow chelate in a molar ratio 2:1 (Ag:R). The reaction is instantaneous, the maximum absorption was obtained at 540 nm and remains stable for 24 hours. The average molar absorptivity and Sandell’s sensitivity were 4.3×104 l mol-1 cm-1 and 5.0 mkg cm-2 of silver (I), respectively. Linear calibration graphs were obtained for 0.1–30 mkgml−1 of silver (I), respectively. A large excess of over 30 cations, anions and complex agents do not interfere in the specification. The method is highly selective for silver and was successfully appliedin a number of oilwater samples. It has high precision and accuracy (s = ± 0.01 for 0.5 mkgl-1). Therefore, it may be used for monitoring to establish trace level of silver (I) in difficult matrices of oilwater samples.

Spectrophptometric Analysis of Clathromycin with Tpooo, Ars and WFB

One simple and sensitive procedure (simple spectrophotometric method) for the assay of drug clarithromycin in pure form and formulations. This method involves the formation of ion-association complex between CAM and the TPOOO, ARS and WFB. In order to establish the optimum conditions necessary for rapid and quantitative formation of coloured product with maximum stability and sensitivity, the author performed experiments by measuring the absorbance at λmax 480nm,420nm and580nm of respective series of solutions, varying one and fixing the other parameters in each case such as type, volume and concentration of acid, organic solvent used for extraction, ratio of organic phase to aqueous phase during extraction, shaking time and temperature. The variable parameters were optimized. The results were statistically validated.

Isoabsorptive Point Method for Simultaneous Determination of Paracetamol and Orphenadrine Citrate in Their Combined Pharmaceutical Dosage Forms

A simple, specific, accurate and precise spectrophotometric method was settled for simultaneous determination of paracetamol and orphenadrine citrate in their pure form and in their pharmaceutical formulation. Isoabsorptive point technique has been used in simultaneous determination of both drugs without prior separation. Isoabsorptive point method parameters were validated according to ICH guidelines in which accuracy, precision, repeatability and robustness were found in accepted limits. Advantages and disadvantages of Isoabsorptive point were discussed and statistical comparison between the proposed method and the reference one was also performed.

Spectrophotometric determination of Sulfasalazine drug in pure and Pharmaceutical preparation using sodium 1, 2-naphthoquinone-4-sulfonate (NQS) reagent

A simple spectrophotometric method was developed to determine the sulfasalazine drug. The method based on the reaction between sodium 1, 2-naphthoquinone-4-sulfonate (NQS) regent with the amino group in the sulfasalazine drug. Maximum absorption of the product was recorded at 456 nm. Beer’s law was obeyed within the concentration range (1-25) ×10−5 M. The molar absorptivity was 1.438 ×104 L. mole−1. cm−1. Molar ratio and Job’s methods revealed that the ratio between the sulfasalazine drug and NQS reagent is 1:1. Average recovery, relative standard deviation (RSD), limit of quantitation (LOQ) and limit of detection (LOD) were 103.6011%, 0.6072%, 0.0273 and 0.0911 M, respectively. The suggested method was also applied to the sulfasalazine tablets (pharmaceutical preparation).

Microdetermination of Palladium(II) using 6-Chloro-3-hydroxy-7-methyl-2-(2′-thienyl)-4-oxo-4H-1-benzopyran

A simple, rapid, sensitive and selective extractive spectrophotometric method is developed for the trace determination of palladium(II) from NaHCO3 medium using 6-chloro-3-hydroxy-7-methyl-2- (2′-thienyl)-4-oxo-4H-1-benzopyran (CHMTB) as a colouring agent. The proposed metal complex can be quantitatively extracted into ethyl acetate and absorbs maximum in the wavelength range 415-426 nm. The 1:1 yellow complex obeys linearity over the Pd(II) concentration range of 0-2.6 μg mL-1; the correlation coefficient being 0.9998. The molar annihilation coefficient and Sandell′s sensitivity when applying spectrophotometric determination at 420 nm, were 6.173 × 104 L mol-1 cm-1 and 0.0017 μg Pd(II) cm-2, respectively. The proposed method is free from the interference of Os(VIII), Cr(VI), Mo(VI), V(V), Nb(V), Ce(IV), Se(IV), Zr(IV), Pt(IV), Ru(III), Ir(III) and Fe(III) . The method was effectively applied to the determination of Pd(II) in various samples including palladium charcoal catalyst and water

Development of Rapid Colorimetric Assay for Detection of Gluconic Acid Using Iron(Ⅱ) and Indigo Carmine

In this work, a simple and rapid spectrophotometric method, which is based on the fact that Iron(Ⅱ) -gluconic acid complex as a kind of reducing agent deterioration of indigo carmine dyes, was developed to detect gluconic acid in food. Under the optimal experimental condition, a linear range of 3.6 M to 900 M was obtained for gluconic acid with a limit of detection of 1.1 μM. The colorimetric method was rapid and robust with a low cost and can be applied to gluconic acid detection in food samples.

Development, Validation and Application on Seized materials by UV Spectrophotometric Method for the determination of a Solid Semi-legal Drug: Tramadol Hydrochloride Case

The present study describes development and validation of simple, fast, non-toxic and economic UV spectrophotometric method for the determination of Tramadol Hydrochloride in bulk, capsules and tablet dosage form using absorbance maxima method. Solubility studies indicated that a Tramadol Hydrochloride shows good solubility in proposed diluent solution as compared to solubility in hydrochloride acid and the λmax of Tramadol Hydrochloride was found to be 271 nm. Distilled water, was selected like diluent with λmax at 271 nm and the high peak time was found to be 20 min. The developed method was validated for linearity, precision, accuracy. The LOD and LOQ were calculated as per protocol for the validation of a method of analysis in chemistry guidelines, they are respectively be 0.177 μg mL-1 and 0.592 μg mL-1. This proposed method was found to be linear with R2 = 0.9996 in the concentration range of 1–120 μg/ml. It is reproducible in this range and can be used in case of possible Tramadol seizures or quality controls. In all cases like intraday and Interday, the % RSD were less than 2. The ratio of similarly was found to be 5.71. The standard was found to be 100%. The present method was found to be simple, linear, precise, accurate and sensitive, and can be used for in laboratories for the quantitative analysis. It also can be preferred because of cost-effectiveness, non-toxicity and could be compared to other UV spectrophotometric validated methods.