scholarly journals Chemometric Methods for the Simultaneous Determination of Some Water-Soluble Vitamins

2011 ◽  
Vol 94 (2) ◽  
pp. 467-481 ◽  
Author(s):  
Abdel-Maaboud I Mohamed ◽  
Horria A Mohamed ◽  
Niveen A Mohamed ◽  
Marwa R El-Zahery
Keyword(s):  
Correlation Coefficients ◽  
Water Soluble ◽  
Multivariate Methods ◽  
Linear Calibration ◽  
Principal Components Regression ◽  
Regression Methods ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Accuracy And Precision

Abstract Two spectrophotometric methods, derivative and multivariate methods, were applied for the determination of binary, ternary, and quaternary mixtures of the water-soluble vitamins thiamine HCl (I), pyridoxine HCl (II), riboflavin (III), and cyanocobalamin (IV). The first method is divided into first derivative and first derivative of ratio spectra methods, and the second into classical least squares and principal components regression methods. Both methods are based on spectrophotometric measurements of the studied vitamins in 0.1 M HCl solution in the range of 200500 nm for all components. The linear calibration curves were obtained from 2.590 g/mL, and the correlation coefficients ranged from 0.9991 to 0.9999. These methods were applied for the analysis of the following mixtures: (I) and (II); (I), (II), and (III); (I), (II), and (IV); and (I), (II), (III), and (IV). The described methods were successfully applied for the determination of vitamin combinations in synthetic mixtures and dosage forms from different manufacturers. The recovery ranged from 96.1 1.2 to 101.2 1.0 for derivative methods and 97.0 0.5 to 101.9 1.3 for multivariate methods. The results of the developed methods were compared with those of reported methods, and gave good accuracy and precision.

scholarly journals Extractive Spectrophotometric Methods for Determination of Zolmitriptan in Tablets

2007 ◽  
Vol 90 (5) ◽  
pp. 1237-1241 ◽  
Author(s):  
Zeynep Aydogmus ◽  
Ipek Inanli
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Bromothymol Blue ◽  
Chromatography Method ◽  
Statistical Comparison ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Liquid Chromatography Method ◽  
Comparison Of The Results

Abstract Two simple and sensitive extractive spectrophotometric methods have been developed for determination of zolmitriptan (ZTP) in tablets. These methods are based on the formation of yellow ion-pair complexes between ZTP and tropaeolin OO (TPOO) and bromothymol blue (BTB) in citratephosphate buffer of pH 4.0 and 6.0, respectively. The formed complexes were extracted with dichloromethane and measured at 411.5 and 410 nm for TPOO and BTB, respectively. The best conditions of the reactions were studied and optimized. Beer's law was obeyed in the concentration ranges of 220 and 1.517 g/mL with molar absorptivities of 1.42 104 and 1.60 104 L/mol/cm for the TPOO and BTB methods, respectively. Correlation coefficients were 0.9998 and 0.9999 for TPOO and BTB methods, respectively. Limits of detection of the TPOO and BTB methods were 0.341 and 0.344 g/mL, respectively, and the limits of quantitation were 1.034 and 1.051 g/mL, respectively. Sandell's sensitivity and stability constant were also calculated. The proposed methods have been applied successfully for the analysis of the drug in its dosage forms. No interference was observed from excipients present in tablets. Statistical comparison of the results with those obtained by a high-performance liquid chromatography method showed excellent agreement and indicated no significant differences in accuracy and precision.

Spectrofluorimetric Determination of Some Water-Soluble Vitamins

2011 ◽  
Vol 94 (6) ◽  
pp. 1758-1769 ◽  
Author(s):  
Abdel-Maaboud I Mohamed ◽  
Horria A Mohamed ◽  
Niveen M Abdel-Latif ◽  
Marwa R Mohamed
Keyword(s):  
Water Soluble ◽  
Good Precision ◽  
Linear Calibration ◽  
Reaction Conditions ◽  
Pharmaceutical Dosage Forms ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Spectrofluorimetric Determination ◽  
Comparison Of The Results

Abstract Two simple and sensitive spectrofluorimetric methods were developed for determination of three water-soluble vitamins (B1, B2, and B6) in mixtures in the presence of cyanocobalamin. The first one was for thiamine determination, which depends on the oxidation of thiamine HCl to thiochrome by iodine in an alkaline medium. The method was applied accurately to determine thiamine in binary, ternary, and quaternary mixtures with pyridoxine HCl, riboflavin, and cyanocobalamin without interference. In the second method, riboflavin and pyridoxine HCl were determined fluorimetrically in acetate buffer, pH 6. The three water-soluble vitamins (B1, B2, and B6) were determined spectrofluorimetrically in binary, ternary, and quaternary mixtures in the presence of cyanocobalamin. All variables were studied in order to optimize the reaction conditions. Linear relationship was obeyed for all studied vitamins by the proposed methods at their corresponding λexc or λem. The linear calibration curves were obtained from 10 to 500 ng/mL; the correlation ranged from 0.9991 to 0.9999. The suggested procedures were applied to the analysis of the investigated vitamins in their laboratory-prepared mixtures and pharmaceutical dosage forms from different manufacturers. The RSD range was 0.46–1.02%, which indicates good precision. No interference was observed from common pharmaceutical additives. Good recoveries (97.6 ± 0.7–101.2 ± 0.8%) were obtained. Statistical comparison of the results with reported methods shows excellent agreement and indicates no significant difference in accuracy and precision.

Validated Stability-Indicating Spectrophotometric Methods for the Determination of Cefixime Trihydrate in the Presence of its Acid and Alkali Degradation Products

2015 ◽  
Vol 98 (1) ◽  
pp. 35-45 ◽  
Author(s):  
Nadia M Mostafa ◽  
Laila Abdel-Fattah ◽  
Soheir A Weshahy ◽  
Nagiba Y Hassan ◽  
Shereen A Boltia
Keyword(s):  
Degradation Product ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Regression Equations ◽  
Acid Degradation ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
Accuracy And Precision ◽  
Significant Difference

Abstract Five simple, accurate, precise, and economical spectrophotometric methods have been developed for thedetermination of cefixime trihydrate (CFX) in the presence of its acid and alkali degradation products without prior separation. In the first method, secondderivative (2D) and first derivative (1D) spectrophotometry was applied to the absorption spectra of CFX and its acid (2D) or alkali (1D) degradation products by measuring the amplitude at 289 and 308 nm, respectively. The second method was a first derivative (1DD) ratio spectrophotometric method where the peak amplitudes were measured at 311 nm in presence of the acid degradation product, and 273 and 306 nm in presence of its alkali degradation product. The third method was ratio subtraction spectrophotometry where the drug is determined at 286 nm in laboratory-prepared mixtures of CFX and its acid or alkali degradation product. The fourth method was based on dualwavelength analysis; two wavelengths were selected at which the absorbances of one component were the same, so wavelengths 209 and 252 nm were used to determine CFX in presence of its acid degradation productand 310 and 321 nm in presence of its alkali degradation product. The fifth method was bivariate spectrophotometric calibration based on four linear regression equations obtained at the wavelengths 231 and 290 nm, and 231 and 285 nm for the binary mixture of CFX with either its acid or alkali degradation product, respectively. The developed methods were successfully applied to the analysis of CFX in laboratory-prepared mixtures and pharmaceutical formulations with good recoveries, and their validation was carried out following the International Conference on Harmonization guidelines. The results obtained were statistically compared with each other and showed no significant difference with respect to accuracy and precision.

scholarly journals Three Different Spectrophotometric Methods for Simultaneous Determination of Pyriproxyfen and Chlorothalonil Residues in Cucumber and Cabbage Samples

2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre
Keyword(s):  
Simultaneous Determination ◽  
Simultaneous Estimation ◽  
Zero Crossing ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
The Third ◽  
Mean Centering ◽  
Relative Standard ◽  
One Way Anova

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.

scholarly journals Uv Spectrophotometric Methods for Determination of Sofosbuvir in Pure Form and Pharmaceutical Dosage Forms in Presence of Its Alkaline Degradate

2020 ◽  
pp. 12-25
Author(s):  
Zeinab Adel Nasr ◽  
Noha S. Said ◽  
Sawsan A. Abdel-Razeq
Keyword(s):  
Good Accuracy ◽  
Dosage Forms ◽  
Difference Spectra ◽  
Pharmaceutical Dosage Forms ◽  
Spectrophotometric Methods ◽  
Good Linearity ◽  
Ratio Difference ◽  
Accuracy And Precision ◽  
Tablet Dosage

Aims: Two spectrophotometric methods were developed and validated for the determination of sofosbuvir in presence of its alkaline degradate. Study Design: Ratio difference and ratio derivative methods were assisted for determination of sofosbuvir in presence of its alkaline degradate, laboratory-prepared mixtures and in tablet dosage forms. Place and Duration of Study: Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy (Girls), Al - Azhar University, between December 2019 and January 2020. Methodology: Two analytical methods were achieved and validated for the quantitative determination of Sofosbuvir in presence of its alkaline degradate. The first method was ratio difference (RD) method, where the UV absorption spectra of different concentrations of sofosbuvir were divided by the spectrum of a certain concentration (15 µg mL-1) as a devisor of its alkaline degradate to get the ratio difference spectra. Afterwards, the peak amplitudes difference between 253.7 and 243.5 nm were measured. The second method was the ratio derivative (1DR) method, where the first derivative of the ratio spectra (1DR) was obtained and its amplitude was measured at 247 and 268 nm. Good linearity was obtained over the concentration range of 3-15 µg mL-1 for the proposed methods. The proposed procedures were adopted for the selective determination of intact Sofosbuvir in presence of up to 80% of its degradation product. Sofosbuvir was exposed to different conditions as alkaline, acidic and oxidative degradation. Results: The proposed methods were developed and validated with good linearity range of 3-15 µg mL-1 for both methods, and also with good accuracy and precision. And the obtained results were statistically compared to those obtained by the reported method. Conclusion: Sofosbuvir was successfully determined by the proposed ratio difference and ratio derivative methods in bulk powder, laboratory prepared mixtures and tablet dosage form with good accuracy and precision. The methods were validated according to ICH guidelines. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals Determination of Two Antibacterial Binary Mixtures by Chemometrics-Assisted Spectrophotometry

2007 ◽  
Vol 90 (1) ◽  
pp. 128-141 ◽  
Author(s):  
Abd El-Maaboud I Mohamed ◽  
Osama H Abdelmageed ◽  
Ibrahim H Refaat
Keyword(s):  
Binary Mixtures ◽  
Colorimetric Method ◽  
Correlation Coefficients ◽  
Dosage Forms ◽  
Considerable Degree ◽  
Zero Crossing ◽  
First Derivative ◽  
Beer's Law ◽  
Beer’S Law

Abstract Simple chemometrics-assisted spectrophotometric methods are described for determination of 2 antibacterial binary mixtures. The mixtures are composed of norfloxacin in combination with tinidazole and erythromycin (as ethylsuccinate ester or stearate salt) in combination with trimethoprim. The normal UV absorption spectra of each pair of drugs in the studied mixtures, in the range of 200-400 nm, showed a considerable degree of spectral overlapping: 77.5% for the norfloxacintinidazole mixture and 84.3% for the erythromycintrimethoprim mixture. Resolution of the norfloxacintinidazole mixture and trimethoprim in the presence of erythromycin was accomplished successfully by using zero-crossing first derivative (1D), classical least-squares (CLS) regression analysis, and principal component regression (PCR) analysis methods. In addition, an alternative simple and accurate colorimetric method was developed for the determination of erythromycin in the presence of trimethoprim using 2,4-dinitrophenylhydrazine. All variables affecting the development of the colored chromogen were studied and optimized, and the product was measured at 526-529 and 538-542 nm for erythromycin stearate and erythromycin ethylsuccinate, respectively. For zero-crossing, first derivative technique Beer’s law was obeyed in the general concentration range of 250 μg/mL for norfloxacin, tinidazole, and trimethoprim with good correlation coefficients (0.9994-0.9996). Overall limits of detection (LOD) and quantification (LOQ) ranged from 0.59 to 2.81 and 1.96 to 9.33 μg/mL, respectively. The obtained results from CLS and PCR were compared with those obtained from a 1D spectrophotometric method. With the exception of erythromycin, overall recoveries in the average range of 97.33-103.0% were obtained with a considerable degree of accuracy when the suggested methods were applied to analysis of synthetic binary mixtures, some commercial dosage forms such as tablets and oral suspension without interference from the commonly encountered excipients and additives. For the colorimetric method, Beer's law was obeyed in the general concentration range of 7.21-28.84 μg/mL erythromycin with good correlation coefficients (0.9980-0.9996). Overall LOD and LOQ ranged from 0.73 to 1.65 and 2.43-5.49 μg/mL, respectively. Erythromycin derivatives were determined in the commercial dosage form, without interference from trimethoprim-encountered excipients and additives. The obtained results, with both chemometric and colorimetric methods, have been compared with those obtained from reported methods, and proper F- and t-values were observed, indicating no significant difference between the results of the suggested methods and reported method(s). The good percentage recoveries and proper statistical data obtained proved the efficiency of the proposed procedures for the determination of the studied drugs in their binary mixtures as well as in the commercial dosage forms with quite satisfactory precision.

Spectrophotometric Methods for Simultaneous Determination of Sofosbuvir and Ledipasvir (HARVONI Tablet): Comparative Study with Two Generic Products

2017 ◽  
Vol 100 (4) ◽  
pp. 976-984 ◽  
Author(s):  
Nisreen F Abo-Talib ◽  
Mohamed R El-Ghobashy ◽  
Marwa H Tammam
Keyword(s):  
Dosage Form ◽  
Drug Dosage ◽  
Spectrophotometric Methods ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Drug Dosage Form ◽  
Generic Products ◽  
Third Derivative ◽  
Combination Pill

Abstract Sofosbuvir and ledipasvir are the first drugs in a combination pill to treat chronic hepatitis C virus. Simple, sensitive, and rapid spectrophotometric methods are presented for the determination of sofosbuvir and ledipasvir in their combined dosage form. These methods were based on direct measurement of ledipasvir at 333 nm (due to the lack of interference of sofosbuvir) over a concentration range of 4.0–14.0 µg/mL, with a mean recovery of 100.78 ± 0.64%. Sofosbuvir was determined, without prior separation, by third-derivative values at 281 nm; derivative ratio values at 265.8 nm utilizing 5.0 µg/mL ledipasvir as a divisor; the ratio difference method using values at 270 and 250 nm using 5.0 µg/mL ledipasvir as a divisor; and the ratio subtraction method using values at 261 nm. These methods were found to be linear for sofosbuvir over a concentration range of 5.0–35.0 µg/mL. The suggested methods were validated according to International Conference on Harmonization guidelines. Statistical analysis of the results showed no significant difference between the proposed methods and the manufacturer's LC method of determination with respect to accuracy and precision. These methods were used to compare the equivalence of an innovator drug dosage form and two generic drug dosage forms of the same strength.

scholarly journals Liquid Chromatographic and Spectrophotometric Determination of Diflucortolone Valerate and Isoconazole Nitrate in Creams

2011 ◽  
Vol 94 (1) ◽  
pp. 128-135 ◽  
Author(s):  
Elif Karacan ◽  
Mehmet Gokhan Çaġlayan ◽  
İsmail Murat Palabiyik ◽  
Feyyaz Onur
Keyword(s):  
Principal Component Regression ◽  
Principal Component ◽  
Derivative Spectrophotometry ◽  
Data Matrix ◽  
Concentration Data ◽  
Spectrophotometric Methods ◽  
First Derivative ◽  
First Derivative Spectrophotometry ◽  
Liquid Chromatographic

Abstract A new RP-LC method and two new spectrophotometric methods, principal component regression (PCR) and first derivative spectrophotometry, are proposed for simultaneous determination of diflucortolone valerate (DIF) and isoconazole nitrate (ISO) in cream formulations. An isocratic system consisting of an ACE® C18 column and a mobile phase composed of methanol–water (95+5, v/v) was used for the optimal chromatographic separation. In PCR, the concentration data matrix was prepared by using synthetic mixtures containing these drugs in methanol–water (3+1, v/v). The absorbance data matrix corresponding to the concentration data matrix was obtained by measuring the absorbances at 29 wavelengths in the range of 242–298 nm for DIF and ISO in the zero-order spectra of their combinations. In first derivative spectrophotometry, dA/dλ values were measured at 247.8 nm for DIF and at 240.2 nm for ISO in first derivative spectra of the solution of DIF and ISO in methanol–water (3+1, v/v). The linear ranges were 4.00–48.0 μg/mL for DIF and 50.0–400 μg/mL for ISO in the LC method, and 2.40–40.0 μg/mL for DIF and 60.0–260 μg/mL for ISO in the PCR and first derivative spectrophotometric methods. These methods were validated by analyzing synthetic mixtures. These three methods were successfully applied to two pharmaceutical cream preparations.

scholarly journals Development and Validation of Spectrophotometric Methods for Determination of Fluoxetine, Sertraline, and Paroxetine in Pharmaceutical Dosage Forms

2005 ◽  
Vol 88 (1) ◽  
pp. 38-45 ◽  
Author(s):  
Ibrahim A Darwish
Keyword(s):  
Correlation Coefficients ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Factors Affecting ◽  
Spectrophotometric Methods ◽  
Linear Relationships ◽  
Relative Standard ◽  
Optimum Reaction ◽  
Standard Deviations

Abstract Three simple and sensitive spectrophotometric methods were developed and validated for determination of the hydrochloride salts of fluoxetine, sertraline, and paroxetine in their pharmaceutical dosage forms. These methods were based on the reaction of the N-alkylvinylamine formed from the interaction of the free secondary amino group in the investigated drugs and acetaldehyde with each of 3 haloquinones, i.e., chloranil, bromanil, and 2,3-dichloronaphthoquinone, to give colored vinylamino-substituted quinones. The colored products obtained with chloranil, bromanil, and 2,3-dichloronaphthoquinone exhibit absorption maxima at 665, 655, and 580 nm, respectively. The factors affecting the reactions were studied and optimized. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.9986–0.9999) were found between the absorbances and the concentrations of the investigated drugs in the range of 4–120 μg/mL. The limits of detection for the assays ranged from 1.19 to 2.98 μg/mL. The precision values of the methods were satisfactory; the relative standard deviations were 0.56–1.24%. The proposed methods were successfully applied to the determination of the 3 drugs in pure and pharmaceutical dosage forms with good accuracy; the recoveries ranged from 99.1 to 101.3% with standard deviations of 1.15–1.92%. The results compared favorably with those of reported methods.

scholarly journals Use of N, N-diethyl-p-phenylenediamine sulphate for the spectrophotometric determination of some phenolic and amine drugs

2010 ◽  
Vol 60 (2) ◽  
pp. 217-227 ◽  
Author(s):  
Padmarajaiah Nagaraja ◽  
Ashwinee Shrestha ◽  
Anantharaman Shivakumar ◽  
Avinash Gowda
Keyword(s):  
Spectrophotometric Determination ◽  
Correlation Coefficients ◽  
Dosage Forms ◽  
Pharmaceutical Dosage Forms ◽  
Variable Parameters ◽  
Spectrophotometric Methods ◽  
Linear Relationships ◽  
Colored Product ◽  
And Performance

Use ofN, N-diethyl-p-phenylenediamine sulphate for the spectrophotometric determination of some phenolic and amine drugsSpectrophotometric methods are proposed for the determination of drugs containing a phenol group [salbutamol sulphate (SLB), ritodrine hydrochloride (RTD), isoxsuprine hydrochloride (IXP)] and drugs containing an aromatic amine group [dapsone hydrochloride (DAP), sulfamethoxazole (SFM), and sulfadiazine (SFD)] in pharmaceutical dosage forms. The methods are based on coupling ofN, N-diethyl-p-phenylenediamine sulphate with the drugs in the presence of KIO4to give a green colored product (λmaxat 670 nm) and a red colored product (λmaxat 550 nm), respectively. Linear relationships with good correlation coefficients (0.9986-0.9996) were found between absorbance and the corresponding concentration of drugs in the range 1-7, 2-22, 1-17, 1.5-12, 2-25, and 2-21 μg mL-1for SLB, RTD, IXP, DAP, SFM and SFD, respectively. Variable parameters such as temperature, reaction time and concentration of the reactants have been analyzed and optimized. The RSD of intra-day and inter-day studies was in the range of 0.2-1.0 and 0.4-1.0%, respectively. No interference was observed from common pharmaceutical adjuvants. The reliability and performance of the proposed methods was validated statistically; the percentage recovery ranged from 99.5 ± 0.1 to 99.9 ± 0.3%. Limits of detection were 0.14, 0.21, 0.51, 0.44, 0.33 and 0.37 μg mL-1for SLB, RTD, IXP, DAP, SFM, and SFD, respectively.

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