scholarly journals Chemometric Calculation for Determination of Betamethasone and Neomycin Mixture in Cream Supply by Ultraviolet Spectrophotometry

2019 ◽  
Vol 7 (22) ◽  
pp. 3911-3916
Author(s):  
Muchlisyam Bachri ◽  
Julia Reveny ◽  
Yade Metri Permata ◽  
D. N. Panjaitan
Keyword(s):  
Analytical Chemistry ◽  
Quality Control ◽  
Multivariate Calibration ◽  
Predictive Ability ◽  
Ultraviolet Spectrophotometry ◽  
Spectrophotometric Methods ◽  
Chemometric Technique ◽  
Relative Standard ◽  
Recovery Percentage

BACKGROUND: Chemometric can be defined as a branch of analytical chemistry using statistical principles to design and select optimal analytical procedures and experiments. The chemometric technique that applies in the design of quantitative calibration curves in the spectral analysis is very important in quality control of the component contained in the drug mixture of 2 or 3 drug components or more, especially the component that has the adjacent wavelength when the spectrum overlap.  AIM: The purpose of this study was to conduct research that examines betamethasone and neomycin mixture in cream with the UV spectrophotometric methods using a chemometric calculation. METHODS: Chemometric calculation for determination of betamethasone and neomycin mixture in cream supply by ultraviolet spectrophotometric. RESULTS: The result of betamethasone and neomycin levels were 91.35% and 97.56%, relative standard deviation (RSD) for betamethasone and neomycin 0.93%; 1.73% and recovery percentage 99.09%; 99.94%. On the multivariate calibration of PLS ​​betamethasone and neomycin with each RMSEC value of 0.0230 and 0.3553 with the value of RMSECV 0.7187 and 0.3586 with RMSEP value 0.1558 and 0.0820. Thus, the predictive ability of the research is still acceptable and is well used for grade determination of betamethasone and neomycin content ​​fulfil the requirement for cream preparation according to USP edition XXX. CONCLUSION: Methods of UV spectrophotometric with chemometric can be used in the determination of BET and NEO levels in cream preparations and BET level is 91.35% with a range of 90-110%, and NEO level is 97.56% with a range of 94.45-98.71%. These levels have met the requirements of the levels listed in Indonesian Pharmacopoeia, 2014.

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 A rapid spectrophotometric determination of imidacloprid in selected commercial formulations in the presence of 6-chloronicotinic acid

2009 ◽  
Vol 74 (12) ◽  
pp. 1455-1465 ◽  
Author(s):  
Valéria Guzsvány ◽  
Zsigmond Papp ◽  
Sanja Lazic ◽  
Ferenc Gaál ◽  
Luka Bjelica ◽  
...  
Keyword(s):  
Spectrophotometric Method ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Model Systems ◽  
Zero Crossing ◽  
Spectrophotometric Methods ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic

A simple first-order derivative spectrophotometric method was developed for the simultaneous determination of imidacloprid and 6-chloronicotinic acid (6-CNA). By using the zero-crossing approach, imidacloprid was determined at 249 nm and 6-CNA at 236 nm with detection limits of 0.32 and 0.17 ?g mL-1, respectively, and relative standard deviations not exceeding 1.2 % in the case of model systems. The proposed method was applied for the determination of imidacloprid and 6-CNA in commercial formulations. A conventional spectrophotometric method (at 270 nm) was also employed for the determination of the content of imidacloprid in the same commercial formulations. The results of the developed spectrophotometric methods were in good agreement with those obtained by the high-performance liquid chromatographic method.

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.

Atorvastatin: A Review of Analytical Methods for Pharmaceutical Quality Control and Monitoring

2019 ◽  
Vol 102 (3) ◽  
pp. 801-809
Author(s):  
Ana Carolina Kogawa ◽  
Ana Elisa Della Torre Pires ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
Analytical Chemistry ◽  
Quality Control ◽  
Analytical Methods ◽  
Pharmaceutical Products ◽  
Point Of View ◽  
Human Consciousness ◽  
Pharmaceutical Samples ◽  
Pharmaceutical Quality ◽  
The Impact

Abstract Background: Atorvastatin, a lipid-regulating drug, was the best-selling drug in the world in the early 2000s. Thus, monitoring of this drug is important because it is accessible to a large portion of the population. In addition, its quality control is fundamental to provide quality medicines. Method of analysis can be the first step in the rational use of pharmaceuticals. Objective/Methods: In this context, a critical review of analytical methods present in the literature and official compendia for the pharmaceutical quality control of atorvastatin was made. Results: Among the analytical methods most used in the evaluation of atorvastatin, HPLC is highlighted, followed by HPLC coupled to MS, and spectrophotometry in UV. Tablets are the most studied pharmaceutical samples, and plasma is the most studied biological matrix. In the literature, studies with atorvastatin-based pharmaceutical products are more common than biological materials. Acetonitrile is the organic solvent most commonly used in the methods surveyed to evaluate atorvastatin. Conclusions: Currently, awareness of the impact that the analytical choice has on the health of the operator and the environment is growing. Therefore, the suitability of existing methods for the determination of atorvastatin can be made to adhere to the current analytical chemistry. In this way, the analytical, environmental, and human consciousness will remain united. Highlights: Although the literature shows interesting methods from an economic and environmental point of view, such as UV, Vis miniaturized, and TLC, they can still be improved to meet the requirements of the current sustainable analytical chemistry.

scholarly journals Simultaneous Determination of Ternary Mixture of Carboxin, Chlorpyrifos, and Tebuconazole Residues in Cabbage Samples Using Three Spectrophotometric Methods

2020 ◽  
Vol 2020 ◽  
pp. 1-16 ◽  
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre
Keyword(s):  
Simultaneous Determination ◽  
Ternary Mixture ◽  
Solid Phase ◽  
Ternary Mixtures ◽  
Simultaneous Estimation ◽  
Great Success ◽  
Determination Limit ◽  
Spectrophotometric Methods ◽  
Relative Standard

Three simple precise and accurate spectrophotometric methods are developed for simultaneous determination of ternary mixtures of carboxin, chlorpyrifos, and tebuconazole residues in cabbage grown in the experimental field. The first method is a double divisor-ratio spectra derivative that relies on the derivative of ratio spectra and attained through dividing the absorption spectra of the ternary mixture by the sum of standard spectrum of a mixture of two from three components, using methanol as a solvent and measuring CAR at 242 nm, CHL at 236 nm, 276 nm, and 300 nm, and TEB at 226 nm. The second method is a successive derivative of ratio spectra which determined CAR at 256 nm and 258 nm, CHL at 290 nm and 292 nm, and TEB at 226 nm and 228 nm. The third method is a mean centering of ratio spectra where CAR, CHL, and TEB were measured at 306 nm, 280 nm, and 240 nm, respectively. These procedures do not involve any previous separation. The extraction of analytes was carried out by using acetonitrile, and the procedure of purification was fulfilled by dispersive solid-phase extraction with a primary-secondary amine (PSA). The proposed methods showed excellent linearity range for three spectrophotometric methods over the concentration ranges of 1–30 μg/mL, 1–50 μg/mL, and 1–45 μg/mL for carboxin, chlorpyrifos, and tebuconazole, respectively. The analytical characteristics such as detection limit, determination limit, relative standard deviation, and accuracy of the three methods were performed. The limits of detection were in the range of 0.153–0.260 μg/mL for carboxin, 0.137–0.272 μg/mL for chlorpyrifos, and 0.109–0.205 μg/mL for tebuconazole with limits of quantification lower than 0.790, 0.824, and 0.621 μg/mL for CAR, CHL, and TEB, respectively. The recoveries ranged from 87.02% to 94.53% for carboxin, 92.32% to 108.53% for chlorpyrifos, and 87.19% to 98.00% for tebuconazole with relative standard deviations less than 5.91%, 5.99%, and 5.53% in all instances for carboxin, chlorpyrifos, and tebuconazole, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed that there were no significant differences between three different spectrophotometric methods. The suggested methods can be applied with great success to the simultaneous estimation of carboxin, chlorpyrifos, and tebuconazole residues in cabbage samples.

Determination of Nitrogen Content in Milk by the Kjeldahl Method Using Copper Sulfate: Interlaboratory Study

1988 ◽  
Vol 71 (5) ◽  
pp. 893-898 ◽  
Author(s):  
R Grappin ◽  
William Horwitz
Keyword(s):  
Quality Control ◽  
Nitrogen Content ◽  
Copper Sulfate ◽  
Interlaboratory Study ◽  
Internal Quality ◽  
Relative Standard ◽  
Nitrogen Concentrations ◽  
Kjeldahl Method ◽  
Repeatability And Reproducibility

Abstract Copper sulfate was substituted for mercury as the catalyst in the International Dairy Federation (IDF) Standard 20A:1986 method for the determination of nitrogen content in milk. The substitution was supported by results obtained in an interlaboratory study by 24 laboratories in 12 countries. Each laboratory analyzed 12 test samples of milk as blind duplicates in a double split level design with high, medium, and low nitrogen concentrations. The method protocol requires the concurrent analyses of an ammonium salt solution and a tryptophan solution as internal quality control standards with a minimum nitrogen recovery between 99 and 100% for the former and at least 98% for the latter. The repeatability and reproducibility relative standard deviations are 0.5 and 1%, respectively, for the range 0.35-0.70 g N/100 g. The performance of the laboratories that did not meet the required quality control specifications was clearly poorer than that of those that did meet the specifications.

A Validated Method for the Quality Control of Andrographis paniculata Preparations

Planta Medica ◽  
2017 ◽  
Vol 83 (14/15) ◽  
pp. 1207-1213 ◽  
Author(s):  
Anastasia Karioti ◽  
Patricia Timoteo ◽  
Maria Bergonzi ◽  
Anna Bilia
Keyword(s):  
Quality Control ◽  
Time Course ◽  
Symptomatic Treatment ◽  
Reversed Phase ◽  
Andrographis Paniculata ◽  
Gradient System ◽  
Solvent Mixtures ◽  
Relative Standard ◽  
Precision And Accuracy

Abstract Andrographis paniculata is a herbal drug of Asian traditional medicine largely employed for the treatment of several diseases. Recently, it has been introduced in Europe for the prophylactic and symptomatic treatment of common cold and as an ingredient of dietary supplements. The active principles are diterpenes with andrographolide as the main representative. In the present study, an analytical protocol was developed for the determination of the main constituents in the herb and preparations of A. paniculata. Three different extraction protocols (methanol extraction using a modified Soxhlet procedure, maceration under ultrasonication, and decoction) were tested. Ultrasonication achieved the highest content of analytes. HPLC conditions were optimized in terms of solvent mixtures, time course, and temperature. A reversed phase C18 column eluted with a gradient system consisting of acetonitrile and acidified water and including an isocratic step at 30 °C was used. The HPLC method was validated for linearity, limits of quantitation and detection, repeatability, precision, and accuracy. The overall method was validated for precision and accuracy over at least three different concentration levels. Relative standard deviation was less than 1.13%, whereas recovery was between 95.50% and 97.19%. The method also proved to be suitable for the determination of a large number of commercial samples and was proposed to the European Pharmacopoeia for the quality control of Andrographidis herba.

Univariate and Multivariate Calibration for the Quantitative Determination of Methyl-Parathion in Pesticide Formulations by FT-Raman Spectroscopy

2000 ◽  
Vol 54 (5) ◽  
pp. 747-752 ◽  
Author(s):  
Stavroula G. Skoulika ◽  
Constantinos A. Georgiou
Keyword(s):  
Quantitative Determination ◽  
Methyl Parathion ◽  
Multivariate Calibration ◽  
Band Intensity ◽  
Calibration Data ◽  
Band Area ◽  
Pesticide Formulations ◽  
Relative Standard ◽  
Ft Raman

A Fourier transform (FT)-Raman method for the quantitative determination of methyl-parathion in pesticide formulations is described. The proposed method was applied to the analysis of formulations of methyl-parathion. Univariate and multivariate calibration were used and compared for quantitative analysis. Bands observed at 634, 661, 1113, 1348, and 1527 cm−1 were used for univariate calibration. Calibration curves were linear (correlation coefficients: 0.996–0.998 and 0.994–0.999 for band intensity and band area measurements, respectively) in the concentration range of 0.6–3.75 M for the 634, 661, and 1527 cm−1 bands; 0.05–3.75 M for the 1113 cm−1 band; and 0.1–3.75 M for the 1348 cm−1 band. Precision ranged from 0.5 to 5.2% and 0.1 to 6.8% relative standard deviation (RSD) ( n = 4) for band intensity and band area measurements, respectively. Spectra normalization against the 802 cm−1 cyclohexane band improved the long-term stability of calibration, allowing the use of calibration data acquired 30 days prior to analysis. The application of the method was extended through multivariate calibration by multiple linear regression using the 858 and 2952 cm−1 bands. Results obtained compare well with those obtained by the high-performance liquid chromatography (HPLC) reference method. The FT-Raman method developed is rapid, simple, and safe, as toxic samples are analyzed “as received” without sample pretreatment.

scholarly journals Kinetic Spectrophotometric Determination of Gemifloxacin Mesylate and Moxifloxacin Hydrochloride in Pharmaceutical Preparations Using 4-Chloro-7-nitrobenzo-2-oxa-1,3-diazole

2014 ◽  
Vol 2014 ◽  
pp. 1-12 ◽  
Author(s):  
Mohammed G. Abdel Wahed ◽  
Ragaa El Sheikh ◽  
Ayman A. Gouda ◽  
Sayed Abou Taleb
Keyword(s):  
Limit Of Detection ◽  
Kinetic Method ◽  
Pharmaceutical Preparations ◽  
Fixed Time ◽  
Spectrophotometric Methods ◽  
Relative Standard ◽  
Significant Difference ◽  
Kinetic Spectrophotometric ◽  
Comparison Of The Results

Simple, sensitive, and accurate kinetic spectrophotometric method was proposed for the determination of gemifloxacin mesylate (GMF) and moxifloxacin hydrochloride (MOX) in pure forms and pharmaceutical preparations (tablets). The method is based on coupling the studied drugs with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl) in the presence of alkaline borate buffer. Spectrophotometric measurement was achieved by recording the absorbance at 466 and 464 nm for GMF and MOX, respectively, after a fixed time of 20 and 15 min on a water bath adjusted at 70 ± 5°C for both drugs. The different experimental parameters affecting the development and stability of the color were carefully studied and optimized. The absorbance-concentration plots were linear over the ranges 0.5–8.0 and 2.0–12 μg mL−1for GMF and MOX, respectively. The limit of detection of the kinetic method was about 0.12 (2.47 × 10−7 M) and 0.36 (8.22 × 10−7 M) μg mL−1for GMF and MOX, respectively. The proposed methods have been applied and validated successfully with percentage relative standard deviation (RSD% ≤ 0.52) as precision and percentage relative error (RE% ≤ 1.33) as accuracy. The robustness of the proposed method was examined with recovery values that were 97.5–100.5 ± 1.3–1.9%. Statistical comparison of the results with the reference spectrophotometric methods shows excellent agreement and indicates no significant difference in accuracy or precision.

scholarly journals Application of Cerium (IV) as an Oxidimetric Agent for the Determination of Ethionamide in Pharmaceutical Formulations

2016 ◽  
Vol 2016 ◽  
pp. 1-9 ◽  
Author(s):  
Kanakapura Basavaiah ◽  
Nagib A. S. Qarah ◽  
Sameer A. M. Abdulrahman
Keyword(s):  
Quality Control ◽  
Pharmaceutical Formulations ◽  
Molar Absorptivity ◽  
Sample Solution ◽  
Standing Time ◽  
Spectrophotometric Methods ◽  
Ich Guidelines ◽  
Back Titration ◽  
Bulk Drug

Two simple methods are described for the determination of ethionamide (ETM) in bulk drug and tablets using cerium (IV) sulphate as the oxidimetric agent. In both methods, the sample solution is treated with a measured excess of cerium (IV) solution in H2SO4 medium, and after a fixed standing time, the residual oxidant is determined either by back titration with standard iron (II) solution to a ferroin end point in titrimetry or by reacting with o-dianisidine followed by measurement of the absorbance of the orange-red coloured product at 470 nm in spectrophotometry. In titrimetry, the reaction proceeded with a stoichiometry of 1 : 2 (ETM : Ce (IV)) and the amount of cerium (IV) consumed by ETM was related to the latter’s amount, and the method was applicable over 1.0–8.0 mg of drug. In spectrophotometry, Beer’s law was obeyed over the concentration range of 0.5–5.0 μg/mL ETM with a molar absorptivity value of 2.66 × 104 L/(mol·cm). The limits of detection (LOD) and quantification (LOQ) calculated according to ICH guidelines were 0.013 and 0.043 μg/mL, respectively. The proposed titrimetric and spectrophotometric methods were found to yield reliable results when applied to bulk drug and tablets analysis, and hence they can be applied in quality control laboratories.

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