scholarly journals Different spectrophotometric and TLC-densitometric methods for determination of olmesartan medoxomil and hydrochlorothiazide and their degradation products

2018 ◽  
Vol 9 (4) ◽  
pp. 400-407 ◽  
Author(s):  
Selvia Maged Adly ◽  
Maha Mohamed Abdelrahman ◽  
Nada Sayed Abdelwahab ◽  
Nourudin Wageh Ali
Keyword(s):  
Multivariate Calibration ◽  
Degradation Products ◽  
External Validation ◽  
Olmesartan Medoxomil ◽  
Partial Least Square ◽  
Least Square ◽  
Pharmaceutical Dosage Form ◽  
Calibration Models ◽  
Significant Difference

In this work, multivariate calibration models and TLC-densitometric methods have been developed and validated for quantitative determination of olmesartan medoxomil (OLM) and hydrochlorothiazide (HCZ) in presence of their degradation products, olmesartan (OL) and salamide (SAL), respectively. In the first method, multivariate calibration models including principal component regression (PCR) and partial least square (PLS) were applied. The wavelength range 210-343 nm was used and data was auto-scaled and mean centered as pre-processing steps for PCR and PLS models, respectively. These models were tested by application to external validation set with mean percentage recoveries 99.78, 100.01, 100.41 and 100.46% for OLM, HCZ, OL and SAL, respectively, for PLS model and also, 100.22, 100.40, 102.25 and 100.13% for them, respectively, for PCR model. The second method is TLC-densitometry at which the chromatographic separation was carried out using silica gel 60F254 TLC plates and the developing system consisted of a mixture of ethyl acetate:chloroform:methanol: formic acid:tri-ethylamine (60:40:4:4:1, by volume) with UV-scanning at 254 nm. The developed methods were successfully applied for determination of OLM and HCZ in their pharmaceutical dosage form. Also, statistical comparison was made between the developed methods and the reported method using student’s-t test and F-test and results showed that there was no significant difference between them concerning both accuracy and precision.

Quality Determination of Glass/Epoxy Prepreg by NIR Spectroscopy

2010 ◽  
Vol 152-153 ◽  
pp. 77-80
Author(s):  
Wei Li ◽  
Wei Jia Gao ◽  
Ping Chen ◽  
Bao Lei Sun
Keyword(s):  
Near Infrared ◽  
Nir Spectroscopy ◽  
Partial Least Square ◽  
Least Square ◽  
Volatile Content ◽  
Calibration Models ◽  
Significant Difference ◽  
Nondestructive Quality ◽  
The Mean

A near-infrared spectroscopy (NIR) technique has been applied for rapid and nondestructive quality determination of glass/epoxy prepreg. Abundant information related with resin and volatile was observed in the NIR spectra of the prepreg cloth. The partial least square (PLS) regression was used to develop the calibration models by utilizing several spectral pretreatments combined with different spectra ranges. Some unknown samples were analyzed by the NIR method. The mean absolute predicted errors were 0.32% and 0.214% for the resin content and the volatile content respectively. The results of the paired t-test revealed that there was no significant difference between the NIR method and standard method. The NIR method can be used to predict the resin and volatile content simultaneously within 30s. The study indicates that the NIR method is sufficiently for quality determination of glass/epoxy prepreg cloth.

scholarly journals Spectrophotometric determination of phenol in the presence of congeners by multivariated calibration

2001 ◽  
Vol 73 (4) ◽  
pp. 519-524 ◽  
Author(s):  
KELY VIVIANE DE SOUZA ◽  
PATRICIO PERALTA-ZAMORA
Keyword(s):  
Spectrophotometric Determination ◽  
Multivariate Calibration ◽  
Close Correlation ◽  
Degradation Process ◽  
Partial Least Square ◽  
Least Square ◽  
Partial Least Square Regression ◽  
Calibration Model ◽  
Transient Species

The generation of poly-hydroxilated transient species during the photochemical treatment of phenol usually impedes the spectrophotmetric monitoring of its degradation process. Frequently, the appearance of compounds such as pyrocatechol, hydroquinone and benzoquinone produces serious spectral interference, which hinder the use of the classical univariate calibration process. In this work, the use of multivariate calibration is proposed to permit the spectrophotometric determination of phenol in the presence of these intermediates. Using 20 synthetic mixtures containing phenol and the interferents, a calibration model was developed by using a partial least square regression process (PLSR) and processing the absorbance signal between 180 and 300 nm. The model was validated by using 3 synthetic mixtures. In this operation, typical errors lower than 3% were observed. Close correlation between the results obtained by liquid chromatography and the proposed method was also observed.

scholarly journals Multivariate method for prediction of fumonisins B1 and B2 and zearalenone in Brazilian maize using Near Infrared Spectroscopy (NIR)

PLoS ONE ◽  
2021 ◽  
Vol 16 (1) ◽  
pp. e0244957
Author(s):  
Denize Tyska ◽  
Adriano Olnei Mallmann ◽  
Juliano Kobs Vidal ◽  
Carlos Alberto Araújo de Almeida ◽  
Luciane Tourem Gressler ◽  
...  
Keyword(s):  
Infrared Spectroscopy ◽  
Near Infrared Spectroscopy ◽  
Near Infrared ◽  
External Validation ◽  
Partial Least Square ◽  
Least Square ◽  
Partial Least Square Regression ◽  
Contamination Level ◽  
Internal Validation ◽  
Significant Difference

Fumonisins (FBs) and zearalenone (ZEN) are mycotoxins which occur naturally in grains and cereals, especially maize, causing negative effects on animals and humans. Along with the need for constant monitoring, there is a growing demand for rapid, non-destructive methods. Among these, Near Infrared Spectroscopy (NIR) has made great headway for being an easy-to-use technology. NIR was applied in the present research to quantify the contamination level of total FBs, i.e., fumonisin B1+fumonisin B2 (FB1+FB2), and ZEN in Brazilian maize. From a total of six hundred and seventy-six samples, 236 were analyzed for FBs and 440 for ZEN. Three regression models were defined: one with 18 principal components (PCs) for FB1, one with 10 PCs for FB2, and one with 7 PCs for ZEN. Partial least square regression algorithm with full cross-validation was applied as internal validation. External validation was performed with 200 unknown samples (100 for FBs and 100 for ZEN). Correlation coefficient (R), determination coefficient (R2), root mean square error of prediction (RMSEP), standard error of prediction (SEP) and residual prediction deviation (RPD) for FBs and ZEN were, respectively: 0.809 and 0.991; 0.899 and 0.984; 659 and 69.4; 682 and 69.8; and 3.33 and 2.71. No significant difference was observed between predicted values using NIR and reference values obtained by Liquid Chromatography Coupled to Tandem Mass Spectrometry (LC-MS/MS), thus indicating the suitability of NIR to rapidly analyze a large numbers of maize samples for FBs and ZEN contamination. The external validation confirmed a fair potential of the model in predicting FB1+FB2 and ZEN concentration. This is the first study providing scientific knowledge on the determination of FBs and ZEN in Brazilian maize samples using NIR, which is confirmed as a reliable alternative methodology for the analysis of such toxins.

scholarly journals Simultaneous Spectrophotometric Determination of Amitriptyline Hydrochloride and Chlordiazepoxide in Pharmaceutical Tablets by Multivariate Calibration Method

2009 ◽  
Vol 6 (s1) ◽  
pp. S111-S116 ◽  
Author(s):  
Amir H. M. Sarrafi ◽  
Ziba Khodakarami ◽  
Masoumeh Karkeabadi
Keyword(s):  
Multivariate Calibration ◽  
Calibration Method ◽  
Test Sample ◽  
Pharmaceutical Products ◽  
Partial Least Square ◽  
Least Square ◽  
Partial Least Square Regression ◽  
Relative Standard ◽  
Amitriptyline Hydrochloride

The multivariate calibration method, partial least square regression (PLS) was applied for the simultaneous spectrophotometry determination of amitriptyline hydrochloride (AMT) and chlordiazepoxide (CHL) in their mixtures. The parameters of chemometric technique were optimized and the proposed method was validated with synthetic samples and applied to analyze these drugs in pharmaceutical products with good accuracy and precision. The results were compared with those given by United State Pharmacopoeia method. The square of the correlation coefficients (R2) for predicted AMT and CHL with the proposed method in a test sample were 0.9951 and 0.9897 respectively. The relative standard deviation for commercial tablets in the proposed method and USP standard method were 0.42 and 2.61%, respectively.

scholarly journals Development of Advanced Chemometric-Assisted Spectrophotometric Methods for the Determination of Cromolyn Sodium and Its Alkaline Degradation Products

Molecules ◽  
2020 ◽  
Vol 25 (24) ◽  
pp. 5953
Author(s):  
Noha M. El Zahar ◽  
Mariam M. Tadros ◽  
Bassam M. Ayoub
Keyword(s):  
Degradation Products ◽  
Principal Component Regression ◽  
Principal Component ◽  
Pharmaceutical Products ◽  
Partial Least Square ◽  
Cromolyn Sodium ◽  
Least Square ◽  
Alkaline Degradation ◽  
Stability Indicating

Advanced and sensitive spectrophotometric and chemometric analytical methods were successfully established for the stability-indicating assay of cromolyn sodium (CS) and its alkaline degradation products (Deg1 and Deg2). Spectrophotometric mean centering ratio spectra method (MCR) and chemometric methods, including principal component regression (PCR) and partial least square (PLS-2) methods, were applied. Peak amplitudes after MCR at 367.8 nm, 373.8 nm and 310.6 nm were used within linear concentration ranges of 2–40 µg mL−1, 5–40 µg mL−1 and 10–100 µg mL−1 for CS, Deg1 and Deg2, respectively. For PCR and PLS-2 models, a calibration set of eighteen mixtures and a validation set of seven mixtures were built for the simultaneous determination of CS, Deg1 and Deg2 in the ranges of 5–13 µg mL−1, 8–16 µg mL−1, and 10–30 µg mL−1, respectively. The authors emphasize the importance of a stability-indicating strategy for the investigation of pharmaceutical products.

scholarly journals ADVANCED AMPLITUDE CENTERING AS AN INVIGORATING MANIPULATION FOR UNIFIED WAVELENGTH SPECTRAL RESOLUTION OF TERNARY MIXTURES

2017 ◽  
Vol 9 (5) ◽  
pp. 43 ◽  
Author(s):  
Hayam M. Lotfy ◽  
Sarah S. Saleh
Keyword(s):  
Standard Addition ◽  
Pharmaceutical Formulations ◽  
Partial Least Square ◽  
Least Square ◽  
Ternary Mixtures ◽  
The Novel ◽  
Validity Of Results ◽  
Accuracy And Precision ◽  
Significant Difference

Objective: This work presented the novel spectrophotometric approach namely, advanced amplitude centering (AAC). The method was applied for the resolution of ternary mixtures with partially or completely overlapped spectra.Methods: Advanced amplitude centering was based on the determination of ternary mixtures using single divisor where the concentrations of the components are determined through progressive manipulation performed on the same ratio spectrum. The centered amplitude at unified wavelength was resolved and applied for the determination of three components with partially and severely overlapped spectra. The work discussed the applications and advantages of the novel univariate advanced amplitude centering compared to the chemometric model, partial least square (PLS).Results: The specificity of the proposed methods was checked using laboratory-prepared mixtures of amlodipine (AML), valsartan (VAL) and hydrochlorothiazide (HCT) and was successfully applied for the analysis of two pharmaceutical formulations. The validity of results was assessed by applying the standard addition technique.Conclusion: The results obtained were found to agree statistically with those obtained by a reported method, showing no significant difference with respect to accuracy and precision.

scholarly journals Genetic algorithm-based wavelength selection in multicomponent spectrophotometric determination by PLS: Application on sulfamethoxazole and trimethoprim mixture in bovine milk

2013 ◽  
Vol 78 (4) ◽  
pp. 555-564 ◽  
Author(s):  
Hadi Givianrad ◽  
Mohammad Saber-Tehrani ◽  
Saber Zarin
Keyword(s):  
Genetic Algorithm ◽  
Simultaneous Determination ◽  
Spectrophotometric Method ◽  
Multivariate Calibration ◽  
Bovine Milk ◽  
Partial Least Square ◽  
Least Square ◽  
Calibration Model ◽  
Calibration Methods

The simultaneous determination of sulfamethoxazole (SMX) and trimethoprim (TMP) mixtures in bovine milk by spectrophotometric method is a difficult problem in analytical chemistry, due to spectral interferences. By means of multivariate calibration methods, such as partial least square (PLS) regression, it is possible to obtain a model adjusted to the concentration values of the mixtures used in the calibration range. Genetic algorithm (GA) is a suitable method for selecting wavelengths for PLS calibration of mixtures with almost identical spectra without loss of prediction capacity using the spectrophotometric method. In this study, the calibration model based on absorption spectra in the 200-400 nm range for 25 different mixtures of SMX and TMP Calibration matrices were formed form samples containing 0.25-20 and 0.3-21 ?g mL-1 for SMX and TMP, at pH=10, respectively. The root mean squared error of deviation (RMSED) for SMX and TMP with PLS and genetic algorithm partial least square (GAPLS) were 0.242, 0.066 ?gmL-1 and 0.074, 0.027 ?g mL-1, respectively. This procedure was allowed the simultaneous determination of SMX and TMP in synthetic and real samples and good reliability of the determination was proved.

Multivariate Model Update Chemometric Methods for Determination of Prednisolone and Esomeprazole in Spiked Human Plasma: a Comparative Study

2021 ◽  
Author(s):  
Nehal F Farid ◽  
Maimana A Magdy ◽  
Basma H Anwar ◽  
Nessreen S Abdelhamid
Keyword(s):  
Human Plasma ◽  
Principal Component ◽  
Partial Least Square ◽  
Least Square ◽  
Peptic Ulcers ◽  
Spiked Human Plasma ◽  
Accuracy And Precision ◽  
Significant Difference ◽  
Spectrophotometric Data

Abstract Background Prednisolone is immunosuppressant and anti-inflammatory drug; it may cause peptic ulcers as a side effect. Esomeprazole is used for treatment of peptic ulcers therefore; the two drugs are co-administered in case of organ transplantation and autoimmune diseases. Objective This work aims to determine simultaneously the two drugs together in bulk and spiked human plasma by eliminating the overlapping between the spectra of each other and the interference of plasma matrix. Methods Two simple and effective model updated chemometric models called principal component analysis (PCA) and partial least square (PLS) were established using UV spectrophotometric data. Results The two updated models have been validated according to the U.S. Food and Drug Administration guidelines with accepted results. The results were statistically compared with those of the reported methods, where no significant difference was found, indicating the validity of the developed methods. The two updated models have been successfully applied for prediction of the proposed drugs with good results regarding accuracy and precision. Conclusion The two updated models are simple, rapid, sensitive, and precise and could be easily applied in quality control laboratories for determination of PRD and ESO, without any preliminary separation steps or interference from plasma matrix. Highlights Two model updated chemometric models called PCA and PLS were established for determination of prednisolone and esomeprazole in spiked human plasma using UV spectrophotometric data.

scholarly journals Simultaneous Detemination of Atorvastatin Calcium and Amlodipine Besylate by Spectrophotometry and Multivariate Calibration Methods in Pharmaceutical Formulations

2011 ◽  
Vol 8 (4) ◽  
pp. 1670-1679 ◽  
Author(s):  
Amir H. M. Sarrafi ◽  
Elahe Konoz ◽  
Maryam Ghiyasvand
Keyword(s):  
Least Squares ◽  
Partial Least Squares ◽  
Multivariate Calibration ◽  
Mean Squared Error ◽  
Sample Pretreatment ◽  
Partial Least Square ◽  
Least Square ◽  
Full Spectrum ◽  
Calibration Methods

Resolution of binary mixture of atorvastatin (ATV) and amlodipine (AML) with minimum sample pretreatment and without analyte separation has been successfully achieved using a rapid method based on partial least square analysis of UV–spectral data. Multivariate calibration modeling procedures, traditional partial least squares (PLS-2), interval partial least squares (iPLS) and synergy partial least squares (siPLS), were applied to select a spectral range that provided the lowest prediction error in comparison to the full-spectrum model. The simultaneous determination of both analytes was possible by PLS processing of sample absorbance between 220-425 nm. The correlation coefficients (R) and root mean squared error of cross validation (RMSECV) for ATV and AML in synthetic mixture were 0.9991, 0.9958 and 0.4538, 0.2411 in best siPLS models respectively. The optimized method has been used for determination of ATV and AML in amostatin commercial tablets. The proposed method are simple, fast, inexpensive and do not need any separation or preparation methods.

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