First-Derivative Spectroscopic Determination of Acetaminophen and Sodium Salicylate in Tablets

1983 ◽  
Vol 66 (6) ◽  
pp. 1450-1454
Author(s):  
David Y Tobias
Keyword(s):  
Sodium Salicylate ◽  
Spectroscopic Method ◽  
Content Uniformity ◽  
First Derivative ◽  
Relative Standard ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic ◽  
Spectral Responses ◽  
Selection Of

Abstract A first-derivative spectroscopic method for the simultaneous determination of acetaminophen and sodium salicylate in tablets was developed. Solutions of this drug combination in acidic ethanol were analyzed using their respective spectral responses at 258.5 and 317.0 nm. The method, which can be used for tablet composite assay and content uniformity analysis, is linear for acetaminophen concentrations ranging from 0.0 to 21.6 μ/mL, and for sodium salicylate concentrations ranging from 0.0 to 36.0 μ/mL. Relative standard deviations for the assay of both drugs in commercial tablets were <2%, and recoveries of acetaminophen and sodium salicylate from spiked samples were 99.7 and 100.1%, respectively. The results obtained by first-derivative spectroscopy were in agreement with the results of a liquid chromatographic procedure for acetaminophen and a fluorometric method for sodium salicylate. The technique used for the selection of wavelengths for analysis is also described.

scholarly journals First derivative ATR-FTIR spectroscopic method as a green tool for the quantitative determination of diclofenac sodium tablets

F1000Research ◽  
2020 ◽  
Vol 9 ◽  
pp. 176
Author(s):  
Khairi M. S. Fahelelbom ◽  
Abdullah Saleh ◽  
Ramez Mansour ◽  
Sadik Sayed
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Ftir Spectroscopy ◽  
Limit Of Detection ◽  
Diclofenac Sodium ◽  
Spectroscopic Method ◽  
First Derivative ◽  
Drug Concentrations ◽  
Relative Standard

Background: Attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy is a rapid quantitative method which has been applied for pharmaceutical analysis. This work describes the utility of first derivative ATR-FTIR spectroscopy in the quantitative determination of diclofenac sodium tablets. Methods: This analytical quantitative technique depends on a first derivative measurement of the area of infrared bands corresponding to the CO stretching range of 1550-1605 cm-1. The specificity, linearity, detection limits, precision and accuracy of the calibration curve, the infrared analysis and data manipulation were determined in order to validate the method. The statistical results were compared with other methods for the quantification of diclofenac sodium. Results: The excipients in the commercial tablet preparation did not interfere with the assay. Excellent linearity was found for the drug concentrations in the range 0.2 – 1.5 w/w %.  (r2= 0.9994). Precision of the method was assessed by the repeated analysis of diclofenac sodium tablets; the results obtained showed small standard deviation and relative standard deviation values, which indicates that the method is quite precise. The high percentage of recovery of diclofenac sodium tablets (99.81, 101.54 and 99.41%) demonstrate the compliance of the obtained recoveries with the pharmacopeial percent recovery. The small limit of detection and limit of quantification values (0.0528 and 0.1599 w/w %, respectively) obtained by this method indicate the high sensitivity of the method. Conclusions: First derivative ATR-FTIR spectroscopy showed high accuracy and precision, is considered as nondestructive, green, low cost and rapid, and can be applied easily for the pharmaceutical quantitative determination of diclofenac sodium tablet formulations.

scholarly journals A Comparative Study of First-Derivative Spectrophotometry and Column High-Performance Liquid Chromatography Applied to the Determination of Repaglinide in Tablets and for Dissolution Testing

2008 ◽  
Vol 91 (3) ◽  
pp. 530-535 ◽  
Author(s):  
Bashar A AlKhalidi ◽  
Majed Shtaiwi ◽  
Hatim S AlKhatib ◽  
Mohammad Mohammad ◽  
Yasser Bustanji
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Spectroscopic Method ◽  
High Performance Liquid Chromatographic ◽  
Dissolution Testing ◽  
First Derivative ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Significant Difference

Abstract A fast and reliable method for the determination of repaglinide is highly desirable to support formulation screening and quality control. A first-derivative UV spectroscopic method was developed for the determination of repaglinide in tablet dosage form and for dissolution testing. First-derivative UV absorbance was measured at 253 nm. The developed method was validated for linearity, accuracy, precision, limit of detection (LOD), and limit of quantitation (LOQ) in comparison to the U.S. Pharmacopeia (USP) column high-performance liquid chromatographic (HPLC) method. The first-derivative UV spectrophotometric method showed excellent linearity [correlation coefficient (r) = 0.9999] in the concentration range of 135 g/mL and precision (relative standard deviation <1.5). The LOD and LOQ were 0.23 and 0.72 g/mL, respectively, and good recoveries were achieved (98101.8). Statistical comparison of results of the first-derivative UV spectrophotometric and the USP HPLC methods using the t-test showed that there was no significant difference between the 2 methods. Additionally, the method was successfully used for the dissolution test of repaglinide and was found to be reliable, simple, fast, and inexpensive.

High Pressure Liquid Chromatographic Determination of Arprinocid in Feed

1979 ◽  
Vol 62 (1) ◽  
pp. 1-4
Author(s):  
David W Fink ◽  
Allen Fox ◽  
James V Pivnichny
Keyword(s):  
High Pressure ◽  
Acidic Solution ◽  
Chromatographic Determination ◽  
Colorimetric Analysis ◽  
High Pressure Liquid Chromatographic ◽  
Relative Standard ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract Arprinocid [9 - (2 - chloro - 6 - fluorophenyl-methyl)-9H-purin-6-amine ] is determined in feed by high pressure liquid chromatography with a silica column and ultraviolet detection. The drug is extracted from the feed into chloroform in the presence of pH 7 phosphate buffer, transferred to 0.1N HCL, and separated from interfering substances by partitioning with hexane. The acidic solution is neutralized, and the analyte is extracted into chloroform for injection into the chromatograph. This procedure has been applied to feeds containing 0.0030—0.0090% arprinocid with a precision of < 5% relative standard deviation at the 0.0060% formulated concentration level. The results of this chromatographic procedure also correlate with those from a colorimetric analysis.

scholarly journals Simultaneous determination of acesulfame-K, aspartame and stevioside in sweetener blends by ultraviolet spectroscopy with variable selection by sipls algorithm

2012 ◽  
Vol 31 (1) ◽  
pp. 17 ◽  
Author(s):  
Yang-Chun He ◽  
Sheng Fang ◽  
Xue-Jiao Xu
Keyword(s):  
Least Squares ◽  
Simultaneous Determination ◽  
Partial Least Squares ◽  
Spectroscopic Method ◽  
Relative Standard Error ◽  
Full Spectrum ◽  
Region Selection ◽  
Relative Standard ◽  
Selection Of

A chemometric-assisted UV absorption spectroscopic method is proposed for the simultaneous determination of acesulfame-K, aspartame and stevioside in raw powder mixtures of commercial sweeteners. The synergy interval partial least squares (siPLS) algorithm was applied to select the optimum spectral range and their combinations. The utilization of spectral region selection aims to construct better partial least squares (PLS) model than that established from the full-spectrum range. The results show that the siPLS algorithm can find out an optimized combination of spectral regions, yielding lower relative standard error of prediction (RSEP) and root mean square error of prediction (RMSEP), as well as simplifying the model. The RMSEP and RSEP obtained after selection of intervals by siPLS were 0.1330 μg·ml–1 and 1.50 % for acesulfame-K, 0.2540 μg·ml–1 and 1.64 % for aspartame, 1.4041 μg·ml–1 and 2.03 % for stevioside respectively. The recovery values range from 98.12 % to 101.88 % for acesulfame-K, 98.63 % to 102.96% for aspartame, and 96.38 % to 104.04 % for stevioside respectively.

Solid-Phase Extraction and Liquid Chromatographic Determination of Monophthalates and Phthalide ExtractedFrom Solution Administration Sets

1993 ◽  
Vol 76 (3) ◽  
pp. 531-534 ◽  
Author(s):  
Robert P Snell
Keyword(s):  
Solid Phase ◽  
Correlation Coefficients ◽  
Chromatographic Determination ◽  
Relative Standard ◽  
Chromatographic Procedure ◽  
Monobutyl Phthalate ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Ethylhexyl Phthalate

Abstract A liquid chromatographic procedure is described for the determination of phthalide, monobutyl phthalate, and mono-2-ethylhexyl phthalate leached by water from solution administration sets. Recoveries varied from 88.8% for phthalide at 1 (μg/50 mL to 113% for monobutyl phthalate at 6 μg/50 mL. Relative standard deviations at 1 μg/50 mL were 2.59% for phthalide, 3.54% for monobutyl phthalate, and 11.6% for mono-2- ethylhexyl phthalate. At 6 μg/50 mL, the relative standard deviation for mono-2-ethylhexyl phthalate decreased to 3.88%. Reproducibilities for 5 standard injections were 1.40% for phthalide, 1.84% for monobutyl phthalate, and 1.95% for mono-2- ethylhexyl phthalate. Correlation coefficients were 1.00 for the 3 compounds. Five sets from 2 manufacturers were examined. No phthalide or monobutyl phthalate was found. One manufacturer’s sets contained 37.6-44.4 μg/L mono-2- ethylhexyl phthalate. The sample matrix had some interference if phthalide or monobutyl phthalate was present.

Liquid Chromatographic Determination of Methscopolamine Bromide in Various Veterinary Formulations

1979 ◽  
Vol 62 (5) ◽  
pp. 1099-1106
Author(s):  
Patrick A Hartman
Keyword(s):  
Degradation Products ◽  
Chromatographic Determination ◽  
Reverse Phase ◽  
Relative Standard ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Neomycin Sulfate ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A reverse phase paired ion liquid chromatographic procedure is described for determining methscopolamine bromide (Pamine) in the presence of neomycin sulfate in 5 veterinary formulations (Biosol M). Methscopolamine bromide is separated from neomycin sulfate and other formulation excipients by extraction into ethanol. The sample preparations are then concentrated and dissolved in water before chromatography. Recovery of methscopolamine bromide added to 5 placebo formulations ranged from 99.7 to 100.7%, with relative standard deviations of less than 2%. Specificity of the method with regard to potential degradation products is demonstrated.

Liquid Chromatographic Determination of Identity, Content, and Content Uniformity of Desipramine, Fluphenazine, and Promazine

1986 ◽  
Vol 69 (1) ◽  
pp. 178-179 ◽  
Author(s):  
Normand Beaulieu ◽  
Charles Gagné ◽  
Edward G Lovering
Keyword(s):  
Hydrochloric Acid ◽  
Active Ingredient ◽  
Dilute Hydrochloric Acid ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Content Uniformity ◽  
Chromatographic Procedure ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic procedure has been developed for the assay, content uniformity, and identification of single active ingredient formulations of desipramine, fluphenazine, and promazine. The drugs are extracted from formulations with methanol or dilute hydrochloric acid and quantitated against an internal standard (norephedrine). The drugs are identified by comparison of retention times with those of the reference standards.

scholarly journals First derivative ATR-FTIR spectroscopic method as a green tool for the quantitative determination of diclofenac sodium tablets

F1000Research ◽  
2020 ◽  
Vol 9 ◽  
pp. 176
Author(s):  
Khairi M. S. Fahelelbom ◽  
Abdullah Saleh ◽  
Ramez Mansour ◽  
Sadik Sayed
Keyword(s):  
Standard Deviation ◽  
Quantitative Determination ◽  
Ftir Spectroscopy ◽  
Limit Of Detection ◽  
Diclofenac Sodium ◽  
Spectroscopic Method ◽  
First Derivative ◽  
Drug Concentrations ◽  
Relative Standard

Background: Attenuated total reflection-Fourier transform infrared (ATR-FTIR) spectroscopy is a rapid quantitative method which has been applied for pharmaceutical analysis. This work describes the utility of first derivative ATR-FTIR spectroscopy in the quantitative determination of diclofenac sodium tablets. Methods: This analytical quantitative technique depends on a first derivative measurement of the area of infrared bands corresponding to the CO stretching range of 1550-1605 cm-1. The specificity, linearity, detection limits, precision and accuracy of the calibration curve, the infrared analysis and data manipulation were determined in order to validate the method. The statistical results were compared with other methods for the quantification of diclofenac sodium. Results: The excipients in the commercial tablet preparation did not interfere with the assay. Excellent linearity was found for the drug concentrations in the range 0.2 – 1.5 w/w %.  (r2= 0.9994). Precision of the method was assessed by the repeated analysis of diclofenac sodium tablets; the results obtained showed small standard deviation and relative standard deviation values, which indicates that the method is quite precise. The high percentage of recovery of diclofenac sodium tablets (99.81, 101.54 and 99.41%) demonstrate the compliance of the obtained recoveries with the pharmacopeial percent recovery. The small limit of detection and limit of quantification values (0.0528 and 0.1599 w/w %, respectively) obtained by this method indicate the high sensitivity of the method. Conclusions: First derivative ATR-FTIR spectroscopy showed high accuracy and precision, is considered as nondestructive, green, low cost and rapid, and can be applied easily for the pharmaceutical quantitative determination of diclofenac sodium tablet formulations.

Stability Indicating Liquid Chromatographic Method for the Determination of Fenofibrate and its Application to Kinetic Studies

2013 ◽  
Vol 5 (4) ◽  
pp. 1866-1874
Author(s):  
K. Srinivasa Rao ◽  
Keshar N K ◽  
N Jena ◽  
M.E.B Rao ◽  
A K Patnaik
Keyword(s):  
Degradation Products ◽  
Kinetic Studies ◽  
Pharmaceutical Formulations ◽  
Assay Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating ◽  
Zero Order Kinetics ◽  
Relative Standard ◽  
Liquid Chromatographic

A stability-indicating LC assay method was developed for the quantitative determination of fenofibrate (FFB) in pharmaceutical dosage form in the presence of its degradation products and kinetic determinations were evaluated in acidic, alkaline and peroxide degradation conditions. Chromatographic separation was achieved by use of Zorbax C18 column (250 × 4.0 mm, 5 μm). The mobile phase was established by mixing phosphate buffer (pH adjusted 3 with phosphoric acid) and acetonitrile (30:70 v/v). FFB degraded in acidic, alkaline and hydrogen peroxide conditions, while it was more stable in thermal and photolytic conditions. The described method was linear over a range of 1.0-500 μg/ml for determination of FFB (r= 0.9999). The precision was demonstrated by relative standard deviation (RSD) of intra-day (RSD= 0.56– 0.91) and inter-day studies (RSD= 1.47). The mean recovery was found to be 100.01%. The acid and alkaline degradations of FFB in 1M HCl and 1M NaOH solutions showed an apparent zero-order kinetics with rate constants 0.0736 and 0.0698  min−1 respectively and the peroxide degradation with 5% H2O2 demonstrated an apparent first-order kinetics with rate constant k = 0.0202 per min. The t1/2, t90   values are also determined for all the kinetic studies. The developed method was found to be simple, specific, robust, linear, precise, and accurate for the determination of FFB in pharmaceutical formulations.  

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.

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