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HPLC chromatogram of a mixture of naphazoline hydrochloride, chlorpheniramine maleate and naphazoline hydrochloride degradation product using 0.1M KH2PO4 (pH=7):methanol (55:45 v/v) as a mobile phase.
Source publication
Four accurate and sensitive methods were developed and validated for determination of naphazoline hydrochloride (NAP) and chlorpheniramine maleate (CLO) in the presence of naphazoline hydrochloride alkaline degradation product (NAP Deg). The first method is a spectrophotometric one , where NAP was determined by the fourth derivative (D4) spectropho...
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Citations
... Four reported impurities, namely; A, B, C and D, are also stated in its British pharmacopoeia (BP) monograph. Carefully reviewed spectrophotometric techniques reveal that NZ has been quantified in the existence of other substances [16][17][18][19][20][21] . ...
This work is concerned with exploiting the power of chemometrics in the assay and purity determination of naphazoline HCl (NZ) and pheniramine maleate (PN) in their combined eye drops. Partial least squares (PLS) and artificial neural network (ANN) were the chosen models for that purpose where three selected official impurities, namely; NZ impurity B and PN impurities A and B, were successfully determined. The quantitative determinations of studied components were assessed by percentage recoveries, standard errors of prediction as well as root mean square errors of prediction. The developed models were constructed in the ranges of 5.0–13.0 μg mL⁻¹ for NZ, 10.0–60.0 μg mL⁻¹ for PN, 1.0–5.0 μg mL⁻¹ for NZ impurity B and 2.0–14.0 μg mL⁻¹ for two PN impurities. The proposed models could determine NZ and PN with respective detection limits of 0.447 and 1.750 μg mL⁻¹ for PLS, and 0.494 and 2.093 μg mL⁻¹ for ANN. The two established models were compared favorably with official methods where no significant difference observed.
... Different columns -Determination of robustness was performed using a new column of the same parameter selected above [48][49][50][51][52]. ...
Aim
The present work aims to develop an analytical method and validate it to determine the assay of an antibacterial dug-in gel formulation.
Background
Background: Analytical Method Validation is a process involving confirmation studies that procedure/ method/ system/ analyst provides precise and reproducible outcome recognized by research laboratory studies that the performance features of the technique follows the necessities required for the analytical applications.
Introduction
Analytical Method Validation is a process involving confirmation studies that procedure/ method/ system/ analyst provides precise and reproducible outcomes recognized by research laboratory studies that the performance features of the technique follow the necessities required for the analytical applications.
Introduction
Analytical Method Validation is a process involving confirmation studies that procedure/ method/ system/ analyst provides precise and reproducible outcomes recognized by research laboratory studies that the performance features of the technique follow the necessities required for the analytical applications.
Objective
Objective: To improve the conditions and parameters which should be followed in the development and validation by developing a new sensitive and accurate RP-HPLC method. Validating the proposed newly developed methods per the analytical parameters mentioned in the IP, USP, BP and ICH guidelines.
Method
HPLC method was validated to indicate that the analytical procedure used is suitable for intended use by using various parameters like specificity, linearity, LOD, LOQ, precision, accuracy, range, robustness, stability in analytical solution and system suitability.
Method
HPLC method was validated to indicate that the analytical procedure used is suitable for intended use by using various parameters like specificity, linearity, LOD, LOQ, precision, accuracy, range, robustness, stability in analytical solution and system suitability.
Result
The standard retention times for the Drug Besifloxacin were 7.781 min, and the sample was 7.731, respectively. The area of standard besifloxacin was 1828547, and the sample area was 1825315. The assay of the sample was 98%. The retention times for the drug Phenoxyethanol standard were found to be 2.010 min, and the sample was at 2.004, respectively. The Area of standard Phenoxyethanol was 438025, and the sample area was 438103. The assay of the sample was 97.04%. The RSD for 5 replicate injections for each peak is 0.33% in system suitability. In specificity, peaks of Diluent, Placebo & Impurities are not interfering with the Besifloxacin peaks. Peaks of Besifloxacin were found to be pure. Degradation products were found to be well separated from the besifloxacin peak. The peak purity factor was NLT 0.9995. In the precision study, the System Precision RSD of the Retention time for Besifloxacin obtained from six replicate injections was 0.33%. The RSD of the Area of Besifloxacin obtained from six replicate injections is 0.46%. Method precision RSD was calculated on 6 determinations assay value of Drug besifloxacin is 0.56%. The RSD calculated on 6 determinations for the assay value of the Drug besifloxacin is 0.50%. In Intermediate precision, RSD was calculated on 6 determinations for the assay value of the Drug besifloxacin is 0.50%. The RSD calculated on 12 determinations (Method precision & Intermediate precision) for assay value is 0.50%. Stability in the analytical solution for the standard and sample, the area difference of besifloxacin peak was within ±2.0% from initial Linearity. The correlation coefficient & regression coefficient (R square) should be not less than 0.995 for Besifloxacin Correlation Coefficient is 0.998 Regression coefficient is 1.000. The % intercept should be within ±5.0% of the response at 100% level Precision at 50% & 150% levels; the RSD is 0.01%. Precision at 50% & 200% level: the RSD was found to be NMT 2.0%. Accuracy means % recovery at each level found to be between 98 to 101 % of the drug besifloxacin. RSD on 9 (3 levels X 3) determinations is 1.2, following the NMT 2% range criteria. A correlation was 1.0% for the accuracy and linearity parameters.
Conclusion
The % recovery is between 98% to 101%, and the % RSD for all recovery values is 1.41% which is within limits. The HPLC method optimized the conditions to obtain an adequate separation of eluted compounds.
Conclusion
The % recovery is between 98% to 101%, and the % RSD for all recovery values is 1.41% which is within limits. The HPLC method optimized the conditions to obtain an adequate separation of eluted compounds.
... Moreover, the BP states four specified official impurities; one of them is impurity B (NPZ impurity B). On reviewing literature, NPZ has been determined as a single drug or in combination using several techniques, namely; spectrophotometry [6][7][8][9][10][11][12][13][14], HPLC [15][16][17][18][19][20][21][22][23][24][25][26][27], TLC [28] and capillary electrophoresis [29][30][31][32][33][34][35][36]. ...
Impurity profiling of a pharmaceutical compound is now taking great attention during quality assessment of pharmaceuticals, as presence of small amount of impurities may affect safety and efficacy. In this work, a novel TLC chromatographic method coupled with densitometric detection was established for the simultaneous quantification of naphazoline HCl, pheniramine maleate and three of their official impurities, namely; naphazoline impurity B, pheniramine impurities; A & B. Chromatographic separation was carried out on TLC aluminum silica plates F254, as a stationary phase, using methanol: ethyl acetate: 33.0% ammonia (2.0: 8.0: 1.0, by volume), as a mobile phase. Plates were examined at 260.0 nm and International Council for Harmonisation (ICH) guidelines were followed for method’s validation. Important factors, such as; composition of mobile phase and detection wavelengths were optimized. Linearity was achieved over the ranges of 2.0–50.0 µg band ⁻¹ for naphazoline, 10.0–110.0 µg band ⁻¹ for pheniramine, 0.1–10.0 µg band ⁻¹ for naphazoline impurity B and 2.0–50.0 µg band ⁻¹ for both pheniramine impurities. The proposed method was assessed in terms of accuracy, precision and robustness where satisfactory results (recovery % ≈ 100% and RSD < 2) were obtained. The method was also applied for the simultaneous determination of naphazoline HCl and pheniramine maleate, in Naphcon-A ® eye drops, with respective recoveries of 101.36% and 100.94%. Method greenness was evaluated and compared to the reported HPLC one via environmental, health and safety tool. The developed method has much potential over the reported one of being simple, selective, economic and time saving for the analysis of the five cited compounds.
... (Nemakal et al., 2019) Literature studies have shown that there are different analytical methods for determination of binary or ternary mixtures of PAR, DEX, CHL and PSE in pharmaceutical formulations, cold syrup formulation and or biological matrix. Fluorescence spectrophotometric (Azmi et al., 2017), spectrophotometric and chemometric (El deen Sayed et al., 2013;Shrestha, Pradhananga, 1970), liquid chromatography-tandem mass spectrometry (LC-MS/ MS) (Hu et al., 2011;Celma et al., 2000, Li et al., 2009, reverse phase high performance liquid chromatographic (RP HPLC) (Hood, Cheung, 2003;Abdelwahab, Abdelaleem, 2017;Dewani et al., 2014;Palabiyik, Onur, 2007), liquid chromatography/quadrupole-time-offlight mass spectrometry (LC/Q-TOF-MS) (Thurman, Ferrer, 2012), liquid chromatography method with fluorimetric detection (Afshar, Rouini, Amini, 2004), capillary electrophoretic (CE) (Kristensen, 1998), raman spectroscopy (Ali et al., 2019), electrochemical method (Tyszczuk-Rotko, Jaworska, Jedruchniewicz, 2019), high performance liquid chromatography coupled to diode array detection (HPLC-DAD) (Santos et al., 2013), HPLC-MS/MS (Hewavitharana et al., 2008), capillary zone electrophoresis (CZE) (Capella-Peiro et al., 2006), high performance thin layer chromatography (HPTLC) (Makhija, Vavia, 2001), derivative spectrophotometry and ratio spectra derivative spectrophotometry (Onur et al., 2000), nonaqueous CE (Dong et al., 2005), and normal-phase LC (Al-Rimawi, 2010) methods have been Ephedrine (EPH), 2-methylamino-1-phenylpropan-1-ol, (Figure 1f) is a medication extracted from a plant called Ephedra sinica that acts as a sympathomimetic stimulant on central nervous system to prevent low blood pressure in cardiovascular diseases and hypotension caused by anesthesia. Also, EPH is the major impurity of PSE. ...
Abstract A capillary electrophoresis method was developed for the first time and optimized for the determination of paracetamol, pseudoephedrine, dextromethorphan, chlorpheniramine, 4-aminophenol and ephedrine in tablet formulation. Optimum electrophoretic conditions were achieved by using a background electrolyte of 75 mmol L-1 sodium borate buffer at pH 8.0, a capillary temperature of 30°C, a separation voltage of 30 kV and a pressure injection of the sample at 50 mbar for 10 s. Calibration graphs showed a good linearity with a coefficient of determination (R2) of at least 0.999 for all compounds. Intraday and interday precision (expressed as relative standard deviation (RSD) %) were lower than 1.39% for capillary electrophoresis method. The developed method was demonstrated to be simple and rapid for the determination of paracetamol, pseudoephedrine, dextromethorphan, chlorpheniramine, 4-aminophenol and ephedrine in tablet formulation providing recoveries in the range between 99.62 and 100.57% for all analytes.
... Chemometrics (multivariate calibration methods) [13][14][15][16][17][18][19] is the art of data processing with different numerical techniques for obtaining useful information. Chemometry is a chemical discipline that designs, selects and provides maximum chemical information by analyzing chemical data using mathematical and statistical methods. ...
Three multivariate calibration-prediction techniques, partial least squares (PLS), principal component regression (PCR) and artifi cial neural networks (ANN), have been applied without separation in the spectrophotometric multi-component analysis of phenylephrine hydrochloride and naphazoline hydrochloride. A set of 25 synthetic mixtures of phenylephrine hydrochloride and naphazoline hydrochloride has been evaluated to determine the predictability of PLS, PCR and ANN. The absorbance data matrix was obtained by measuring zero-order absorbances between 230-300 nm at intervals of 3 nm. The suitability of the models was determined on the basis of root mean square error (RMSE), root mean squared cross validation error (RMSECV) and root mean squared prediction error (RMSEP) values of calibration and validation data. The results showed a very good correlation between true values and the predicted concentration values. Therefore, the methods developed can be used for routine drug analysis without chemical pre-treatment.
... The combination of NAP and CPM in eye and nose drops is not official in any pharmacoepia; however, several methods are available in the literature for their determination based on various spectrophotometric techniques (10-13), thin-layer chromatography (10,13), high-performance liquid chromatography (14)(15)(16) and gas chromatography (17). ...
A simple and efficient liquid chromatographic method has been developed and validated for the simultaneous determination of naphazoline and chlorpheniramine in eye/nose drops, in presence of naphazoline degradation product and naphthalene acetic acid (NAPD). The separation was achieved within 6.0 min, employing a mixture of 53.5% v/v water-acetonitrile containing 78.70 mM/L sodium dihydrogen orthophosphate adjusted to pH 5.30 as isocratic mobile phase, pumped at 1.0 mL/min through a strong cation-exchange column (10 µm particle size), the analytes were monitored at 230 nm. Statistical experimental designs and graphic representations (response surface methodology) were used for optimizing the chromatographic separation. The linearity plots were linear over concentration range up to 125% of the analytes nominal concentrations (100%) with regression coefficients (r) > 0.99, method's accuracy (RSD < 2.0%), repeatability and intermediate precision (RSD < 2.0%) were verified. System suitability parameters were also within the acceptable range. The validated method was successfully employed for the routine analysis of eye/nose drops.
Drug impurities are now seen as a major threat to drug safety around the world, especially when it comes to carcinogenic impurities. Here, we present the first spectrophotometric approach for the quantification of lignocaine and fluorescein in the presence of 2,6-xylidine, lignocaine’s carcinogenic impurity. The approach depends on overcoming unresolved bands through a data processing strategy employing 10 affordable, simple, and sensitive spectrophotometric methods. Fluorescein analysis (1–16 μg mL ⁻¹ ) was performed using direct ultraviolet spectrophotometry (D ⁰ ) at 478 nm; then, the ratio subtraction method allowed the removal of interference caused by the fluorescein spectrum. From the resulting ratio spectra, 2,6-xylidine (40–160 μg mL ⁻¹ ) can be efficiently determined at 280 nm. However, lignocaine (72–320 μg mL ⁻¹ ) was analyzed using different ultraviolet-based methods, including continuous wavelet transform, ratio derivative by Savitzky–Golay filters, mean centering, second derivative of ratio spectra, ratio spectra difference spectrophotometry, extended ratio subtraction, absorbance subtraction, Q-absorbance ratio, and area under the curve. In line with International Council for Harmonization of Technical Requirements for Pharmaceuticals for Human Use (ICH), the presented approach was evaluated by its coefficients of determination, detection limits, quantification limits, and relative standard deviations. Similarly, the developed approach was assessed for whiteness, greenness, and sustainability using five assessment tools, including National Environmental Method Index, Eco-Scale Assessment, Complementary Green Analytical Procedure Index, Analytical Greenness Metric, and RGB12, offering promising results. Owing to the satisfactory analytical performance, besides the sustainability, affordability, simplicity, and cost efficiency of the presented methods, their application for quality control and in situ analysis in minimal-infrastructure laboratories increases, increasing the surveillance potential.
Spectroscopic method in the UV-Vis region is considered the most molecular spectrometric method for content determination of a single component. However, a lot of pharmaceutical dosage forms comprise two or more components which lead to peak overlapping. Moreover, in the chemical stability test, active pharmaceutical ingredient (API) was also found along with the degradation products, impurities, and adulterant compounds. UV-Vis spectroscopy is one of the methods of choice for the determination or quantification of a single component in pharmaceutical preparations. The pharmaceutical products typically contain two or more APIs having chromophoric agents capable of absorbing UV-Vis beams and the absorbance values are summative from the absorption of each UV-Vis active compound according to the additive nature of Lambert-Beer law. The main problem for the simultaneous determination of API along with impurities and the degradation products in pharmaceutical preparations is the presence of overlapping peaks of UV-Vis spectra. The chemometrics-assisted spectroscopy is one of the analytical efforts to solve these problems. This review highlighted the application of chemometrics in combination with UV-Vis spectroscopy for the assay of API, impurities, adulteration issues and degradation products present in pharmaceutical dosage forms.
