Determination of Residues of Acetaminophen, Caffeine, and Drotaverine Hydrochloride on Swabs Collected from Pharmaceutical Manufacturing Equipment Using HPLC in Support of Cleaning Validation

2014 ◽  
Vol 97 (5) ◽  
pp. 1439-1445 ◽  
Author(s):  
Mohamed E M Hassouna ◽  
Yousry M Issa ◽  
Ashraf G Zayed
Keyword(s):  
Mobile Phase ◽  
Hplc Method ◽  
Pharmaceutical Manufacturing ◽  
Manufacturing Equipment ◽  
Cleaning Validation ◽  
Accuracy And Precision ◽  
Drotaverine Hydrochloride ◽  
Time Required ◽  
Isocratic Mode

Abstract An HPLC method was developed for the simultaneous determination of residues of acetaminophen (paracetamol, PA), caffeine (CA), and drotaverine HCl (DH) on swabs collected from pharmaceutical manufacturing equipment surfaces. The challenge in cleaning validation is to develop analytical methods that are sensitive enough to detect traces of the active compounds remaining on the surface of pharmaceutical manufacturing equipment after cleaning. Chromatography was performed in the isocratic mode on a Hypersil C18 BDS column using the mobile phase 0.02 M tetrabutylammonium bisulfate–methanol (100 + 45, v/v) at 50°C with UV detection at 210 nm. The method was tested for specificity, linearity, LOD, LOQ, accuracy, and precision for determination of traces of the above-mentioned drugs. The time required for a single analysis was 12 min. The response was linear in the ranges of 6.900–52.100, 1.040–7.800, and 0.694–5.210 μg/mL for PA, CA, and DH, respectively.

scholarly journals Determination of Fenspiride Hydrochloride Residues on Pharmaceutical Manufacturing Equipment Surfaces by HPLC Method

2018 ◽  
Vol 6 (1) ◽  
pp. 7-15
Author(s):  
Ganna Fedosenko ◽  
Alla Yegorova ◽  
Yulia Scrypynets ◽  
Inna Leonenkoa ◽  
Ekaterina Vitukova
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Pharmaceutical Manufacturing ◽  
Detection Accuracy ◽  
Manufacturing Equipment ◽  
Accuracy And Precision ◽  
Liquid Chromatographic

The cleaning procedure must be validated, so special attention must be devoted to the methods used for determination of trace amounts of drugs. A rapid, sensitive, and specific reverse phase high-performance liquid chromatographic (HPLC) method was developed for the quantitative determination of fenspiride hydrochloride residues on pharmaceutical manufacturing equipment surfaces. The calibration curve was linear over a concentration range from 1.0 to 100.0 μg/ml with a correlation coefficient of 0.99994. The detection limit and quantitation limit were 0.41 μg/ml and 1.25 μg/ml, respectively. The developed method was validated with respect to specificity, linearity, limit of detection, accuracy and precision.

Stability-Indicating Chromatographic Methods for the Investigation of Ritodrine Hydrochloride Stability and Characterization of the Oxidative Degradation Product

2019 ◽  
Vol 57 (8) ◽  
pp. 730-737
Author(s):  
Noha Salem Rashed ◽  
Ola Mostafa Abdallah ◽  
Ahmed El-Olemy ◽  
Asmaa Ibrahim Hosam Eldin
Keyword(s):  
Degradation Product ◽  
Mobile Phase ◽  
Oxidative Degradation ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Chromatographic Methods ◽  
Ritodrine Hydrochloride ◽  
Accuracy And Precision ◽  
Intact Drug

Abstract Two simple and sensitive chromatographic methods were developed and validated for quantitative determination of ritodrine hydrochloride in presence of its oxidative degradation product. The first method depends on densitomeric determination of thin-layer chromatograms of the intact drug in presence of its oxidative degradate. Excellent separation was achieved at 220 nm using a mobile phase of dichloromethane–methanol–glacial acetic acid (15 : 5 : 0.25, v/v/v). The second was an HPLC method, in which efficient separation was carried out on C18 column (150 × 4.6 × 5 μm) using a mobile phase consisting of water: acetonitrile (70,30, v/v) at a flow rate of 1 mL min−1 and UV detection at 220 nm. Beer’s law was obeyed in the range of 0.025–0.3 μg/spot and 5–40 μg mL−1 of the intact drug using the two methods, respectively. The proposed methods were validated according to International Conference on Harmonization guidelines and successfully applied for the determination of ritodrine hydrochloride in bulk powder, laboratory prepared mixtures and pharmaceutical dosage form with good accuracy and precision. The results obtained were compared with those of the reported method and were found to be in good agreement.

scholarly journals Rapid Determination of α-Hederin and Hederacoside C in Extracts of Hedera helix Leaves Available in the Czech Republic and Poland

2015 ◽  
Vol 10 (9) ◽  
pp. 1934578X1501000
Author(s):  
Lucie Havlíková ◽  
Kateřina Macáková ◽  
Lubomír Opletal ◽  
Petr Solich
Keyword(s):  
Mobile Phase ◽  
Ammonium Acetate ◽  
Rapid Determination ◽  
Hplc Method ◽  
Leaf Extracts ◽  
Hedera Helix ◽  
The Czech Republic ◽  
Upper Respiratory ◽  
Isocratic Mode

Leaf extracts of Hedera helix L. are widely used in the treatment of upper respiratory diseases. The saponins α-hederin and hederacoside C are considered to be the main compounds responsible for the biological activity. α-Hederin and hederacoside C were determined in H. helix leaf extracts using a fast, simple and validated HPLC method. An XTerra MS C18 column and mobile phase composed of 10 mM ammonium acetate at pH 8.5 (adjusted with triethylamine) and acetonitrile were used for the chromatography at 1.2 mL min−1. The column was kept at 30°C. Detection was performed at 220 nm. An approach utilizing a basic pH of the aqueous part of the mobile phase enabled analysis in 5 minutes in isocratic mode. The method was validated and used for the quality control of H. helix leaf ethanolic extracts.

scholarly journals APPLICATION OF VALIDATED RP-HPLC METHOD FOR THE DETERMINATION OF ARMODAFINIL IN BULK AND FORMULATION

2017 ◽  
pp. 158-161
Author(s):  
Devi Ramesh ◽  
Mohammad Habibuddin
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
Isocratic Mode

Objective: The objective of the present study is to develop and validate a simple, rapid, sensitive reverse phase HPLC method for the determination of Armodafinil present in bulk and its pharmaceutical formulations.Methods: The chromatographic separation was achieved by using Hypersil ODS C-18 (150 x 4.6 mm, 5µ) in an isocratic mode with mobile phase methanol: phosphate buffer 3.0 (60:40 %v/v) was used. The flow rate was 1 ml/min and effluent was monitored at 225 nm. The method was validated for validation parameters i.e. linearity, accuracy, precision and robustness according to ICH guidelines.Results: The retention time of Armodafinil was 4.2 min and the linearity range of the method was 500-20000ng/ml with regression (r2) coefficient 0.9998. The method was validated for precision, accuracy, robustness and which were found to be within the acceptable limits according to the ICH guidelines. Also, the method was successfully applied for the estimation of Armodafinil in the marketed formulation of Nuvigil and the recovery was found to be>98%.Conclusion: The developed method possess good selectivity, specificity, there is no interference found in the blank at a retention time of ARM and good correlation between the peak area and concentration of the drugs under prescribed conditions. Hence, the method can be applied for routine analysis of Armodafinil. 

scholarly journals Validation method for determining sodium benzoate in fruit juice drinks in Malang

2019 ◽  
Vol 4 (1) ◽  
pp. 19
Author(s):  
Engrid Juni Astuti ◽  
Roha Fakhri Naufal Ilham ◽  
Januar Rahman
Keyword(s):  
Sodium Benzoate ◽  
Mobile Phase ◽  
High Performance ◽  
Glacial Acetic Acid ◽  
Fruit Juice ◽  
Hplc Method ◽  
Mobile Phase Composition ◽  
Validation Method ◽  
Accuracy And Precision

Sodium benzoate is a preservative that is permitted to be used in food and beverages. The maximum limit for using sodium benzoate in food is 600 mg/L of ingredients calculated as benzoic acid. In this study, High-Performance Liquid Chromatography (HPLC) method using a PDA detector was used for sodium benzoate levels analysis in fruit juice drink circulating in Malang. The mobile phase composition used in this study was methanol pro-HPLC:aqua pro injection (70:30) and added glacial acetic acid to reach pH 3. The analysis was conducted at a wavelength of 245 nm, and the flow rate was set at 1.00 mL/minute. This method was validated against the parameters of selectivity, linearity, accuracy, and precision, and the results obtained to meet the validation requirements. The application of the HPLC method after being validated in the determination of sodium benzoate levels in fruit juice drink circulating in Malang resulted in selectivity Rs ≥ 1.5, linearity obtained in the range 0.1-5 μg/mL with a correlation coefficient (r) = 0,9999, recovery at a concentration of 80%, 100%, and 120% was 105.31%, and precision with an RSD value of 1.40%. Based on the results, it can be concluded that the validation method of analysis shows that the method can be used to determine sodium benzoate level using HPLC with PDA detectors for routine use in fruit juice drink samples.

scholarly journals DEVELOPMENT AND VALIDATION OF A HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD DETERMINATION OF ZIDOVUDINE ENCAPSULATED IN PCL NANOPARTICLES

2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.

scholarly journals DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF ESCITALOPRAM OXALATE AND FLUPENTIXOL DIHYDROCHLORIDE IN COMBINED DOSAGE FORM AND PLASMA

2021 ◽  
pp. 61-66
Author(s):  
MALATHI SELLAPPAN ◽  
DARTHI DEVAKUMAR
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Accuracy And Precision ◽  
Relative Standard ◽  
Photodiode Array ◽  
Development And Validation ◽  
Potassium Dihydrogen Orthophosphate

Objective: The objective of the study was to develop a simple and rapid chromatographic method for quantification of escitalopram oxalate and flupentixol dihydrochloride in combined dosage form and plasma. Methods: The separation was achieved with a sun fire C8 [150×4.6 mm] 3.5 µm column with an isocratic mobile phase containing a mixture of potassium dihydrogen orthophosphate buffer: methanol: acetonitrile [30:60:10 v/v/v] pH adjusted to 11. The flow rate of the mobile phase was 1.5 ml/min with a Photodiode array [PDA] detection at 230 nm. Results: The HPLC method was developed and validated with respective linearity, accuracy, and precision, detection of limit, robustness, and specificity. The precision of the results stated as the relative standard deviation was below 2 %. The calibration curve was linear over a concentration range from 10-50 µg/ml for escitalopram oxalate and 1-5 µg/ml for flupentixol dihydrochloride with a correlation co-efficient 0.994 and 0.977 respectively. The accuracy of the method was demonstrated at levels in the range of 100 % and 120 % of the specification limit. The recovery of escitalopram oxalate and flupentixol dihydrochloride was found to be in the range of 90 % to 88 %, respectively. The lowest detection limits were found to be 2 µg/ml for escitalopram oxalate and 0.1 µg/ml for flupentixol dihydrochloride. The lowest quantification limits were found to be 5 µg/ml of escitalopram oxalate and 0.5 µg/ml of flupentixol dihydrochloride. Conclusion: The developed method was validated for linearity, accuracy, precision, the limit of detection and quantification, specificity. The method was applied successfully for the determination of escitalopram oxalate and flupentixol dihydrochloride in the combined dosage form and plasma.

scholarly journals RP-HPLC Method for the Estimation of Donepezil Hydrochloride Dosage Form

2009 ◽  
Vol 6 (2) ◽  
pp. 594-600 ◽  
Author(s):  
Tushar G. Barot ◽  
P. K. Patel
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Orthophosphoric Acid ◽  
Hplc Method ◽  
Rp Hplc ◽  
Accuracy And Precision ◽  
Donepezil Hydrochloride ◽  
Tablet Dosage ◽  
Isocratic Mode ◽  
Routine Quality Control

A simple and accurate methods to determine donepezil, in tablet dosage form, were developed and validated using liquid chromatography (LC). The LC separation was achieved on a Inertsil C8-3, 25 cm x 4.6-mm, 5 µ in the isocratic mode using buffer : methanol : triethylamine (550:450:5)v/v, adjusted to pH 2.50±0.05 with orthophosphoric acid, as the mobile phase at a flow rate of 1.0 mL/min. The methods were performed at 271 nm. In LC method, quantification was achieved with PDA detection over the concentration range of 20-60 µg/mL with mean recovery of 100.18±0.75%. The method was validated by determining its sensitivity, accuracy and precision. The proposed method is simple, fast, accurate and precise and hence can be applied for routine quality control of donepezil HCl in bulk and tablet dosage form

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