scholarly journals Fast and selective HPLC-DAD method for determination of pholcodine and related substances

2011 ◽  
Vol 30 (2) ◽  
pp. 139 ◽  
Author(s):  
Ana Petkovska ◽  
Hristina Babunovska ◽  
Marina Stefova
Keyword(s):  
Quality Control ◽  
Degradation Products ◽  
Ammonium Hydroxide ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Real Sample Analysis ◽  
Related Substances ◽  
Structural Analogues ◽  
Reliable Methods

Quality control of pharmaceuticals requires development of fast, efficient and reliable methods for determination of active compounds as well as known and very often unknown impurities within defined concentration ranges. In this work, a simple and rapid HPLC-UV-DAD method for identification and quantification of pholcodine process related impurities and some degradation products was developed and validated. Pholcodine and its five structural analogues such as morphine, codeine, thebaine, oripavine, and papaverine were separated in less than 10 minutes using reversed phase LiChrospher C-8 column. For optimal chromatographic performance with reproducible retention times, gradient elution with 2% ammonium hydroxide in water and acetonitrile was used. The method was validated by establishing its selectivity, specifity, sensitivity, linearity, intra- and inter-day precision and robustness. All tested parameters confirmed that the method is suitable for determination of pholcodine and its five impurities in pharmaceutical drug samples. The results obtained from real sample analysis give support to the suitability of the proposed method for the purpose of quality control.

scholarly journals Determination of Mesalamine Related Impurities from Drug Product by Reversed Phase Validated UPLC Method

2011 ◽  
Vol 8 (1) ◽  
pp. 131-148 ◽  
Author(s):  
Trivedi Rakshit Kanubhai ◽  
Patel Mukesh C ◽  
Kharkar Amit R
Keyword(s):  
Degradation Products ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Forced Degradation ◽  
Limit Of Quantification ◽  
Release Formulation ◽  
Delayed Release ◽  
Related Substances

In the present study gradient reversed-phase UPLC method was developed for simultaneous determination and separation of impurities and degradation products from drug product. The chromatographic separation was performed on acquity UPLC BEH C18 column (50 mm×2.1 mm, 1.7 µm) using gradient elution. Other UPLC parameters which were optimised are flow rate, 0.7 mL/min; detection wavelength, 220 nm; column oven temperature, 40°C and injection volume 7 µL. Stability indicating capability was established by forced degradation experiments and separation of known degradation products. The method was validated as per International Conference on Harmonization (ICH) guideline. For all impurities and mesalamine, LOQ (limit of quantification) value was found precise with RSD (related standard daviation) of less than 2.0%. In essence, the present study provides an improved low detection limit and lower run time for evaluation of pharmaceutical quality of mesalamine delayed-release formulation. Moreover, the developed method was successfully applied for quantification of impurities and degradation products in mesalamine delayed-release formulation. The same method can also be used for determination of related substances from mesalamine drug substance.

scholarly journals A reliable HPLC-DAD method for simultaneous determination of related substances in TBI-166 active pharmaceutical ingredient

2020 ◽  
Vol 32 (2) ◽  
pp. 80-85
Author(s):  
Tingting Zhang ◽  
Wanting Yin ◽  
Bo Jin ◽  
Tong Li ◽  
Chen Ma
Keyword(s):  
High Performance ◽  
Correlation Coefficients ◽  
Active Pharmaceutical Ingredient ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Phase System ◽  
Related Substances ◽  
Ich Guidelines ◽  
Bulk Drug

A sensitive, stability-indicating reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) method has been developed for the determination of TBI-166 and its 10 kinds of related impurities. Chromatographic separation was achieved on a Kromasil ODS column (250 mm × 4.6 mm, 5 μm), with a gradient elution of the mobile phase system consisting of acetonitrile and 1% ammonium formate solution (with 0.2% formic acid). The flow rate was 1.0 mL/min, and the detection wavelength was set at 251 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to selectivity, linearity, limits, accuracy, precision, and robustness. The calibration curves were linear from LOQ to 150% of the specification limit of impurity with correlation coefficients not less than 0.999. The limits of quantitation were between 0.123 and 0.257 μg/mL. Accuracy for the related substances was estimated by the recovery ranged from 94.6% to 111.2%. The method was proved to be reliable for the determination of related substances in TBI-166 bulk drug, which is essential and important in the quality control.

scholarly journals Reversed-Phase Ultra-Performance Liquid Chromatographic Method Development and Validation for Determination of Impurities Related to Torsemide Tablets

2011 ◽  
Vol 94 (1) ◽  
pp. 143-149 ◽  
Author(s):  
Hitesh B Patel ◽  
Arivozhi Mohan ◽  
Hitendra S Joshi
Keyword(s):  
Method Development ◽  
Degradation Products ◽  
Drug Product ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Ratio Method ◽  
Response Factors ◽  
Slope Ratio Method ◽  
Determination Of Impurities

Abstract A simple RP-ultra-performance LC method was developed and validated for determination of impurities related to torsemide tablets. The rapid method provided adequate separation of all known related impurities and degradation products. Separation was achieved on a Zorbax SB-C18 column (50 × 4.6 mm id, 1.8 μm particle size) with binary gradient elution, and detection was performed at 288 nm. The drug product was subjected to oxidative, hydrolytic, photolytic, and thermal stress conditions to prove the specificity of the proposed method. The linearity and recovery were investigated for known impurities in the range of 0.025 to 1.0%, with respect to the drug concentration in the prepared sample. The linearity of the calibration curve for each of the impurities and torsemide was found to be very good (r2 > 0.999). Relative response factors for each of the known impurities were established by the slope ratio method from the linearity study.

scholarly journals An Improved LC-MS/MS Method for Simultaneous Determination of the Eleven Bioactive Constituents for Quality Control of Radix Angelicae Pubescentis and Its Related Preparations

2015 ◽  
Vol 2015 ◽  
pp. 1-10 ◽  
Author(s):  
Jin Li ◽  
Qiu-Hong Zhang ◽  
Jun He ◽  
Er-wei Liu ◽  
Xiu-mei Gao ◽  
...  
Keyword(s):  
Quality Control ◽  
Simultaneous Determination ◽  
Control Method ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Bioactive Constituents ◽  
Linear Gradient ◽  
Radix Angelicae Pubescentis ◽  
Aqueous Ammonium Acetate

An improved LC-MS/MS method was developed for simultaneous determination of eleven bioactive constituents of Radix Angelicae Pubescentis and its related preparations. It was the first report on the quantification of bioactive constituents in different preparations of Radix Angelicae Pubescentis by LC-MS/MS analytical method. These samples were separated with an Agilent Zorbax Extend reversed-phase C18 column (1.8 μm, 4.6 × 100 mm) by linear gradient elution using aqueous ammonium acetate and acetonitrile as mobile phase. The flow rate was 0.3 mL min−1. The eleven bioactive constituents showed good regression(R>0.990)within test ranges and the recoveries were in the range of 87.1–110%. The limit of detections and quantifications for most of the major constituents were less than 0.5 and 1.0 ng mL−1, respectively. All results indicated that the developed method could be readily utilized as a suitable quality control method for Radix Angelicae Pubescentis and related preparations.

scholarly journals Validation of a liquid chromatographic method for determination of related substances in a candidate certified reference material of captopril

2011 ◽  
Vol 47 (2) ◽  
pp. 351-362 ◽  
Author(s):  
Raquel Nogueira ◽  
Wagner Wollinger ◽  
Thaís Elias da Silva ◽  
Leonardo Mesquita de Oliveira ◽  
Eliane Cristina Pires do Rego ◽  
...  
Keyword(s):  
Reference Material ◽  
Mass Balance ◽  
Certified Reference Material ◽  
High Performance ◽  
Degradation Products ◽  
Reversed Phase ◽  
Scanning Calorimetry ◽  
Chromatography Method ◽  
Related Substances

This paper describes the validation of a reversed-phase high performance liquid chromatography method (RP-HPLC) with diode array detection (DAD) for determination of related substances (impurities from organic synthesis and degradation products) of captopril according to the Brazilian Pharmacopeia IV. The aim of this study was to guarantee the method accuracy for quantification of related substances, an essential requisite to determine, using the mass balance approach, the captopril content in the first Brazilian certified reference material (CRM) of an active pharmaceutical ingredient (API), developed by Inmetro. The captopril instability in solution is discussed and the captopril content determined by mass balance is compared to the results from titration and differential scanning calorimetry (DSC).

Simultaneous Determination of Eight Potential Q-Markers in Zishen Tongguan Capsules Based on UHPLC-MS/MS

2020 ◽  
Vol 17 (1) ◽  
pp. 47-56
Author(s):  
Shun Liu ◽  
Xun Wang ◽  
Kaiping Zou ◽  
Wei Liu ◽  
Cunyu Li ◽  
...  
Keyword(s):  
Quality Control ◽  
Chinese Medicine ◽  
Simultaneous Determination ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Quality Markers ◽  
High Repeatability ◽  
Comprehensive Study

Background: Zishen Tongguan (ZSTG) capsules were prepared at the Affiliated Hospital of Nanjing University of Chinese Medicine and have been proven to be clinically effective for treating pyelonephritis and benign prostatic hyperplasia. However, the quality standards are not ideal; a comprehensive study of the “quality markers” (Q-markers), the chemicals inherent in traditional Chinese medicine and its preparations, has not been carried out. Experimental Methods: In this paper, a sensitive and specific ultra-high-performance liquid chromatographictandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of eight potential Q-markers of ZSTG, including timosaponin A3, berberine, jatrorrhizine, phellodendrine, palmatine, mangiferin, neomangiferin, and timosaponin BII. A Kromasil 100-3.5 C18 column was used with a mobile phase of 0.2% formic acid with acetonitrile, and gradient elution at a flow rate of 0.2 mL/min was achieved in 13 minutes and used for separation. Detection was performed in positive/negative mode with multiple reaction monitoring (MRM). Results: The analytical method was validated in terms of the sensitivity, linearity, accuracy, precision, repeatability, stability and recovery. The method established here was successfully applied to study the potential Q-markers in 8 batches of commercial samples, which demonstrated its use in improving the quality control of ZSTG. Conclusion: The developed method had high repeatability and accuracy and was suitable for the simultaneous analysis of multiple Q-markers, which may provide a new basis for the comprehensive assessment and overall quality control of ZSTG.

Simultaneous Determination of Methocarbamol and Paracetamol in the Presence of Three Related Substances by Ultra Performance Liquid Chromatography

2019 ◽  
Vol 15 (5) ◽  
pp. 505-510
Author(s):  
Yanjuan Zheng ◽  
Qiushi Peng ◽  
Rui Dong ◽  
Tingyu Chen ◽  
Yi Bao ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Pharmaceutical Preparations ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Related Substances ◽  
Bulk Powder ◽  
Highly Sensitive ◽  
Optimal Protocol ◽  
Acquity Uplc

Introduction: A rapid, and accurate Ultra Performance Liquid Chromatography (UPLC) method was developed to simultaneously analyze Methocarbamol, Paracetamol and the related substances Materials and Methods: Waters ACQUITY UPLC® BEH Phenyl C18 column was used in conjunction with UV detection at 225nm. Gradient elution with 0.05M, pH 6 phosphate buffer and acetonitrile flow at 0.3mL /min rate were used to separate the substances. The retention times for 4-Aminopheno, Paracetamol, Guaifenesin, Methocarbamol, and 4-Chloroacetanilide were 1.319 minute, 2.224 minute, 4.467 minute, 4.769 minute and 5.433 minute respectively. The concentration was linear in the range of 2-100 µg/ml for Methocarbamol, and 1-100 µg/mL for Paracetamol. The percentage recoveries were between 99.28±1.23% to 100.57±0.99% for Methocarbamol, and between 99.08±1.23% to 101.23±1.39% for Paracetamol. Results and Discussion: The validated optimal protocol is robust and accurate for simultaneous analysis of Methocarbamol, Paracetamol and the related substances, applicable for bulk powder as well as pharmaceutical formulation. Conclusion: In this paper, a highly sensitive, accurate, and precise UPLC method with UV-Vis detection was developed and validated for quality control of MET and PAR in bulk as well as in pharmaceutical preparations.

A Versatile Stability-indicating Liquid Chromatographic Method for the Simultaneous Determination of Atenolol, Hydrochlorothiazide and Chlorthalidone

2020 ◽  
Vol 16 (8) ◽  
pp. 1037-1051
Author(s):  
Ehab Farouk Elkady ◽  
Marwa Ahmed Fouad ◽  
Abdulgabar A. Ezzy Faquih
Keyword(s):  
Quality Control ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Pharmaceutical Dosage Forms ◽  
Potassium Dihydrogen ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Potassium Dihydrogen Orthophosphate

Background: Atenolol is a selective beta 1 blocker that can be used alone or in combination with hydrochlorothiazide or with chlorthalidone for the treatment of hypertension and prevention from a heart attack. Objective: The main target of this work was to improve modern, easy, accurate and selective liquid chromatographic method (RP-HPLC) for the determination of these drugs in the presence of their degradation products. These methods can be used as analytical gadgets in quality control laboratories for a routine examination. Methods: In this method, the separation was accomplished through an Inertsil® ODS-3V C18 column (250 mm x 4.6 mm, 5 μm), the mobile phase used was 25 mM aqueous potassium dihydrogen orthophosphate solution adjusted to pH 6.8 by using 0.1M sodium hydroxide and acetonitrile (77 : 23, v/v), the flow rate used was 1 ml/min and detection was achieved at 235 nm using UV. Results: All peaks were sharp and well separated, the retention times were atenolol degradation (ATN Deg.) 2.311 min, atenolol (ATN) 2.580 min, hydrochlorothiazide degradation (HCT Deg.) 5.890 min, hydrochlorothiazide (HCT) 7.016 min, chlorthalidone degradation CTD Deg 8.018 min and chlorthalidone (CTD) 14.972 min. Linearity was obtained and the range of concentrations was 20- 160 μg/ml for atenolol, 10-80 μg/ml for hydrochlorothiazide and 10-80 μg/ml for chlorthalidone. According to ICH guidelines, method validation was accomplished, these methods include linearity, accuracy, selectivity, precision and robustness. Conclusion: The optimized method demonstrated to be specific, robust and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

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