scholarly journals A High-Performance Liquid Chromatography:Chemiluminescence Method for Potential Determination of Vardenafil in Dietary Supplement

2011 ◽  
Vol 2011 ◽  
pp. 1-6 ◽  
Author(s):  
Youjun Di ◽  
Min Zhao ◽  
Yingchun Nie ◽  
Fei Wang ◽  
Jiagen Lv
Keyword(s):  
Aqueous Solution ◽  
Mobile Phase ◽  
High Performance ◽  
Ethylenediaminetetraacetic Acid ◽  
Disodium Salt ◽  
Relative Standard ◽  
Oral Liquid ◽  
Interday Precision ◽  
Ethylenediaminetetraacetic Acid Disodium Salt

A flow method of high-performance liquid chromatography (HPLC) seperation and chemiluminescence (CL) detection for sensitive vardenafil analysis in dietary supplements was developed. The vardenafil separation was achieved on a C18 column at 30∘C using ethanol-H3PO4and ethylenediaminetetraacetic acid disodium salt (Na2EDTA) aqueous solution (25 : 75, v/v%) as mobile phase. The followed continuous CL detection was conducted based on the strong CL enhancement by the presence of vardenafil to luminol-K3Fe(CN)6reaction in alkaline medium. At the flow rate of 0.8 mL/min, the vardenafil retention time () was 6.4 min. Factors that affected the HPLC resolution and CL detection were studied and optimized. The calibration curve obtained for vardenafil standard was linear in concentration range of  mol/L. The relative standard deviations (RSD) of intraday and interday precision were less than 3.5%. The proposed method was applied to the vardenafil determination in oral liquid, wine, and capsule samples.

scholarly journals SENSITIVE DETERMINATION OF RELATED SUBSTANCES IN PIOGLITAZONE HYDROCHLORIDE BY HPLC

2017 ◽  
Vol 9 (2) ◽  
pp. 34
Author(s):  
N. Balaji ◽  
Sayeeda Sultana
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Internal Diameter ◽  
Related Substances ◽  
Relative Standard ◽  
Limit Of Quantitation

Objective: An efficient, high performance liquid chromatographic method has been developed and validated for the quantification of related substances in pioglitazone hydrochloride drug substance.Methods: This method includes the determination of three related substances in pioglitazone hydrochloride. The mobile phase A is 0.1% w/v triethylamine in water with pH 2.5 adjusted by dilute phosphoric acid. The mobile phase B is premixed and degassed mixtures of acetonitrile and methanol. The flow rate was 1 ml/min. The elution used was gradient mode. The HPLC column used for the analysis was symmetry C18 with a length of 250 mm, the internal diameter of 4.6 mm and particle size of 5.0 microns.Results: The developed method was found to be linear with the range of 0.006-250% with a coefficient of correlation 0.99. The precision study revealed that the percentage relative standard deviation was within the acceptable limit. The limit of detection and limit of quantitation of the impurities was less than 0.002%and 0.006% with respect to pioglitazone hydrochloride test concentration of 2000 µg/ml respectively. This method has been validated as per ICH guidelines Q2 (R1).Conclusion: A reliable, economical HPLC method was magnificently established for quantitative analysis of related substances of pioglitazone hydrochloride drug substance.

scholarly journals Development and validation of reversed phase high performance liquid chromatography (RP-HPLC) for quantification of captopril in rabbit plasma

2020 ◽  
Author(s):  
Muhammad Fawad Rasool ◽  
Umbreen Fatima Qureshi ◽  
Nazar Muhammad Ranjha ◽  
Imran Imran ◽  
Mouqadus Un Nisa ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Reversed Phase ◽  
Rabbit Plasma ◽  
Rp Hplc ◽  
Relative Standard

AbstractTh accurate rapid, simple and selective reversed phase high performance liquid chromatography (RP-HPLC) has been established and validated for the determination of captopril (CAP). Chromatographic separation was accomplished using prepacked ODSI C18 column (250 mm × 4.6 mm with 5 μm particle size) in isocratic mode, with mobile phase consisting of water: acetonitrile (60:40 v/v), pH adjusted to 2.5 by using 85% orthophosphoric acid at a flow rate of 1 mL/min and UV detection was performed at 203 nm. RP-HPLC method used for the analysis of CAP in mobile phase and rabbit plasma was established and validated as per ICH-guidelines. It was carried out on a well-defined chromatographic peak of CAP was established with a retention time of 4.9 min and tailing factor of 1.871. The liquid–liquid extraction method was used for extraction of CAP from the plasma. Excellent linearity (R2 = 0.999) was shown over range 3.125–100 µg/mL with mean percentage recoveries ranges from 97 to 100.6%. Parameters of precision and accuracy of the developed method meet the established criteria. Intra and inter-day precision (% relative standard deviation) study was also performed which was less than 2% which indicate good reproducibility of the method. The limit of detection (LOD) and quantification for the CAP in plasma were 3.10 and 9.13 ng/mL respectively. The method was suitably validated and successfully applied to the determination of CAP in rabbit plasma samples.

High Performance Liquid Chromatographic Determination of Primidone in Tablets

1982 ◽  
Vol 65 (5) ◽  
pp. 1063-1065
Author(s):  
Stanley E Roberts
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Hplc Method ◽  
Average Recovery ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A high performance liquid chromatographic (HPLC) method is described for the quantitative determination of primidone in tablets. A ground tablet sample is diluted directly in the mobile phase, at a concentration of about 1 mg/mL of primidone, mixed and deaerated, and filtered. The resulting solution is then quantitated by HPLC. The average spike recoveries for the 50 mg and 250 mg tablets were 101.2% and 99.0%, respectively. The average recovery for an authentic mixture formulated at the 250 mg level was 100.1% with a relative standard deviation of 0.45%.

scholarly journals RP-LC method for simultaneous determination of sulfamethoxazole and trimethoprim content in veterinary drugs

2015 ◽  
Vol 40 (1) ◽  
pp. 32 ◽  
Author(s):  
Gabriela Padovani Tahan ◽  
Simone Caetani Machado ◽  
Evandro Conti Malaguti ◽  
Patrícia Penido Maia ◽  
Susanne Rath ◽  
...  
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Simultaneous Analysis ◽  
Ultraviolet Detector ◽  
Veterinary Medicines ◽  
Alternative Approach ◽  
Relative Standard ◽  
Water Ph ◽  
Comparison Of The Results

This study describes the development of a method for simultaneous analysis of sulfamethoxazole (SMX) and trimethoprim (TMP) through the use of high-performance liquid chromatography/ultraviolet detector, with the application to veterinary medicines. Satisfactory chromatographic separation of SMX and TMP was isocratically with a C18 column (150 x 4.6 mm, 5 mm). A mobile phase consisting of water, pH 3.5, and methanol (60:40, v/v) was delivered at a flow rate of 1.0 mL min-1 for five minutes and then, increased to 1.8 mL min-1. Detection of the drugs was performed at 213 and 230 nm. Linearity was demonstrated in the range of 5 to 70 mg mL-1 for SMX and 1 to 30 mg mL-1 for TMP (r2 ≥ 0.99 for both compounds). The relative standard deviation was ≤ 5%, and the comparison of the results with the concentrations reported on the drug labels indicated that the quantification was accurate. The resultant stressed samples were analysed by the method. The proposed method shows great potential for simultaneous analysis of the drugs evaluated and represents a new alternative approach to quality control of veterinary medicines.

scholarly journals High performance liquid chromatographic method for the determination of ambroxol hydrochloride in presence of antimicrobial preservatives in oral liquid formulation

2015 ◽  
Vol 18 (1) ◽  
pp. 8-14 ◽  
Author(s):  
T Sudha ◽  
K Manthena ◽  
VR Ravikumar ◽  
V Ganesan
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Methyl Paraben ◽  
Propyl Paraben ◽  
Liquid Chromatographic Method ◽  
Oral Liquid ◽  
Ambroxol Hydrochloride ◽  
Liquid Chromatographic

A simple gradient reversed phase high performance liquid chromatographic method was developed for the determination of ambroxol hydrochloride in presence of antimicrobial preservatives in oral liquid formulation. The chromatographic separation was achieved by an Inertsil C8 (250 X 4.6 mm, 5? particle size) column using gradient technique. The eluents were detected at 245 nm with photodiode array detector. The optimized mobile phase consisted of 0.1% trifluoroacetic acid as a mobile phase A and a mixture of mobile phase A and acetonitrile in the ratio of 76:24 % v/v as mobile phase B. Ambroxol hydrochloride and microbial preservatives were eluted at a flow rate of 1.0 ml/min. The method validated according to the International Conference of Harmonization (ICH) guidelines. The calibration curves were linear over the (r2 > 0.99) concentrations range from 300 to 900 ppm for ambroxol hydrochloride, 10 to 30 ppm for propyl paraben and 100 to 300 ppm for methyl paraben. The limit of detection was found to be 0.024 ppm for ambroxol hydrochloride, 0.018 ppm for propyl paraben and 0.009 ppm for methyl paraben. The percentage recoveries were found to be in the range from 99.55 to 101.1% for ambroxol hydrochloride, 100.31 to 101.46% for propyl paraben and 98.18 to 101.61% for methyl paraben. Stability indicating capability was established by forced degradation experiments. No chromatographic interference from the degradation products was found. The proposed method was highly sensitive, precision and accurate and hence successfully applied for the quantification of ambroxol active pharmaceutical ingredients (API) and preservatives content in the commercially available oral liquid formulation.Bangladesh Pharmaceutical Journal 18(1): 8-14, 2015

scholarly journals New High-Performance Liquid Chromatographic Method for Determination of Clopidogrel in Coated Tablets

2008 ◽  
Vol 91 (1) ◽  
pp. 67-72 ◽  
Author(s):  
Juliana Sippel ◽  
Letcia L Sfair ◽  
Elfrides E S Schapoval ◽  
Martin Steppe
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Chromatographic Method ◽  
High Performance Liquid Chromatographic ◽  
Array Detector ◽  
Aqueous Sample ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic

Abstract A new high-performance liquid chromatographic method was developed and validated for clopidogrel determination in pharmaceutical formulations. The system consisted of an ACE 5 octadecylsilane (C18; 150 4.6 mm id), 5.0 m particle size column; methanol0.1 triethylamine (75 + 25, v/v), pH 5.3, mobile phase at a flow rate of 1.2 mL/min; and a diode array detector set at 220 nm. Specificity, linearity, precision, accuracy, and robustness were the parameters evaluated. The retention time for clopidogrel was 6.8 min. To estimate specificity, an aqueous sample solution was subjected to degradation by ultraviolet light and by acid, alkaline, and oxidation media. The peaks of degradation products did not interfere with the compound signal, and there was no interference when a placebo solution was analyzed. Linearity over a concentration range of 10.0 to 90.0 g/mL was shown (correlation coefficient = 0.9998). Low values of relative standard deviation indicated the adequate intraday and interday precision. The average recovery was found as 99.16. In the robustness test, small modifications to the mobile phase composition did not affect the determination of clopidogrel. The proposed method proved to be simple, fast, and cost efficient for the intended use.

scholarly journals SIMULTANEOUS DETERMINATION OF PARACETAMOL AND IBUPROFENE MIXTURES BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY

2010 ◽  
Vol 3 (1) ◽  
pp. 9-13 ◽  
Author(s):  
Sophi Damayanti ◽  
Slamet Ibrahim ◽  
Kurnia Firman ◽  
Daryono H Tjahjono
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Standard Deviation ◽  
Retention Time ◽  
Analytical Method ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Relative Standard

Analytical method for the determination of paracetamol and ibuprofene mixtures has been developed by High Performance Liquid Chromatography using C-18 column and acetinitrile - phosphate buffer pH = 4.5 (75:25) containing 0.075% sodium hexanesulfunate as a mobile phase. The detector was set at 215 nm. Using such conditions, retention time for paracetamol and ibuprofen was 4.89 and 7.11 min, respectively. The recovery for paracetamol and ibuprofen was found to be 101.07± 0.73% and 102.02 ± 1.58%, respectively. The detector limits of the method was 1.30 and 1.60 μg/mL with the relative standard deviation (RSD) 0.74 and 1.52% for paracetamol and ibuprofen, respectively.   Keywords: paracetamol, ibuprofen, multi-component, validation, HPLC.

Rapid Determination of Metronidazole and 2-Hydroxymetronidazole in Murine Blood Plasma

2021 ◽  
Author(s):  
Nina Zemanová ◽  
Pavel Anzenbacher ◽  
Tomáš Hudcovic ◽  
Eva Anzenbacherová
Keyword(s):  
Plasma Proteins ◽  
Mobile Phase ◽  
High Performance ◽  
Rapid Determination ◽  
Internal Standard ◽  
Hplc Method ◽  
Primary Metabolite ◽  
Relative Standard ◽  
Protozoan Infections

Abstract Metronidazole is a drug used to treat bacterial and protozoan infections. Nowadays, it is one of the most frequently prescribed drugs worldwide. The main aim of this paper is to present a rapid, reliable and simple high-performance liquid chromatography (HPLC) method to determine metronidazole along with its primary metabolite, 2-hydroxymetronidazole, in plasma or serum using paracetamol as an internal standard. A total of 100% methanol was used to denature plasma proteins. After centrifugation, the supernatant was evaporated under nitrogen flow. The samples were dissolved in the mobile phase and injected into a Li-Chrospher RP-18 column. A total of 10 mmol/L NaH2PO4: acetonitrile (90:10, v/v) solution with a flow rate of 1 mL/min was used as the mobile phase. Metronidazole and 2-hydroxymetronidazole were detected at two different wavelengths at 320 nm and 311 nm, respectively. The method is characterized by high precision (relative standard deviation % < 6). The method was used for the determination of metronidazole and 2-hydroxymetronidazole in murine blood using small amounts of plasma (≤100 μL).

scholarly journals Determination of the Insecticide Imidacloprid in Fruit Juices Using Micellar High-Performance Liquid Chromatography

2009 ◽  
Vol 92 (5) ◽  
pp. 1551-1556 ◽  
Author(s):  
Mei-Liang Chin-Chen ◽  
Josep Esteve-Romero ◽  
Samuel Carda-Broch
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Quality Evaluation ◽  
Sodium Dodecyl ◽  
Hplc Method ◽  
Fruit Juices ◽  
Food Control ◽  
Specific Affinity ◽  
Interday Precision

Abstract A simple and reliable HPLC method was developed to determine imidacloprid, a chloronicotinyl insecticide that has a highly specific affinity to the nicotinic acetylcholine receptor of insects, above its permissible limit of consumption in fruit juices (orange, apple, and a mixture of pineapple and pear). Samples were injected directly into a Kromasil C18 column, without any pretreatment step, using the micellar mobile phase 0.10 M sodium dodecyl sulfate and 2.5 (v/v) propanol buffered at pH 7 and UV detection at 210 nm. Under these conditions, imidacloprid was eluted in <4 min with no interference by the endogenous compounds of the juice fruits. The analytical parameters linearity (r > 0.9998) and intraday and interday precision (RSD 0.1 2.8 and 0.077, respectively) were obtained in the method validation. LOD and LOQ were calculated to be 0.4 and 1.5 ng/mL, respectively. Recoveries were in the 98103 range. The simplicity of the method makes it a good candidate for application in routine analysis in the area of food control and quality evaluation.

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