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 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 HPLC methods of fexofenadine quantitative analysis in rabbits’ liver

2020 ◽  
Vol 8 (1) ◽  
pp. 40-47
Author(s):  
P. Yu. Mylnikov ◽  
I. V. Chernykh ◽  
A. V. Shchulkin ◽  
N. M. Popova ◽  
E. N. Yakusheva
Keyword(s):  
Quantitative Determination ◽  
Functional Activity ◽  
Mobile Phase ◽  
High Performance ◽  
Methylene Chloride ◽  
Test Tube ◽  
Hepatic Tissue ◽  
Ultraviolet Detector ◽  
P Glycoprotein

The investigation of pharmacokinetics of marker substrates of carrier protein P-glycoprotein (Pgp, ABCB1-protein) including fexofenadine, is one of the methods of its functional activity evaluation.The aim of the study was to work out the HPLC methods of the quantitative determination of fexofenadine in rabbits’ liver.Materials and methods. The quantitative determination of fexofenadine was performed using Stayer chromatographic system (Akvilon, Russia) with UVV 104 ultraviolet detector. Reverse-phased chromatographic column Luna C18 100Å (250*4.6) was used with 5 µm granulation at 45°С. The сoncentration of fexofenadine was determined by methods of absolute peak area calibration.Results. The work was conducted in the isocratic mode. The composition of the mobile phase consisted of deionized water, acetonitrile and glacial acetic acid at the ratio of 267.4:120:4.33 brought to pH=6.7 with triethylamine. The sample processing was in the form of homogenization of 500 mg of ground liver in 500 µl of purified water with the subsequent centrifugation (1750 g) and selection of the supernatant. The proteins were precipitated by acetonitrile (2.5 ml) acidified with 375 µl of hydrochloric acid by shaking at 500 rev/min. The supernatant was transported into a separate test tube, where methylene chloride, diethyl ether and ethyl acetate were added (2 ml each). Then the solution was again shaken for 10 minutes (500 rev/min). After that, the solution was centrifuged (1750 g) and the supernatant was evaporated on a rotor-vacuum evaporator at 50°С. 300 µl of the mobile phase was added to the dry residue, and 100 µl was injected into the chromatograph. The method was validated in the linear range from 3 to 60 µg/g of fexofenadine with the acceptable intra- and intercycle accuracy, precision and stability. The method was tested on rabbits after the intravenous administration of fexofenadine at the dose of 11 mg/kg.Conclusion. The HPLC methods of fexofenadine quantitative determination in the hepatic tissue of rabbits has been worked out. It can be used for the evaluation of the functional activity of Pgp in preclinical studies.Abbreviations: Pgp – P-glycoprotein, HPLC – high performance liquid chromatography, rev/min – revolutions per minute

scholarly journals Determining the Levels of Four Phenylethanoid Glycosides and Five Triterpene Acids in Liuwei Dihuang Capsule Using Solid Phase Extraction with HPLC-UV

2019 ◽  
Vol 2019 ◽  
pp. 1-9
Author(s):  
Yong Zhang ◽  
Xian-Liang Zou ◽  
Yong-Li Wang ◽  
Lu Gao ◽  
Gui-Xin Chou
Keyword(s):  
Solid Phase Extraction ◽  
High Performance ◽  
Solid Phase ◽  
Phase Extraction ◽  
Phenylethanoid Glycosides ◽  
Triterpene Acids ◽  
Ultraviolet Detector ◽  
Relative Standard ◽  
Removal Of Impurities

In this study, we used quantitative high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV) and solid phase extraction (SPE) to determine the levels of four phenylethanoid glycosides and five triterpene acids in Liuwei Dihuang capsules (LDCs). LDCs were methanol-extracted and purified using a 500 mg/6 mL silica-based C18 SPE cartridge. Two elutions were analyzed on a ChromCore C18 column under two HPLC conditions. To improve the pretreatment clean-up, an array of silica- and polymer-based SPE cartridges were compared. Both wash and elution steps were also optimized to achieve the highest removal of impurities. Under optimal chromatographic conditions, good linearity was achieved for all compounds (correlation coefficient of r ≥ 0.999), with a quantification limit ranging from 0.0076 to 0.418 μg/mL. The method had satisfactory efficiency and reproducibility with recovery rates ranging from 91.6 to 99.3% with a relative standard deviation below 1.5%. Taken together, this demonstrated SPE as a suitable extension of HPLC-UV for the determination of phenylethanoid glycosides and triterpene acids in complex LDCs.

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 MÉTODO PARA DETERMINAÇÃO DE RESÍDUOS DE CLORPIRIFÓS EM ALFACE POR CROMATOGRAFIA A LÍQUIDO DE ALTA EFICIÊNCIA

2003 ◽  
Vol 13 ◽  
Author(s):  
MARILENA FERREIRA PENA ◽  
ELIANE HOOPER AMARAL ◽  
EDUARDO VON SPERLING ◽  
IVAN CRUZ
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Residual Analysis ◽  
Average Recovery ◽  
Ultraviolet Detector

Este trabalho propõe método de análise de resíduos de Clorpirifós em amostras de alface por cromatografia a líquido de alta eficiência (CLAE). A análise foi realizada em cromatógrafo Shimadzu, com detector de ultravioleta ajustado em 229 nm, Coluna C-18, modelo Zorbax ODS (4,6 mm x 25 cm, 5 µm), fluxo de 1 mL/min e temperatura de 35ºC. Usou-se Metanol:Água (82:18) como fase móvel e volume injetado de 50 µL. Amostras de alface (20 g) foram trituradas e homogeneizadas na presença de 50 mL de Diclorometano (DCM). O material foi filtrado a vácuo e evaporado a temperatura de 50ºC. O resíduo foi retomado com fase móvel, agitado, desgaseificado, filtrado em membrana 0,22 µm e injetado no cromatógrafo (injetor automático). Os resultados do teste de repetitividade mostraram recuperação média de 101,91%. O método proposto é simples e rápido para determinação de resíduos de Clorpirifós em amostras de alface. METHOD FOR THE DETERMINATION OF CHLORPIRYFOS RESIDUES IN LETTUCE BY USING HPLC (High Performance Liquid Cromatograph) Abstract This paper suggests a method for the residual analysis of chlorpiryfos in lettuce samples by using HPLC (High Performance Liquid Cromatograph). The analysis has been carried out in a Shimadzu cromatograph, with ultraviolet detector adjusted to 229 nm, column C-18, model Zorbax ODS (4.6 mm x 25 cm, 5 µm), flux 1mL/min, temperature of 350C. The mobile phase used was methanol:water (82:18) and the injected volume of 50 µL. Lettuce samples have been triturated and homogenized in the presence of 50 mL of the solvent Dichlormethan (DCM). The vacuum filtered material was evaporated at the temperature of 500C. The residue has been retaken in a mobile phase, stirred, degasified, filtered in a 0.22 µm membrane and automatically injected in the HPLC. Good results were obtained in a repetitivity test, with an average recovery of 101.91%. The proposed test presents simplicity and quickness in the residual determination of Chlorpiryfos in lettuce samples.

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).

Quantification of Pyrazinamide in Human Plasma by Validated High Performance Liquid Chromatography Method

2021 ◽  
Vol 15 (10) ◽  
pp. 2896-2899
Author(s):  
Waleed Arshad ◽  
Naseem Saud Ahmad ◽  
Abdul Muqeet Khan ◽  
Iram Imran ◽  
Qura- Tul-Ain ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Plasma ◽  
Mobile Phase ◽  
High Performance ◽  
Ultra Violet ◽  
Chromatography Method ◽  
Ultraviolet Detector ◽  
Relative Standard ◽  
Liquid Chromatography Method

Objective: To be able to accurately determine the quantity of Pyrazinamide (PZA) in different tablet preparations and human plasma using an Ultra violet detector equipped high performance liquid chromatography (HPLC). Study Design: Experimental study Place and Duration of Study: Department of Bioequivalence Studies, University of Veterinary and Animal Sciences Lahore and the Department of Pharmacology, University of Health Sciences, Lahore the from 1st April 2017 to 31st March 2018. Methodology: Two mobile phases were used, the first compromised of disodium hydrogen phosphate buffer having a pH of 6.8 and acetonitrile in the proportion of (95:5) and the second was a combination of aforesaid substances in equivalent proportion (50:50 v/v). The gradient for the first 5 min was exclusively Mobile phase “a” after which 5-6 min Mobile phase “b” was raised from 0 to 100% and was kept at 100% till the completion of the cycle. The flow of mobile phase was kept at 1000 µl/min. Determination of PZA was done using a ultraviolet detector at a wavelength of 238 nm. Amount of sample injected was 40 μl. Procedure was done by using Shizmadu Chromatographic System, Japan equipped with a SIL-20AC HT auto-sampler, SPD-M20A, CTO 20 AC, a LC-20AT VP pump, and CBM 20A controller unit. A C18 column was used as well. Results: Retention time of PZA was 6.1±2%. Precision was 0.46 to 2.20% relative standard deviation for intra assay and for inter assay we obtained 0.29 to 34.45% RSD for all quality control levels. The overall recovery of PZA was 96.75%. Conclusion: High selectivity for PZA was seen and no other spikes from drugs present in FDC regimen were observed at the time when PZA is detected in blank plasma samples Key words: Chromatography, High pressure liquid. Pyrazinamide. Tuberculosis

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