scholarly journals Determination of Finasteride in Tablets by High Performance Liquid Chromatography

2007 ◽  
Vol 4 (1) ◽  
pp. 109-116 ◽  
Author(s):  
K. Basavaiah ◽  
B. C. Somashekar
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Calibration Graph ◽  
Official Method ◽  
Pharmaceutical Dosage Forms ◽  
Bulk Drug ◽  
Liquid Chromatographic

A rapid, highly sensitive high performance liquid chromatographic method has been developed for the determination of finasteride(FNS) in bulk drug and in tablets. FNS was eluted from a ODS C18reversed phase column at laboratory temperature (30 ± 2°C) with a mobile phase consisting of methanol and water (80+20) at a flow rate of 1 mL min-1with UV detection at 225 nm. The retention time was ∼ 6.1 min and each analysis took not more than 10 min. Quantitation was achieved by measurement of peak area without using any internal standard. Calibration graph was linear from 2.0 to 30 μg mL-1with limits of detection (LOD) and quantification (LOQ) being 0.2 and 0.6 μg mL-1, respectively. The method was validated according to the current ICH guidelines. Within-day co efficients of variation (CV) ranged from 0.31 to 0.69% and between-day CV were in the range 1.2-3.2%. Recovery of FNS from the pharmaceutical dosage forms ranged from 97.89 – 102.9 with CV of 1.41-4.13%. The developed method was compared with the official method for FNS determination in its tablet forms.

scholarly journals Development of a New High-Performance Liquid Chromatographic Method for the Determination of Ceftazidime

2008 ◽  
Vol 91 (4) ◽  
pp. 739-743 ◽  
Author(s):  
Andréia de Haro Moreno ◽  
Hérida Regina Nunes Salgado
Keyword(s):  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Calibration Graph ◽  
Raw Material ◽  
Relative Standard ◽  
Validation Parameters ◽  
Liquid Chromatographic

Abstract A rapid, accurate, and sensitive high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of ceftazidime in pharmaceuticals. The method validation parameters yielded good results and included range, linearity, precision, accuracy, specificity, and recovery. The excipients in the commercial powder for injection did not interfere with the assay. Reversed-phase chromatography was used for the HPLC separation on a Waters C18 (WAT 054275; Milford, MA) column with methanolwater (70 + 30, v/v) as the mobile phase pumped isocratically at a flow rate of 1.0 mL/min. The effluent was monitored at 245 nm. The calibration graph for ceftazidime was linear from 50.0 to 300.0 g/mL. The values for interday and intraday precision (relative standard deviation) were <1. The results obtained by the HPLC method were calculated statistically by analysis of variance. We concluded that the HPLC method is satisfactory for the determination of ceftazidime in the raw material and pharmaceuticals.

Liquid-chromatographic determination of 4-aminopyridine in serum, saliva, and urine.

1981 ◽  
Vol 27 (3) ◽  
pp. 437-440 ◽  
Author(s):  
D R Uges ◽  
P Bouma
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Drug Concentrations ◽  
Liquid Chromatographic Determination ◽  
High Concentrations ◽  
Liquid Chromatographic

Abstract We have developed "high-performance" liquid-chromatographic methods for determining 4-aminopyridine, an acetylcholine-releasing drug, in serum, saliva, and urine. As little as 1 microgram/L can be detected by extracting the alkalinized sample plus the internal standard (3,4-diaminopyridine) into dichloromethane, mixing the organic phase with 1-pentanol, evaporating the dichloromethane, and injecting the residue onto a reversed-phase column, where it is eluted with acetonitrile/methanol/aqueous ammonium carbonate, with detection at 245 nm. Analytical recoveries from serum averaged 86.7%. The CV at 50 micrograms/L was 2.9% (n = 8). For urine samples containing very high concentrations of 4-aminopyridine, we mixed urine and potassium carbonate in an automatic injector vial, extracted the drug into dichloromethane, centrifuged, and injected an aliquot of the extract into the chromatograph. Analytical recoveries averaged 92%, and the CV was about 2% for drug concentrations of 0.1-8 mg/L of urine.

A high-performance liquid-chromatographic method for routine simultaneous determination of nicotine and cotinine in plasma.

1988 ◽  
Vol 34 (4) ◽  
pp. 724-729 ◽  
Author(s):  
M Hariharan ◽  
T VanNoord ◽  
J F Greden
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Methylene Chloride ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Standard Curve ◽  
Liquid Chromatographic

Abstract We describe a rapid, sensitive method for the routine simultaneous determination of nicotine and cotinine in 1 mL of plasma. Extraction in 10-mL screw-capped Teflon tubes with methylene chloride after deproteinization with trichloroacetic acid eliminated emulsion formation. The extract, after evaporation and reconstitution in 30 microL of mobile phase, is injected into a reversed-phase C-18 ion-pair column of an isocratic high-performance liquid-chromatographic unit. Absorbance is monitored at 256 nm. The mobile phase is a citrate-phosphate (30 mmol each per liter) buffer mixture containing 50 mL of acetonitrile and 1 mmol of sodium heptanesulfonate per liter. 2-Phenylimidazole is the internal standard. The detection limit is 1 microgram/L for nicotine and 3 micrograms/L for cotinine. The standard curve is linear from 0 to 700 micrograms/L for both compounds. The average CV for nicotine in the concentration range 0-100 micrograms/L is 6.5%, and that for cotinine in the concentration range 50-700 micrograms/L is 4%.

Simultaneous liquid-chromatographic determination of prednisone and prednisolone in plasma.

1988 ◽  
Vol 34 (9) ◽  
pp. 1897-1899 ◽  
Author(s):  
M H Cheng ◽  
W Y Huang ◽  
A I Lipsey
Keyword(s):  
High Performance ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Liquid Chromatographic Determination ◽  
Standard Solution ◽  
Liquid Chromatographic

Abstract This high-performance liquid-chromatographic (HPLC) method for simultaneous determination of prednisone and its metabolite, prednisolone, in plasma is a modification of the method of Frey et al. (Clin Chem 1979;25:1944-7). Heparinized plasma (1.0 mL) with 0.1 mL of internal standard solution (11-deoxy-17-hydroxycorticosterone, 2 mg/L) is extracted with 7.0 mL of dichloromethane, then washed sequentially with 0.1 mol/L HCl, 0.1 mol/L NaOH, and deionized water, 2.0 mL each. The extract is evaporated and the residue reconstituted with 75 microL of mobile phase, methanol/H2O (40/60 by vol). Thirty microliters of this is injected onto a reversed-phase C6 column, which is eluted at 1.4 mL/min. Analytical recoveries of prednisone and prednisolone were 94-98% and 102-106%, respectively. Day-to-day precision (CV) was 3.8% for prednisone, 6.1% for prednisolone. We encountered no interference from the 21 other steroids and 25 drugs tested. This method is simple, accurate, and precise.

Liquid-chromatographic determination of alpha- and gamma-tocopherols in erythrocytes, with fluorescence detection.

1983 ◽  
Vol 29 (10) ◽  
pp. 1840-1842 ◽  
Author(s):  
J Lehmann ◽  
H L Martin
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We have adapted to erythrocytes a method for the determination of alpha- and gamma-tocopherols in plasma and platelets. Erythrocytes (50 microL) were extracted with methanol containing tocol (internal standard) and pyrogallol. Tocopherols were partitioned into chloroform, washed, and injected in methanol onto a reversed-phase (C18) "high-performance" liquid-chromatographic column. The mobile phase was methanol/water (99/1 by vol) at a flow rate of 2 mL/min and detection was with a "high-performance" spectrophotofluorometer. The limit of detection for either tocopherol is 0.10 microgram/mL of packed cells. Analytical recoveries ranged from 93 to 104%. Some values for tocopherols in human erythrocytes are presented.

Liquid-chromatographic determination of propisomide and its mono-N-dealkylated metabolite in plasma and urine.

1985 ◽  
Vol 31 (7) ◽  
pp. 1222-1224 ◽  
Author(s):  
G Houin ◽  
J P Jeanniot ◽  
P Ledudal ◽  
J Barré ◽  
J P Tillement
Keyword(s):  
High Performance ◽  
Clinical Sample ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Unchanged Drug ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe a "high-performance" liquid-chromatographic assay for simultaneously determining propisomide and its mono-N-dealkylated metabolite in plasma and urine. After extraction with dichloromethane at alkaline pH, the unchanged drug, its metabolite, and the internal standard are separated by liquid chromatography on a reversed-phase column and the absorbance of the eluate is measured at 254 nm. Selectivity, sensitivity, and reproducibility are excellent. Results are similar to those by gas chromatography for propisomide but, in addition, the metabolite can be simultaneously measured in the same clinical sample. We also report results by this method for blood and plasma samples from a volunteer receiving a single 200-mg dose of propisomide.

scholarly journals Column Reversed-Phase High-Performance Liquid Chromatographic Method for Simultaneous Determination of Rabeprazole Sodium and Domperidone in Combined Tablet Dosage Form

2008 ◽  
Vol 91 (2) ◽  
pp. 344-348 ◽  
Author(s):  
Shweta Sadanand Sabnis ◽  
Nilesh Dnvandev Dhavale ◽  
Vijay Yeshawantrao Jadhav ◽  
Santosh Vilashchand Gandhi
Keyword(s):  
Simultaneous Determination ◽  
High Performance ◽  
Dosage Form ◽  
Internal Standard ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Rabeprazole Sodium ◽  
Tablet Dosage ◽  
Liquid Chromatographic

Abstract A new, simple column reversed-phase high-performance liquid chromatographic (HPLC) method for simultaneous determination of rabeprazole sodium (RAB) and domperidone (DOM) in a combined tablet dosage form has been developed and validated. Determination was performed using a Jasco HPLC system with a HiQ SiL octadecylsilane (C18) column (250 4.6 mm id), acetonitrile0.1 M ammonium acetate (50 + 50, v/v) mobile phase, and paracetamol as an internal standard. The detection was performed using a UV detector set at 280 nm. The method was validated with respect to linearity, accuracy, precision, and robustness. Beer's law was obeyed in the concentration range of 1.010.0 and 0.55.0 g/mL for RAB and DOM, respectively. The method has been successfully applied for the analysis of drugs in a pharmaceutical formulation.

Quantitative Analysis of 5-Hydroxymethylfurfural in Linezolid Injection by High Performance Liquid Chromatography

2020 ◽  
Vol 16 (8) ◽  
pp. 1059-1067
Author(s):  
Jéssica Maurício Batista ◽  
Christian Fernandes
Keyword(s):  
High Performance ◽  
Potassium Phosphate ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Official Method ◽  
Ph Variation ◽  
Drug Products ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic

Background: Linezolid is a synthetic broad-spectrum antibacterial belonging to the class of oxazolidinones. Linezolid for intravenous infusion is isotonized with dextrose. In acidic environment, the dehydration of dextrose produces furan derivatives, 5-hydroxymethylfurfural (5-HMF) being the main one. The determination of this degradation product is of fundamental importance, since there is evidence it is cytotoxic, genotoxic, mutagenic and carcinogenic. However, there is no official method for the determination of 5-HMF in drug products. Objective: The aim of this study was to develop and validate a high performance liquid chromatographic method to quantify 5-HMF in injection of linezolid. Methods: The chromatographic separation, after optimization, was performed on C18 (150 x 4.6 mm, 5 μm) column. Mobile phase was composed of 14 mM potassium phosphate buffer pH 3.0 ([H+] = 1.0 x 10-3) and methanol in gradient elution at 1.0 mL min-1. The injection volume was 10 μL and detection was performed at 285 nm. Results: The method was optimized and validated, showing selectivity, linearity in the range from 0.075 to 9.0 μg mL-1, precision (RSD ≤ 2.0%), accuracy (mean recovery of 100.07%) and robustness for temperature and pH variation. Conclusion: The method was shown to be adequate to determine 5-HMF in injection containing linezolid in routine analysis.

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