scholarly journals A simple method for the quantification of diclofenac potassium in oral suspension by high-performance liquid chromatography with UV-detection

2013 ◽  
Vol 49 (3) ◽  
pp. 589-597 ◽  
Author(s):  
Alexandre Machado Rubim ◽  
Jaqueline Bandeira Rubenick ◽  
Luciane Varine Laporta ◽  
Clarice Madalena Bueno Rolim
Keyword(s):  
High Performance ◽  
Low Cost ◽  
Oral Suspension ◽  
Reverse Phase ◽  
Intermediate Precision ◽  
Simple Method ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Validation Parameters

A rapid, simple and low cost method was developed to determine diclofenac potassium (DP) in oral suspension, using a reverse-phase column (C8, 150 mm x 4.6 mm, 5 µm), mobile phase containing methanol/buffer phosphate (70:30 v/v, pH 2.5), at a flow rate of 1.0 mL/min, isocratic method, and ultraviolet detection at 275 nm. A linear response (r = 1.0000) was observed in the range of 10.0-50.0 µg/mL. Validation parameters such as linearity, specificity, precision, accuracy and robustness were evaluated. The method presented precision (repeatability: relative standard deviation = 1.21% and intermediate precision: between-analyst = 0.85%). The specificity of the assay was evaluated by exposure of diclofenac potassium under conditions of stress such as hydrolysis, photolysis, oxidation and high temperature. The method presented accuracy values between 98.28% and 101.95%. The results demonstrate the validity of the proposed method that allows determination of diclofenac potassium in oral suspension and may be used as an alternative method for routine analysis of this product in quality control.

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.

High Performance Liquid Chromatography with Fluorescence and Ultraviolet Detection of Polynuclear Aromatic Hydrocarbons in Barley Malt

1982 ◽  
Vol 65 (6) ◽  
pp. 1395-1402
Author(s):  
Frank L Joe ◽  
Jean Salemme ◽  
Thomas Fazio
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Aromatic Hydrocarbons ◽  
High Performance ◽  
Polynuclear Aromatic Hydrocarbons ◽  
Alumina Column ◽  
Reverse Phase ◽  
Barley Malt ◽  
Relative Standard

Abstract A simple, rapid method has been developed for the separation and determination of polynuclear aromatic hydrocarbons (PAHs) in barley malt. An ultrasonic- cyclohexane extraction method was used to separate the PAHs from ground barley malt. The cyclohexane extracts were purified by chromatography through a water-deactivated silica gel-alumina column. The eluate from the column was concentrated and purified further by partitioning between dimethyl sulfoxide (DMSO) and cyclohexane. The DMSO extract was diluted with water and the PAHs were extracted back into cyclohexane. The cyclohexane extract was washed with water, dried through sodium sulfate, and evaporated, and the resulting residue was dissolved in 80% aqueous acetonitrile-methanol (1 + 1) and subjected to reverse phase high performance liquid chromatography. Thirty barley malt samples were analyzed using this procedure. Peaks having the same retention time as the carcinogen benzo(a)pyrene were isolated from 18 of the samples, and were equivalent to trace levels ranging from <0.1 to 0.2 ppb. Average recoveries of 11 PAHs, including benzo(a)pyrene, benzo(b)fluoranthene, indeno(l,2,3-cd)pyrene, and benz(a)anthracene, added to 25 g samples at 2.5 and 5 ppb, ranged from 78 to 97%, with a mean relative standard deviation of 6.6%.

Rapid Method for Extraction and Reverse Phase Liquid Chromatographic Determination of Paraquat Residues in Water

1983 ◽  
Vol 66 (3) ◽  
pp. 663-666
Author(s):  
Ijaz Ahmad
Keyword(s):  
High Performance ◽  
Chromatographic Determination ◽  
High Performance Liquid Chromatographic ◽  
Reverse Phase ◽  
Ultraviolet Detection ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Low Levels ◽  
Liquid Chromatographic

Abstract A simple and fast analytical method is described for the quantitative determination of low levels of paraquat residues in water. The method involves extraction and concentration of paraquat in water by using a C18 Sep-Pak cartridge followed by reverse phase high performance liquid chromatographic determination with ultraviolet detection at 257 nm. Recoveries of paraquat from spiked samples were above 93% with a coefficient of variation of 6.1%. The method can be used for water samples with paraquat concentrations as low as 0.05 ppm.

scholarly journals Determination of Tianeptine in Tablets by High-Performance Liquid Chromatography with Fluorescence Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 720-724
Author(s):  
Sevgi Tatar Ulu
Keyword(s):  
Lower Limit ◽  
High Performance ◽  
Limit Of Detection ◽  
Internal Standard ◽  
Linear Calibration ◽  
Fluorescence Detector ◽  
Relative Standard ◽  
Validation Parameters ◽  
Limit Of Quantitation

Abstract A sensitive and selective high-performance liquid chromatographic method has been developed for the determination of tianeptine (Tia) in tablets. The method is based on derivatization of Tia with 4-chloro-7-nitrobenzofurazan (NBD-Cl). A mobile phase consisting of acetonitrile10 mM orthophosphoric acid (pH 2.5; 77 + 23) was used at a flow rate of 1 mL/min on a C18 column. The Tia-NBD derivative was monitored using a fluorescence detector, with emission set at 520 nm and excitation at 458 nm. Gabapentin was selected as an internal standard. Linear calibration graphs were obtained in the concentration range of 45300 ng/mL. The lower limit of detection (LOD) was 10 ng/mL at a signal-to-noise ratio of 4. The lower limit of quantitation (LOQ) was 45 ng/mL. The relative standard values for intra- and interday precision were <0.46 and <0.57%, respectively. The recovery of the drug samples ranged between 98.89 and 99.85%. No chromatographic interference from the tablet excipients was found. The proposed method was validated in terms of precision, robustness, recovery, LOD, and LOQ. All the validation parameters were within the acceptance range. The proposed method was applied for the determination of Tia in commercially available tablets. The results were compared with those obtained by an ultraviolet spectrophotometric method using t- and F-tests.

Determination of Chloramphenicol Residues in Aquatic Products Using Immunoaffinity Column Cleanup and High Performance Liquid Chromatography with Ultraviolet Detection

2013 ◽  
Vol 96 (4) ◽  
pp. 897-901 ◽  
Author(s):  
Qing-Jie Zhang ◽  
Tao Peng ◽  
Dong-Dong Chen ◽  
Jie Xie ◽  
Xiong Wang ◽  
...  
Keyword(s):  
High Performance ◽  
Low Cost ◽  
Ammonium Hydroxide ◽  
Optimal Conditions ◽  
Immunoaffinity Column ◽  
Ultraviolet Detection ◽  
Aquatic Products ◽  
Highly Sensitive ◽  
The Mean

Abstract A method based on HPLC with UV detection was developed for the quantitative determination of chloramphenicol (CAP) residues in aquatic products. The samples were extracted with ethyl acetate–ammonium hydroxide (98 + 2, v/v), followed by a cleanup step using an immunoaffinity column. The analytes were determined by HPLC-UV. Optimal conditions for the extraction and cleanup procedures are described. The linear regression equation was y = 91.47x – 8.60 with R2 = 0.9998 (y = peak area and x = CAP concentration) and showed a good reproducibility. The LOQ was 0.25 μg/kg for determining CAP spiked in the aquatic products. The mean recoveries of CAP from fish and shrimp samples fortified at 0.25–1.0 μg/kg were 88.7–93.1 and 92.0–97.3%, respectively; the repeatability RSDs were less than 8.1%. It was concluded that the method is simple, highly sensitive, and low cost for quantitatively measuring CAP residues in aquatic products. Analyte identification was confirmed by HPLC/MS/MS analysis.

Determination of Ivermectin in Medicated Swine Feeds at the 2 ppm Concentration Level

1990 ◽  
Vol 73 (6) ◽  
pp. 931-934
Author(s):  
Stephen J Doherty ◽  
Allen Fox ◽  
David W Fink
Keyword(s):  
Chromatographic Analysis ◽  
Concentration Level ◽  
Reverse Phase ◽  
Ultraviolet Detection ◽  
Mean Relative Error ◽  
Relative Standard ◽  
Liquid Chromatographic Analysis ◽  
Liquid Chromatographic ◽  
Medicated Feeds

Abstract An analytical method has been developed that Is applicable to the determination of Ivermectin in medicated feeds at the 2 ppm concentration level. It Is based upon liquid chromatographic analysis with a reverse-phase column and ultraviolet detection. After the drug Is extracted from the feed Into methanol, an analytical sample Is prepared by the consecutive use of column chromatography on alumina and solidphase extraction on Sep-Pak C18 and silica cartridges. This procedure has been applied to the concentration range 0.50- 3.0 ppm of Ivermectin In feed with an accuracy of ±2% mean relative error and a precision of ± 2% relative standard deviation at the 2 ppm concentration level.

scholarly journals Development of simple and sensitive HPLC method for determination of glyphosate residues in soybean

2015 ◽  
Vol 3 ◽  
pp. 21-26
Author(s):  
Om Prakash Sharma ◽  
Nanthanit Pholphana ◽  
Nuchanart Rangkadilok ◽  
Preeda Parkpian ◽  
Jutamaad Satayavivad
Keyword(s):  
High Performance ◽  
Limit Of Detection ◽  
Hplc Method ◽  
Reverse Phase Hplc ◽  
Intermediate Precision ◽  
Soybean Sample ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Residue Levels

The purpose of this study was to develop a simple and sensitive high performance liquid chromatography (HPLC) method for determination of glyphosate (GP) residues in soybean grains. From soybean matrix, glyphosate was extracted with a mixture of water and methanol (4:1, v/v) from soybean samples followed by protein precipitation with equal volume of methanol. No preconcentration and further clean up of the sample were required. Pre-column derivatization was carried out with excess amount of 9- fluorenylmethyl chloroformate (FMOC-Cl) in the presence of borate buffer. The gradient program developed in this method was successfully applied to a reverse phase HPLC system with a C18 column (ACE 5 μm 4.6 x 250 mm), and eluted with a mobile phase consisting of 50 mM phosphate buffer, pH 2.5, and acetonitrile at the flow rate of 0.8 ml/min and fluorescence detection. Parameters and conditions affecting extraction, derivatization reaction and chromatographic separation were systematically examined. Linearity of the method ranged from 0.005 - 1.0 μg/ml. The correlation coefficient (r2) of calibration curve for glyphosate in soybean sample was found to be 0.99929. The limit of detection (LOD) and limit of quantitation (LOQ) values were determined to be 0.125 mg/kg and 0.25 mg/kg, respectively. Average recovery was 95.2%. Repeatability and intermediate precision calculated on the basis of peak area were excellent and showed relative standard deviation ranged from 0.15 - 1.29% and 1.15 - 3.87%, respectively. The developed method has been successfully applied for determination of glyphosate residues in soybean grains obtained from Thailand and Nepal. Soybean samples (53) from two different lots were analyzed and glyphosate residues ranged from 0.23 mg/kg to 5.06 mg/kg. Almost 50% soybean samples contained nearly consistent residue levels in both lots but in remaining samples there was a significant variation of glyphosate levels between two lots. Relatively higher residues were detected in samples from Thailand (0.27-5.06 mg/kg) compared to Nepal (0.23-0.99 mg/kg). The results suggest that the proposed method can be used to determine glyphosate residues in foods derived from soybean and other crops such as corn, cotton, wheat, etc. where glyphosate is widely applied to these crops.

scholarly journals Determination of Available Lysine by Planar Chromatography: A Useful Tool for Protein Quality Evaluation in Fish Feed

2009 ◽  
Vol 92 (3) ◽  
pp. 699-702 ◽  
Author(s):  
Mario Vega ◽  
Mario Aranda
Keyword(s):  
Quality Control ◽  
High Throughput ◽  
Protein Quality ◽  
Low Cost ◽  
Fish Feed ◽  
Planar Chromatography ◽  
Intermediate Precision ◽  
Relative Standard ◽  
Available Lysine

Abstract Due to the essentiality of lysine for fish, its availability is commonly used as a predictor of the protein nutritional quality of fish feed. The objective of this work was to establish a high-throughput analytical method for protein quality control in fish feed through the measurement of available lysine by planar chromatography. Sample was first incubated with 1-fluoro-2,4-dinitrobenzene to obtain the dinitrophenyl-lysine derivative and then hydrolyzed with hydrochloric acid in order to release the derivative from proteins. Chromatography was performed on silica gel 60 F254 HPTLC plates using n-propanol25 ammonia (7 + 3, v/v) as mobile phase. Quantitative analysis was performed by densitometry in the absorbance mode at 360 nm. Calibration showed a polynomial relationship with an R2 of 0.9991 in the range of 25 to 125.0 ng/band. Repeatability relative standard deviation (RSD) and intermediate precision (RSD) in matrix were 0.8 and 3.6, respectively. Recoveries of spiked samples at two levels ranged from 72 to 85 with RSD from 3 to 8. This method provides the salmon feed industry with a reliable, high-throughput, and low-cost means for routine quality control of available lysine.

Sign in / Sign up

Export Citation Format

Share Document