Determination of Gentamicin Sulf ate C1a, C2, and C1 Components by Ion Pair Liquid Chromatography with Electrochemical Detection

1983 ◽  
Vol 66 (1) ◽  
pp. 172-175
Author(s):  
Timothy A Getek ◽  
A Carol Haneke ◽  
George B Selzer

Abstract The 3 major components of gentamicin sulfate (C1a, C2, and C1) were separated by a liquid chromatographic method using a reverse phase C18 bonded silica gel column and an aqueous ion pair solvent system consisting of 0.015M pentanesulfonic acid sodium salt, 0.2M sodium sulfate, and 0.1% acetic acid. Individual C components as well as several unknown minor constituents were detected by an electrochemical flow cell with a glassy carbon working electrode set at a potential of +1.3 ± 0.1 V vs Ag/Agd. The analytical response was linear over a concentration range of 16-30 μg. A plot of peak areas vs concentration of C fractions yielded a correlation coefficient of 0.999 or better for the Cla, C2, and C1 components of gentamicin sulfate.

2012 ◽  
Vol 9 (3) ◽  
pp. 1327-1331 ◽  
Author(s):  
A. Narendra ◽  
D. Deepika ◽  
M. Mathrusri Annapurna

A reverse phase LC method was developed for the determination of Brimonidine in eye drops. Chromatography was carried on an Inertsil ODS 3V column (C18) using a mixture of Octane 1- sulfonic acid sodium salt (0.02M) (pH 3.5 ± 0.05) and acetonitrile (64:36 v/v) as mobile phase at a flow rate of 1 mL/min with UV detection at 254 nm. The drug was eluted at 4.636 min. The detector response was linear in the concentration range of 0.4–72 μg/mL. The limit of detection and limit of quantification were found to be 0.0561 and 0.1848 μg/mL respectively. The proposed method was validated as per the ICH guidelines and can be applied for the routine analysis of Brimonidine in eye drops.


1984 ◽  
Vol 67 (2) ◽  
pp. 321-324
Author(s):  
Carola H Spurlock ◽  
Horst G Schneider

Abstract Separate assay methods have been developed for the 2 components of an SO + 20 drug blend of bevantolol and hydrochlorothiazide (HCT) in admixtures with animal feed. Drug/diet admixtures are extracted with methanol for reverse phase ion-pair liquid chromatographic (LC) assay of bevantolol, and with acetonitrile for ultraviolet spectrophotometric assay of HCT. Bevantolol, a cardioselective beta blocker, is separated from soluble feed components with an RP-18 column, using methanol–water–acetic acid (60 + 40 + 1) containing 0.005M octanesulfonic acid, sodium salt, as ion-pairing reagent. HCT is determined spectrophotometrically in acetonitrile extracts, using a suitable blank extract as reference. Average recovery of HCT from an admixture of 0.5 mg blend/g diet is 94.5% ± 4.3 RSD and at 2.0 mg/g, 101.5% ± 3.5 RSD. Bevantolol recovery from the same admixtures is 101.8% ± 2.7 RSD and 99.0% ± 3.5 RSD, respectively, using the method as described.


1986 ◽  
Vol 69 (5) ◽  
pp. 825-826
Author(s):  
Donald Shostak ◽  
Clifford Klein

Abstract A liquid chromatographic method has been developed for determination of flucytosine in capsules. Flucytosine and p-aminobenzoic acid, the internal standard, are separated on a C18 reverse phase column using water-methanol-acetic acid mobile phase containing 1-octanesulfonic acid sodium salt. Compounds are detected photometrically at 285 nm. Mean assay results for 250 and 500 mg commercial capsules were 101.5% (n = 5) and 100.2% (n = 5) of declared, respectively. Mean recovery of flucytosine added to commercial capsules was 99.3 %.


1988 ◽  
Vol 71 (1) ◽  
pp. 53-55 ◽  
Author(s):  
Kenneth M Weaver ◽  
Michael E Neale ◽  
Ann Laneville

Abstract A method was developed for the detection and quantitation of piperine in Piper nigrum. A reverse-phase liquid chromatographic system equipped with a C18 column with detection at 340 nm was used. A rapid 1 h acetone extraction followed by solvent dilution was used to avoid sample cleanup. The detection limit is 3 ng injected piperine, with 97.5-100.5% recovery of added piperine.


1985 ◽  
Vol 68 (3) ◽  
pp. 545-546
Author(s):  
Michael Tsougros

Abstract A stability indicating liquid chromatographic method for the determination of diazepam in tablets was collaboratively studied by 6 laboratories. The method uses a Cig reverse phase column, a methanolwater mobile phase, p-tolualdehyde as the internal standard, and photometric detection at 254 nm. The collaborators were supplied with a synthetic tablet powder and 3 commercial tablet samples. The mean recovery of diazepam from the synthetic tablet powder was 100.2%. For all samples analyzed, the coefficient of variation was < 1.5%. The method has been adopted official first action.


1987 ◽  
Vol 70 (4) ◽  
pp. 689-691
Author(s):  
Abdel-Aziz M Wahbi ◽  
Mohammad A Abounassif ◽  
El-Rasheed A Gad-Kariem ◽  
Mahmoud W Ibrahim

Abstract A liquid chromatographic method for the individual determination of benzoic and cinnamic acids in 2 benzoin preparations is presented. The method specifies a reverse phase column and 0.01M KH2P04- methanol (85 + 15) as mobile phase at a flow rate of 1.8 mL/min, with detection at 254 nm. The method has been applied to 2 benzoin preparations and the results were compared with those from the British Pharmacopoeia method.


1989 ◽  
Vol 72 (2) ◽  
pp. 231-234 ◽  
Author(s):  
Mercedes Jalón ◽  
Majesús Peńa ◽  
Julián C Rivas

Abstract A reverse-phase liquid chromatographic method is described for the determination of carminic acid in yogurt. A C18 column is used with acetonitrile-1.19M formic acid (19 + 81) as mobile phase and diode array detection. Sample preparation includes deproteinization with papain and purification in a polyamide column. The relative standard deviation for repeated determinations of carminic acid in a commercial strawberry-flavored yogurt was 3.0%. Recoveries of carminic acid added to a natural-flavored yogurt ranged from 87.2 to 95.3% with a mean of 90.2%. The method permits measurement of amounts as low as 0.10 mg/kg.


1984 ◽  
Vol 67 (3) ◽  
pp. 653-655
Author(s):  
Malin Åkerblom ◽  
Gunborg Alex

Abstract Bentazon was selectively extracted as an ion pair with tetrabutylammonium ion into dichloromethane. This technique was used to clean up crop and soil samples before determination of bentazon by reverse phase liquid chromatography and UV detection. Recoveries from potatoes, cucumbers, wheat grain, and clay soil were 77–103%, with a detection limit of 0.02 mg/kg.


1984 ◽  
Vol 67 (3) ◽  
pp. 497-499
Author(s):  
Stephen C Slahck ◽  
◽  
J B Audino ◽  
O O Bennett ◽  
B D Folsom ◽  
...  

Abstract A liquid chromatographic method for the determination of propoxur in technical and formulated products has been subjected to a collaborative study with 8 participating collaborators. Formulations are extracted with acetonitrile and analyzed by reverse phase chromatography, with n-butyrophenone as an internal standard. Collaborators were furnished with samples of technical, 70% wettable powder, 1.5 emulsifiable, and 2% bait. Coefficient of variation values obtained on the 4 samples were 0.34, 0.68, 3.25, and 5.41%, respectively. The method has been adopted official first action.


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