scholarly journals A Liquid Chromatographic Method for Routine Analysis of 5-Mononucleotides in Pediatric Formulas

2010 ◽  
Vol 93 (3) ◽  
pp. 966-973 ◽  
Author(s):  
Brendon D Gill ◽  
Harvey E Indyk ◽  
Maureen C Kumar ◽  
Nathan K Sievwright ◽  
Merilyn Manley-Harris

Abstract An RP-HPLC method for the routine determination of supplemented 5-mononucleotides (uridine 5-monophosphate, inosine 5-monophosphate, adenosine 5-monophosphate, guanosine 5-monophosphate, and cytidine 5-monophosphate) in pediatric formulas and milk products is described. Following sample dissolution, potential interferences were removed by anion-exchange SPE. Chromatographic analyses were performed using a C18 stationary phase with gradient elution, UV detection, and quantitation by an internal standard technique. A single-laboratory validation was performed, with recoveries of 92101 and repeatability RSDs of 1.02.3. The method was optimized for the rapid, routine analysis of nucleotide-supplemented bovine milk-based infant and follow-on formulas.

1988 ◽  
Vol 71 (3) ◽  
pp. 523-525 ◽  
Author(s):  
Ella S Walker

Abstract A simple and rapid liquid chromatographic method is described for the qualitative and quantitative determination of carbamazepine in tablet composites and individual tablets, using the internal standard technique. Analyses were performed on a C-18 reverse-phase column with tetrahydrofuran-methanol-water (8 + 37 + 55) as the mobile phase. A linear relationship was obtained between detector responses at 254 nm and amounts of carbamazepine injected ranging from 0.2 to 1.7 ng. The coefficient of variation for 10 consecutive injections of a standard preparation was 0.4%. Recoveries of carbamazepine from 100 and 200 mg tablets averaged 101.4 and 99.7%, respectively. Assay results for commercial tablets analyzed by the proposed method agreed favorably with those obtained by the method of USP XXI. The assay results for individual tablets indicated that deviations from the average value and the range of individual values are much wider with the compendial method than with the proposed method


2010 ◽  
Vol 7 (3) ◽  
pp. 821-826 ◽  
Author(s):  
C. H. Venkata Kumar ◽  
D. Ananth Kumar ◽  
J. V. L. N. Seshagiri Rao

A rapid, selective and sensitive high performance liquid chromatographic method for the estimation of nevirapine in human plasma has been developed. Chromatography was carried out on a Hypersil BDS C18column using a mixture of ammonium acetate buffer (pH 4.0 ± 0.05) and acetonitrile (85:15 v/v) as the mobile phase. The eluents were monitored for the drug by UV detection at 254 nm. Oxcarbazepine was used as an internal standard for this study. The retention times for nevirapine and oxcarbazepine were found to be 7.2 and 14.7 min respectively. The method was found to be linear in the concentration range of 50 ng/mL to 5003.7 ng/mL. The method was validated as per FDA guidelines and was found to be suitable for bioequivalence and pharmacokinetic studies.


2020 ◽  
Vol 16 (8) ◽  
pp. 1059-1067
Author(s):  
Jéssica Maurício Batista ◽  
Christian Fernandes

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.


INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 43-49
Author(s):  
B.P. Manjula ◽  
V. G Joshi ◽  
Siddamsetty Ramachandra Setty ◽  
M Geetha ◽  

Tea tree oil, an active ingredient of skin, hair and nail care cosmeceuticals, has claims for topical antimicrobial, analgesic and anti-inflammatory activity. Its complex composition is governed by ISO 4730:2017. Terpinene-4-ol is the principal constituent of the oil (35% - 48%) followed by γ-terpinene (14% -28%), α-terpinene (6%-12%) and 1,8-cineole (≤15%). A reversed-phase, isocratic high performance liquid chromatographic method has been developed and validated for routine determination of tea tree oil based on1,8-cineole content in bulk and commercially available cosmeceuticals using C18 column, methanol-water (70:30 v/v) as mobile phase and flow rate of 1mL/min. UV detection was done at 200 nm. Linearity of the method was established for 20-100μL/mL (R2 = 0.9992) with LOD, LOQ values of 0.5594 μL/mL and 5.5941μL/mL respectively. The % RSD values for robustness and precision were <1% and recovery ranged between 99.09-102.96%. The method was successfully applied for determination of 1,8-cineole content in cosmeceuticals.


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 &lt; 1.5%. The method has been adopted official first action.


1973 ◽  
Vol 56 (5) ◽  
pp. 1277-1280
Author(s):  
Victor W Winkler

Abstract A GLC method for the determination of menadione bisulfite addition products in feed premixes was tested by 8 laboratories. Menadione sodium bisulfite complex (trihydrate) is extracted with methanol containing 1 mg diethyl phthalate/ml as internal standard and injected directly onto a 2% OV-17 (silylated) GLC column. The principle of the method is on-column pyrolysis of menadione bisulfite and subsequent GLC analysis of the pyrolytic product, menadione. The method is simple, rapid, and free from interference. The average recovery values for 4 samples at 16.0, 14.4, 4.0, and 3.6 g/lb ranged from 95.8 to 100.4% with coefficients of variations between 5.5 and 6.5%. The method has been adopted as interim official first action.


1988 ◽  
Vol 34 (8) ◽  
pp. 1565-1568 ◽  
Author(s):  
M A Hedaya ◽  
R J Sawchuk

Abstract We describe a liquid-chromatographic assay for AZT in human plasma and urine. This assay involves the use of two internal standards, allowing reference of AZT peaks to the appropriate internal standard, the choice depending on the range of concentrations encountered. This method is isocratic, specific, sensitive enough to allow quantification of AZT in concentrations observed clinically, and requires only 13 min of chromatographic time. We saw no interference from various over-the-counter and prescription drugs often used in treating the infectious complications of AIDS.


1983 ◽  
Vol 66 (4) ◽  
pp. 909-912 ◽  
Author(s):  
Steven P Swanson ◽  
Venkatachalam Ramaswamy ◽  
Val R Beasley ◽  
William B Buck ◽  
Harold H Burmeister

Abstract The gas-liquid chromatographic method for the determination of T-2 toxin in plasma is described. The toxin is extracted with benzene, washed with aqueous sodium hydroxide, and chromatographed on a small Florisil column; the heptafluorobutyryl derivative is prepared by reaction with heptafluorobutyrylimidazole. The T-2 HFB derivative is chromatographed onOV-1 at 230°C and measured with an electron capture detector. Iso-T-2, an isomer of T-2 toxin, is added to samples as an internal standard before extraction. Recoveries averaged 98.0 ± 5.5% at levels ranging from 50 to 1000 ng/m L. The limit of detection is 25 ng/mL.


1985 ◽  
Vol 68 (3) ◽  
pp. 586-589
Author(s):  
Stephen C Slahck

Abstract A liquid chromatographic method for the determination of triadimefon (Bayleton™) in triadimefon technical and formulated products has been developed and subjected to a collaborative study with 7 participating collaborators. Formulations were extracted with mobile solvent and analyzed by normal phase chromatography, with 4-chlorophenyl sulfoxide as an internal standard. Collaborators were furnished with standards and samples of technical products, 50% wettable powders, and 25% wettable powders for analysis. Coefficients of variation of the values obtained on these samples were 1.42, 0.82, and 1.05%, respectively. The method has been adopted official first action.


1978 ◽  
Vol 61 (1) ◽  
pp. 161-163
Author(s):  
Giuseppe Cellerino ◽  
Mariarosa Re

Abstract Simultaneous determination of the active ingredient and of by-products in technical and formulated pyridazinones was rapidly performed by gas-liquid chromatography with complete resolution of all compounds. Quantitative determination by the internal standard technique is accurate and precise. The lower limit of detectability is 8 × 10–12 g/sec with a flame ionization detector and 1 × 10–12 g/sec with a nitrogen-phosphorus selective detector operating in the nitrogen mode.


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