Liquid Chromatographic Determination of Carbamazepine in Tablets

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

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.


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.


1982 ◽  
Vol 28 (10) ◽  
pp. 2143-2148 ◽  
Author(s):  
P M Edelbroek ◽  
E J de Haas ◽  
F A de Wolff

Abstract To study correlations between the concentrations, in serum, of amitriptyline and its most important metabolites with clinical response in patients, we developed a "high-performance" liquid-chromatographic method for routine determination of amitriptyline, nortriptyline, total 10-hydroxy-amitriptyline, desmethylnortriptyline, and E(trans)- and Z(cis)-10-hydroxynortriptyline. These compounds are extracted from 1 mL of alkalinized serum into hexane/isoamyl alcohol (99/1 by vol). Perazine is the internal standard. To minimize irreversible adsorption of the drugs onto the glassware, 5 micrograms of maprotiline is added to the organic phase just before evaporation. After a 10-min resolution on a silica column eluted with acetonitrile/methanol/NH4OH (1 mol/L), absorbance is measured at 240 nm. Only chlorimipramine, doxepin, procainamide, and N-acetylprocainamide may interfere with assay of the compounds that probably are therapeutically relevant: amitriptyline, nortriptyline, and E-10-hydroxynortriptyline. Uremia, lipemia, and icterus also do not affect the analysis.


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.


1986 ◽  
Vol 69 (5) ◽  
pp. 908-911
Author(s):  
Peter L Carter ◽  
Keith C Overton ◽  
◽  
P G Baker ◽  
O O Bennett ◽  
...  

Abstract A liquid chromatographic method for determination of bendiocarb in technical materials and wettable powders was tested by 12 collaborators. Bendiocarb is dissolved in acetonitrile containing 0.1% propiophenone as internal standard. This solution is analyzed on a liquid chromatograph utilizing a reverse phase (C18) column. The compound is detected at 254 nm and peak area is used for quantitation. The 3 different materials studied contained 20, 80, and nominally 100% bendiocarb. Each was examined in duplicate to provide the necessary matched pairs. Collaborators approved of the ease and simplicity of the method and, in particular, the way the method can be applied to automatic injection assemblies. The statistical data show acceptable precision of the method: Reproducibility coefficients of variation were 20% material, 2.04%; 80% material, 1.02%; and nominal 100% material (technical product), 0.64%. The method has been adopted official first action.


1982 ◽  
Vol 28 (8) ◽  
pp. 1772-1774 ◽  
Author(s):  
R N Gupta ◽  
P T Smith ◽  
F Eng

Abstract We describe a liquid-chromatographic method involving a new, nonsilica column (XAD-2, Hamilton Co.) for pentobarbital in plasma. Plasma is extracted with chloroform after addition of the internal standard, 5-ethyl-5-p-tolyl-barbituric acid. Acidic drugs are back-extracted into alkali, then chromatographed on the resin-base reversed-phase column. The use of alkaline mobile phase allows enhanced sensitivity and detection of barbiturates at 240 nm. The within-run CV for 10 samples was 1.9%, the between-run CV 1.8%. Ten commonly used barbiturates are separated isocratically in less than 15 min. Other commonly prescribed acidic drugs do not interfere with determination of pentobarbital.


1976 ◽  
Vol 59 (3) ◽  
pp. 708-710
Author(s):  
Alan R Hanks ◽  
Christine W Cramer

Abstract A gas-liquid chromatographic method has been developed to determine pentachloronitrobenzene (PCNB) in pesticide formulations including dusts, powders, granules, liquids, and fertilizers. Captan, disulfoton, and Terrazole do not interfere. Samples are extracted with chloroform, and an aliquot is mixed with an equal volume of internal standard solution containing o-terphenyl. PCNB is chromatographed on a 5% SE-30 column and quantitated by peak height ratios. The method has been subjected to a ruggedness test which indicates little sensitivity to changes in extraction and chromatographic conditions.


1978 ◽  
Vol 61 (1) ◽  
pp. 136-138
Author(s):  
Walter F Staruszkiewicz ◽  
John F Bond

Abstract A multiple internal standard technique has been developed for the official first action gas-liquid chromatographic (GLC) method for determining indole in shrimp. The modification was developed because interfering GLC peaks are occasionally observed when 2-methylindole is used as the internal standard. An internal standard solution containing 1-methylindole, 2- methylindole, and diphenylamine was added to extracts of shrimp before silica gel cleanup and separation by GLC. All of the compounds were quantitatively recovered and were separated on the GLC column under identical experimental conditions. Extracts of acceptable shrimp to which indole was added at levels of 3–10 μg/ 100 g and extracts of decomposed shrimp were stored at room temperature for 2 weeks. Average and maximum changes (μg indole/100 g) during storage were, respectively, for each internal standard: average 0.6, 0.4, and 1.1; maximum 1.7, 0.9, and 2.9.


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