Determination of carbamazepine in blood or plasma by high-pressure liquid chromatography.

1976 ◽  
Vol 22 (7) ◽  
pp. 1070-1072 ◽  
Author(s):  
P M Kabra ◽  
L J Marton

Abstract We described a sensitive and precise high-pressure liquid-chromatographic method in which 5-(p-methylphenyl)-5-phenylhydantoin is used as the internal standard in determining carbamazepine in whole blood or plasma. Carbamazepine is well separated from normal blood constituents in less than 8 min, and other commonly used anticonvulsants do not interfere with the analysis. The sensitivity of this method is adequate to quantitate 0.25 mg of carbamazepine per liter in 2 ml of sample, and the lower limit of detection is 100 ng. Twenty specimens were analyzed by a gas-chromatographic method and by the present method; the resulting correlation coefficient was greater than .980.

1976 ◽  
Vol 22 (6) ◽  
pp. 824-827 ◽  
Author(s):  
P M Kabra ◽  
G Gotelli ◽  
R Stanfill ◽  
L J Marton

Abstract We describe a sensitive, precise high-pressure liquid chromatographic method in which 5-(p-methylphenyl)-5-phenylhydantoin is used as the internal standard for simultaneous determination of diphenylhydantoin, phenobarbital, and primidone in whole blood and plasma. These anticonvulsant drugs are well separated from each other and from normal blood constituents in less than 10 min. The lower limit of detection for each drug is 100 ng for primidone, 200 ng for dilantin, and 300 ng for phenobarbital. The eluted drugs were detected by their absorption at 254 nm, and evaluated from their peak heights as compared to internal standard. The method was successfully adapted for pediatric samples (100 to 500 mul of whole blood or plasma). Fifty specimens were analyzed for phenobarbital and diphenylhydantoin and 25 specimens for primidone by a standard gas-chromatographic method and by our liquid-chromatographic method; the resulting correlation coefficient was greater than 0.98.


1977 ◽  
Vol 23 (6) ◽  
pp. 957-959 ◽  
Author(s):  
G R Gotelli ◽  
P M Kabra ◽  
L J Marton

Abstract We describe a sensitive and precise high-pressure liquid chromatographic method in which acetoacetanilide is used as the internal standard to simultaneously determine acetaminophen and phenacetin in plasma. Therapeutic as well as toxic concentrations can be determined on as little as 0.1 ml of plasma. Sample preparation is rapid and chromatography is complete in 5 min. Quantitation is accurate at 0.5 mg/liter concentration for both drugs. Day-to-day precision within 5% is attainable. Of 36 other drugs tested, only theophylline interfered, with the determination of acetaminophen.


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.


1974 ◽  
Vol 57 (2) ◽  
pp. 358-359
Author(s):  
Manjeet Singh

Abstract A high-pressure liquid chromatographic method is presented for the isolation and determination of uncombined intermediates in FD&C Yellow No. 6 (sunset yellow FCF, CI. No. 15895). Samples of FD&C Yellow No. 6 containing 0.1-0.4% sulfanilic acid, 0.1-0.4% 6-hydroxy-2-naphthalenesulfonic acid, and 0.3— 1.0% 6,6'-oxybis(2-naphthalenesulfonic acid) were prepared and analyzed using this method. Recoveries ranged between 94 and 101%. Twenty-two samples of FD&C Yellow No. 6 were analyzed by the conventional column elution chromatographic method as well as by the high-pressure liquid chromatographic method. Good agreement was obtained between the 2 methods.


1975 ◽  
Vol 58 (4) ◽  
pp. 754-756 ◽  
Author(s):  
George M Ware

Abstract Patulin is extracted from apple butter samples with ethyl acetate and the extract is cleaned up on a silica gel column, using benzene-ethyl acetate (75+25) as the eluant. High-pressure liquid chromatography, using a 25 cm Zorbax-Sil column, isooctane-ethyl ether-acetic acid (750+250+0.5) as the mobile solvent, and a 254 nm ultraviolet detector, is used for the determinative step. Under these conditions, patulin is eluted before 5-hydroxymethylfurfural, a component of apple butter which interferes with other liquid chromatographic and thin layer chromatographic methods. Recoveries of patulin added at levels of 34.6, 138.4, and 276.8 μg/kg ranged from 89.0 to 112.1%.


1978 ◽  
Vol 61 (3) ◽  
pp. 687-694
Author(s):  
Paul J Vollmer ◽  
Thomas G Alexander ◽  
Carol Haneke

Abstract A high pressure liquid chromatographic method for determining probenecid in oral suspensions of amoxicillin was applied to the determination of probenecid in oral suspensions of ampicillin. Three preparations containing various known amounts of probenecid in synthetic mixtures of ampicillin oral suspensions were analyzed by 5 chemists in an intralaborastory study, with satisfactory results. Blind duplicates of 3 prepared oral suspensions were sent to 12 collaborators, who were instructed to analyze the samples in a fixed random order. The standards showed a satisfactory linear response. Average recoveries of probenecid in the interlaboratory study for the 6 mixtures ranged from 95.2 to 99.1%, and the coefficients of variation ranged from 1.63 to 4.9%.


1978 ◽  
Vol 39 (02) ◽  
pp. 466-473 ◽  
Author(s):  
Thorir D Bjornsson ◽  
Sarah E Swezey ◽  
Peter J Meffin ◽  
Terrence F Blaschke

SummaryA convenient, accurate and reproducible high pressure liquid chromatographic method for the quantitation of radio-labelled vitamin K1 and vitamin K1 epoxide in plasma is described. The method involves the determination of total ether extractable radioactivity, and a chromatographic separation to determine the relative quantities of radio-labelled vitamin K1 and vitamin K1 epoxide. The method is useful over a wide range of ratios of the two compounds, and has a coefficient of variation of approximately 5%.


1987 ◽  
Vol 70 (5) ◽  
pp. 825-828
Author(s):  
Alfred V Del Grosso ◽  
Joan C May

Abstract Three methods for the determination of glycerin are examined as applied to several allergenic extracts and diagnostic antigens. The liquid chromatographic procedure uses a sulfonic acid functional PSDVB resin (Aminex HPX-87H), a mobile phase of 0.013N H2S04; and refractive index detection. The titrimetric procedure involves oxidation of glycerin with sodium metaperiodate followed by potentiometric titration of the resulting formic acid with sodium hydroxide. Samples are quantitated by comparing the equivalence point obtained from the sample to those obtained from a series of standards. The gas chromatographic procedure includes a column of 5% Carbowax 20 M on 80-100 mesh Chromosorb WHP; p-cresol was used as an internal standard. The 3 procedures are shown to be valid for the majority of product types examined. A positive interference was encountered in the titrimetric analysis of a tuberculin purified protein derivative that contained simple sugars. Recoveries of added glycerin ranged from 95.0 to 100.2% by the liquid chromatographic method, from 98.7 to 101.4% by the gas chromatographic method, and from 99.8 to 101.6% by the metaperiodate oxidation method when interference from simple sugars was not present. Coefficients of variation determined from 8 replicates of samples that contained glycerin were 2.2% or less for the liquid chromatographic method, 2.3% or less for the GC method, and 3.6% or less for the metaperiodate oxidation method.


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