Automated High-Pressure Liquid Chromatographic Assay for Antiepileptic Drugs and Their Major Metabolites by Direct Injection of Serum Samples

1984 ◽  
Vol 6 (4) ◽  
pp. 478-483 ◽  
Author(s):  
Wilhelm Kuhnz ◽  
Heinz Nau
1979 ◽  
Vol 62 (3) ◽  
pp. 637-641
Author(s):  
Warren A Widicus ◽  
James R Kirk

Abstract A rapid method for the simultaneous determination of vitamins A and E in fortified cereal products has been developed. Saponification of retinyl or tocopheryl esters is not required, permitting direct injection of the extracted lipids onto the high pressure liquid chromatographic column without sample cleanup. Elution times of 2.46 and 3.40 min were determined for retinyl palmitate and tocopheryl acetate, respectively, using a μPorasil column and an isocratic mobile phase of hexane-chloroform (85+15) with a flow rate of 1.5 mL/min. The average recovery of retinyl palmitate was 99.2% (std dev. 4.28), and the average recovery of tocopheryl acetate was 94.9% (std dev. 4.10) in 2 cereals containing corn, oat, rice, and wheat. No significant amounts of naturally occurring tocopherols were found in the cereals.


1979 ◽  
Vol 62 (2) ◽  
pp. 297-303
Author(s):  
Timothy S Stevens

Abstract A rapid and precise fully automated, direct injection high pressure liquid chromatographic method is described for assaying liquid formulations of 2,4-dichlorophenoxyacetic acid (2,4-D) and/or picloram (4-amino-3,5,6-trichloropicolinic acid). The method is specific for the 2,4-D and picloram isomers. No sample preparation is needed, triplicate assays can be performed in 1 hr, and precision is about 1% relative at the 95% confidence level. Compounds are separated on a 9 mm id reverse phase microparticulate column with an eluant of ace* tonitrile-water (1+4) , buffered at pH 2.95. No bias was observed between this method and the official final action HPLC method for picloram and 2,4-D in picloram-2,4-D mixtures, 6.B09-6.B12.


1976 ◽  
Vol 22 (1) ◽  
pp. 25-31 ◽  
Author(s):  
R F Adams ◽  
F L Vandemark

Abstract We describe procedures for simultaneously determining some anticonvulsants (phenobarbital, diphenylhydantoin, primidone, ethosuximide, methsuximide, carbamazepine) in serum by high-pressure liquid chromatography. The drugs, together with an internal standard, phenacetin, are adsorbed from serum onto charcoal and eluted from it with organic solvent. The eluate is analyzed isocratically on a reverse-phase column with a mobile phase consisting of acetonitrile/water (17/83 by volume). The eluted drugs are detected by their absorption at 195 nm, and quantities estimated from their peak areas as compared with those of extracted standards. Results are reproducible to about 6%. Sensitivities, for 0.5-ml serum samples, of 0.1 mg/liter for all the drugs analyzed except ethosuximide (0.5 mg/liter) are attained routinely. Correlation of results with gas chromatography was 0.912 for phenobarbital, 0.982 for diphenylhydantoin, 0.886 for primidone, and 0.966 for ethosuximide. Amobarbital and secobarbital interfere with the analysis; chlordiazepoxide, methaqualone, salicylate, diazepam, and oxazepam do not. Including extraction, analysis time for a single sample is 20 min.


1976 ◽  
Vol 22 (4) ◽  
pp. 471-474 ◽  
Author(s):  
P J Kudirka ◽  
R R Schroeder ◽  
T E Hewitt ◽  
E C Toren

Abstract The isoenzymes of lactate dehydrogenase (EC 1.1.1.27) were separated with excellent resolution in less than 1 h by high-pressure anion-exchange chromatography. These isoenzymes were determined in some tissue extracts and high-activity serum samples by this technique.


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