Liquid-chromatographic determination of alpha- and gamma-tocopherols in erythrocytes, with fluorescence detection.

1983 ◽  
Vol 29 (10) ◽  
pp. 1840-1842 ◽  
Author(s):  
J Lehmann ◽  
H L Martin

Abstract We have adapted to erythrocytes a method for the determination of alpha- and gamma-tocopherols in plasma and platelets. Erythrocytes (50 microL) were extracted with methanol containing tocol (internal standard) and pyrogallol. Tocopherols were partitioned into chloroform, washed, and injected in methanol onto a reversed-phase (C18) "high-performance" liquid-chromatographic column. The mobile phase was methanol/water (99/1 by vol) at a flow rate of 2 mL/min and detection was with a "high-performance" spectrophotofluorometer. The limit of detection for either tocopherol is 0.10 microgram/mL of packed cells. Analytical recoveries ranged from 93 to 104%. Some values for tocopherols in human erythrocytes are presented.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt

Abstract This method for determination of haloperidol in plasma is based on "high-performance" isocratic liquid chromatography with the use of a C8 bonded reversed-phase column at room temperature. Haloperidol and the internal standard (chloro-substituted analog) are extracted from alkalinized plasma into isoamyl alcohol/heptane (1.5/98.5 by vol) and back-extracted into dilute H2SO4. The aqueous phase is directly injected onto the column. The mobile phase is a 30/45/25 (by vol) mixture of phosphate buffer (16.5 mmol/L, pH 7.0), acetonitrile, and methanol. Unlike other liquid-chromatographic procedures for haloperidol, commonly used psychotropic drugs do not interfere. Analysis can be completed within an hour. The procedure is extremely sensitive (1.0 microgram/L) and is well reproducible (CV 5.6% for a 2.5 micrograms/L concentration in plasma).


1981 ◽  
Vol 27 (3) ◽  
pp. 437-440 ◽  
Author(s):  
D R Uges ◽  
P Bouma

Abstract We have developed "high-performance" liquid-chromatographic methods for determining 4-aminopyridine, an acetylcholine-releasing drug, in serum, saliva, and urine. As little as 1 microgram/L can be detected by extracting the alkalinized sample plus the internal standard (3,4-diaminopyridine) into dichloromethane, mixing the organic phase with 1-pentanol, evaporating the dichloromethane, and injecting the residue onto a reversed-phase column, where it is eluted with acetonitrile/methanol/aqueous ammonium carbonate, with detection at 245 nm. Analytical recoveries from serum averaged 86.7%. The CV at 50 micrograms/L was 2.9% (n = 8). For urine samples containing very high concentrations of 4-aminopyridine, we mixed urine and potassium carbonate in an automatic injector vial, extracted the drug into dichloromethane, centrifuged, and injected an aliquot of the extract into the chromatograph. Analytical recoveries averaged 92%, and the CV was about 2% for drug concentrations of 0.1-8 mg/L of urine.


1988 ◽  
Vol 34 (9) ◽  
pp. 1897-1899 ◽  
Author(s):  
M H Cheng ◽  
W Y Huang ◽  
A I Lipsey

Abstract This high-performance liquid-chromatographic (HPLC) method for simultaneous determination of prednisone and its metabolite, prednisolone, in plasma is a modification of the method of Frey et al. (Clin Chem 1979;25:1944-7). Heparinized plasma (1.0 mL) with 0.1 mL of internal standard solution (11-deoxy-17-hydroxycorticosterone, 2 mg/L) is extracted with 7.0 mL of dichloromethane, then washed sequentially with 0.1 mol/L HCl, 0.1 mol/L NaOH, and deionized water, 2.0 mL each. The extract is evaporated and the residue reconstituted with 75 microL of mobile phase, methanol/H2O (40/60 by vol). Thirty microliters of this is injected onto a reversed-phase C6 column, which is eluted at 1.4 mL/min. Analytical recoveries of prednisone and prednisolone were 94-98% and 102-106%, respectively. Day-to-day precision (CV) was 3.8% for prednisone, 6.1% for prednisolone. We encountered no interference from the 21 other steroids and 25 drugs tested. This method is simple, accurate, and precise.


1985 ◽  
Vol 31 (7) ◽  
pp. 1222-1224 ◽  
Author(s):  
G Houin ◽  
J P Jeanniot ◽  
P Ledudal ◽  
J Barré ◽  
J P Tillement

Abstract We describe a "high-performance" liquid-chromatographic assay for simultaneously determining propisomide and its mono-N-dealkylated metabolite in plasma and urine. After extraction with dichloromethane at alkaline pH, the unchanged drug, its metabolite, and the internal standard are separated by liquid chromatography on a reversed-phase column and the absorbance of the eluate is measured at 254 nm. Selectivity, sensitivity, and reproducibility are excellent. Results are similar to those by gas chromatography for propisomide but, in addition, the metabolite can be simultaneously measured in the same clinical sample. We also report results by this method for blood and plasma samples from a volunteer receiving a single 200-mg dose of propisomide.


1983 ◽  
Vol 29 (6) ◽  
pp. 1104-1105 ◽  
Author(s):  
B A Robinson ◽  
F N Cornell

Abstract A simple, rapid "high-performance" liquid-chromatographic procedure is presented for the determination of aminoglutethimide in plasma. After precipitation of the protein with acetonitrile, an aliquot of the supernate is injected directly onto a radially compressed, reversed-phase column. The aminoglutethimide is isocratically eluted with a mobile phase of acetonitrile/water/tert-butyl ammonium phosphate. The method is both accurate and precise and has been in routine use in our laboratory for more than 12 months.


1980 ◽  
Vol 63 (1) ◽  
pp. 47-48
Author(s):  
James M Zehner ◽  
Richard A Simonaitis ◽  
Roy E Bry

Abstract A high performance liquid chromotographic method is presented for determining bendiocarb (2,2-dimethyl-1,3-benzodioxol-4-yl methylcarbamate) on wool. Bendiocarb is extracted from wool with methanol containing methyl benzoate as internal standard, eluted through a Zorbax ODS column with methanol-water (55 + 45), and detected with a UV detector at 280 nm. The method can be used to determine bendiocarb at 0.001–0.02% by weight. The limit of detection is 0.0004%, or 4 ppm. At 4 analyses each, recovery at 0.013% was 101%, standard deviation 2.8%; at 0.003%, recovery was 96%, standard deviation 5.6%; at 0.001%, recovery was 103%, standard deviation 2.9%.


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