Quantitative liquid-chromatographic technique for the simultaneous assay of tricyclic antidepressant drugs in plasma or serum.

1982 ◽  
Vol 28 (3) ◽  
pp. 457-461 ◽  
Author(s):  
P K Sonsalla ◽  
T A Jennison ◽  
B S Finkle

Abstract A quantitative "high-pressure" liquid-chromatographic assay for tricyclic antidepressant drugs in plasma or serum is described in which amitriptyline, nortriptyline, imipramine, desipramine, doxepin, and desmethyldoxepin are separated with a 10-micrometer particle size silica column and a methanol/NH4OH/NH4NO3 solvent system. The drugs and two internal standards are extracted with hexane/isoamyl alcohol, the solvent layer is evaporated at 40 degrees C, and the drugs are detected at 254 nm. Drug concentrations are linear with absorbance from 25 to 1000 micrograms/L; within-assay and between-assay CVs are less than or equal to 10%.

1978 ◽  
Vol 24 (11) ◽  
pp. 1948-1953 ◽  
Author(s):  
H F Proelss ◽  
H J Lohmann ◽  
D G Miles

Abstract We report a method for simultaneous measurement of five commonly used tricyclic antidepressant drugs (doxepin, desipramine, nortriptyline, imipramine, and amitriptyline) in serum by paired-ion high-performance liquid chromatography, with use of a reversed-phase column and ultraviolet detection at 254 nm. The drugs are extracted from 2 ml of serum at pH 14 into hexane/isoamyl alcohol (99/1 by vol) and re-extracted into 200 microliter of 0.1 mol/liter HCI. An aliquot of the aqueous acid phase is chromatographed with use of a methanol/acetonitrile/water (41/15/44) solvent system, containing 5 mmol of pentanesulfonic acid per liter of phosphate buffer (0.1 mol/liter, pH 6.5), at a flow rate of 1,5 ml/min. Analytical recoveries of the drugs from serum increase with increasing concentration, from 62% at 25 microgram/liter to 93% at 300 microgram/liter. Linear response is observed for drug concentrations up to 1500 microgram/liter and the detection limit is 2-3 microgram/liter. Within-run precision ranges from 1.4 to 2.9% and day-to-day precision from 1.7 to 7%, depending on the specific drug. The entire procedure can be completed within 45 min and is well adapted to the routine clinical laboratory. Of 48 common basic and several neutral drugs tested for possible interferences, only three benzodiazepines, three phenothiazines, and three antihistamines interfere with the assay of doxepin, desipramine, and nortriptyline, respectively.


1981 ◽  
Vol 27 (6) ◽  
pp. 849-855 ◽  
Author(s):  
S J Bannister ◽  
S van der Wal ◽  
J W Dolan ◽  
L R Snyder

Abstract We describe a single procedure for assay of seven tricyclic antidepressant drugs and metabolites in serum or plasma: protriptyline, nortriptyline, amitriptyline, desmethyldoxepin, doxepin, desipramine, and imipramine. With the Technicon "FAST-LC" system, samples are aspirated directly into the unit and pretreated via double extraction; the concentration of each drug is then determined by "high-performance" liquid chromatography. Final chromatograms are monitored at 205 nm, at analysis rates of 7.5 samples/h. Concentration and absorbance are linearly related for each drug from 0 to 1400 micrograms/L. Day-to-day CVs averaged 5 to 6% for each drug, and there is good correlation of FAST-LC values with those obtained by gas-chromatographic methods. Total sample volume is 750 microliters.


1983 ◽  
Vol 66 (5) ◽  
pp. 1220-1225 ◽  
Author(s):  
Robert B Grorud ◽  
John E Forrette

Abstract A high pressure liquid chromatographic method has been developed for liquid herbicide combinations that contain different combinations of 3 active ingredients including 2,4-dichlorophenoxyacetic acid (2,4-D), 2-(2-methyl-4-chlorophenoxy)propionic acid (MCPP), and dicamba. A reverse phase column in the ion suppression mode and a binary solvent system separate all 3 herbicides quantitatively on a single chromatogram. The internal standard solution may contain 2 internal standards, salicylic acid and butyrophenone, for use with certain combinations of the herbicides. The solvent system resolves the compounds of interest from all significant impurities.


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