Liquid Chromatographic Determination of Identity, Content, and Content Uniformity of Desipramine, Fluphenazine, and Promazine

1986 ◽  
Vol 69 (1) ◽  
pp. 178-179 ◽  
Author(s):  
Normand Beaulieu ◽  
Charles Gagné ◽  
Edward G Lovering

Abstract A liquid chromatographic procedure has been developed for the assay, content uniformity, and identification of single active ingredient formulations of desipramine, fluphenazine, and promazine. The drugs are extracted from formulations with methanol or dilute hydrochloric acid and quantitated against an internal standard (norephedrine). The drugs are identified by comparison of retention times with those of the reference standards.

1985 ◽  
Vol 68 (2) ◽  
pp. 168-171
Author(s):  
Edward G Lovering ◽  
Normand Beaulieu ◽  
Robert C Lawrence ◽  
Roger W Sears

Abstract A liquid chromatographic (LC) procedure has been developed for the assay, content uniformity, and identification of single active ingredient solid and liquid formulations of amitriptyline, chlorpromazine, imipramine, thioridazine, and trifluoperazine. The drugs are extracted from their formulations with methanol or dilute hydrochloric acid, and identified by comparison of retention times with those of known standards; drugs are quantitated against these standards with rf/-norephedrine hydrochloride as the internal standard. The precision of replicate injections is better than 2.5% for peak area and better than 1% for peak height. The precision of triplicate determinations of tablet composites is better than 2.2%.


1982 ◽  
Vol 65 (3) ◽  
pp. 753-756
Author(s):  
Walter F Schmidt

Abstract A high performance liquid chromatographic procedure has been developed for the assay of phenprocoumon in tablets. In comparison to the present official USP assay procedure, it is equivalent in precision and accuracy and is faster and more specific. A mobile phase consisting of a 1% solution of acetic acid in acetonitrile-water (4 + 3) separates phenprocoumon from warfarin internal standard on a 6 μm octadecylsilane (ODS) column with UV detection at 311 nm. The method enables the concurrent determination of phenprocoumon and possible contaminants such as salicylic acid.


1982 ◽  
Vol 28 (10) ◽  
pp. 2154-2157 ◽  
Author(s):  
J J Tasset ◽  
F M Hassan

Abstract We describe a liquid-chromatographic procedure for amoxapine and 8-hydroxyamoxapine, its active metabolite, in serum. We used a mu-Bondapak C18 reversed-phase column and a mobile phase of acetonitrile/water (74/26 by vol) plus 26 microL of n-butylamine per liter. The compounds were measured at 254 nm, with 8-methoxyloxapine as internal standard. Necessary pre-analysis purification consisted of adsorbing the drug from serum onto extraction columns, eluting with 1-butanol/hexane (1/5 by vol), re-extracting into aqueous acid, and from that re-extracting again into the elution-solvent mixture. We prefer this procedure for monitoring both therapeutic and toxic concentrations of amoxapine, because parent drug and metabolite are measured separately.


1983 ◽  
Vol 29 (6) ◽  
pp. 1085-1087 ◽  
Author(s):  
R N Gupta ◽  
R B Haynes ◽  
A G Logan ◽  
L A Macdonald ◽  
R Pickersgill ◽  
...  

Abstract We describe a liquid-chromatographic procedure for determining nadolol in plasma. After an analog of nadolol is added as internal standard, the plasma sample is passed through a disposable BondElut C18 column. After several column washes, nadolol and the internal standard are eluted with methanol, and the eluate is evaporated and reconstituted with the mobile phase (acetonitrile/water, perchloric acid, and tetramethylammonium hydroxide). An aliquot of the extract is chromatographed on a non-silica resin-base reversed-phase column. The peaks are detected by fluorescence (lambda ex = 265 nm and lambda em = 305). Drug and internal standard are well resolved, and only a few extraneous peaks appear. The standard curve ranges from 10 to 400 micrograms/L. We are using this procedure to determine steady-state concentrations of nadolol in patients receiving various dosages of nadolol along with other types of antihypertensive drugs.


1997 ◽  
Vol 80 (4) ◽  
pp. 767-774 ◽  
Author(s):  
John C Reepmeyer ◽  
Don C Cox

Abstract A simple, isocratic liquid chromatographic method for assay of thalidomide in tablets, capsules, and raw materials was developed. The method uses a Nova-Pak octadecylsilane bonded-phase column (150 × 3.9 mm, 4 μm particle size), a mobile phase of acetonitrile-water (15 + 85), a flow rate of 1 mL/min, detection at 237 nm, and phenacetin as internal standard. Phosphoric acid was used in preparation of sample solutions to inhibit thalidomide hydrolysis. Assays ranged from 99.3 to 100.4% in raw materials from 4 manufacturers, from 79.7 to 104.8% in tablets from 7 manufacturers, and from 75.3 to 102.6% in capsules from 4 manufacturers. Assay method precisions for triplicate analyses on 5 days were 0.30% for tablets, 0.22% for capsules, and 0.22% for raw materials. Recovery from simulated tablet formulations was 100%. The method has been used to analyze individual tablets and capsules for determination of content uniformity.


1975 ◽  
Vol 58 (5) ◽  
pp. 961-964 ◽  
Author(s):  
Alan R Hanks ◽  
Barbara S Engdahl ◽  
Billy M Colvin

Abstract A simple and rapid gas-liquid chromatographic procedure, using a 6’ × ¼“ glass column packed with 5% SE-30 on Chromosorb W (DMCS) and a flame ionization detector, is described. Grain baits containing strychnine alkaloid are ground, mixed, and extracted by shaking with chloroform containing an internal standard, 1,3,5-triphenylbenzene. Without further cleanup, extract nitrates are injected directly into a gas chromatograph. Peak height ratios are used for quantitation of strychnine. The analysis of commercial samples shows that the method compares well with a commonly employed ultraviolet spectrophotometric method; good precision, with recoveries ranging from 89.9 to 91.7%, is obtained in the analysis of prepared samples. The method is sensitive to 2 μg strychnine.


2003 ◽  
Vol 68 (11) ◽  
pp. 883-892 ◽  
Author(s):  
Dragica Zendelovska ◽  
Trajce Stafilov

A rapid, specific and sensitive high-performance liquid chromatographic method for the determination of famotidine in human plasma has been developed. Famotidine and the internal standard were chromatographically separated from plasma components using a Lichrocart Lichrospher 60 RP select B cartridge for solid-phase separation with a mobile phase composed of 0.1 % (v/v) triethylamine in water (pH 3) and acetonitrile (92:8, v/v). UV detection was set at 270 nm. The calibration curve was linear in the concentration range of 10.0 ? 350.0 ng mL-1. The method was implemented to monitor the famotidine levels in patient samples.


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).


1974 ◽  
Vol 57 (5) ◽  
pp. 1089-1091
Author(s):  
David O Edlund ◽  
Florido A Filippini ◽  
James K Datson

Abstract A gas-liquid chromatographic procedure used to determine vitamin D2 in multiple vitamin tablets has been modified to make it applicable for analysis of multiple vitamin tablets containing minerals and vitamin E acetate. The procedure modifications involve pre-extraction with ether, solution in an alcoholic sulfuric acid-pyridine mixture, and column chromatographic separation on phosphate-treated alumina. The modified procedure has been statistically evaluated. A 2.2% coefficient of variation and 100.3% average recovery were obtained for the samples evaluated.


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