Liquid Chromatographic Determination of Organic Nitrogenous Bases in Dosage Forms: A Progress Report

1985 ◽  
Vol 68 (3) ◽  
pp. 539-542
Author(s):  
Samuel T Walker
Keyword(s):  
Mobile Phase ◽  
General Procedure ◽  
Chromatographic Determination ◽  
Dosage Forms ◽  
Chlorpheniramine Maleate ◽  
Photometric Detection ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Good Agreement

Abstract A liquid chromatographic (LC) method has been developed as a general procedure for the assay of the salts of organic nitrogenous bases in a variety of dosage forms. The method uses a nitrile-bonded reverse phase column, a methanol-0.003M ammonium acetate (90 + 10) mobile phase, and photometric detection at 254 nm. The sample is dissolved in the mobile phase and an aliquot is injected through a 20 μL injection loop. Average recovery values for duplicate assays were chlorpheniramine maleate injection 97.8%, chlorpheniramine maleate tablets 99.1%, cyclizine hydrochloride tablets 100.0%, doxylamine succinate tablets 103.3%, mesoridazine besylate tablets 100.4%, pentazocine hydrochloride tablets 103.0%, promethazine hydrochloride injection 98.4%, protriptyline hydrochloride tablets 101.2%, pyrilamine maleate tablets 97.8%, pyrimethamine tablets 100.0%, tripelennamine citrate elixir 100.0%, and tripelennamine hydrochloride tablets 97.2%. Results by this method were in good agreement with those obtained by the USP XX method. This study, which is being continued, will be expanded to include additional drugs.

Liquid Chromatographic Determination of Acetaminophen in Multicomponent Analgesic Tablets

1984 ◽  
Vol 67 (2) ◽  
pp. 339-341
Author(s):  
David J Krieger
Keyword(s):  
Chromatographic Determination ◽  
Ultraviolet Region ◽  
Active Components ◽  
Chlorpheniramine Maleate ◽  
Reverse Phase ◽  
Phenylephrine Hydrochloride ◽  
Photometric Detection ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple, rapid LC method is presented for the separation and determination of acetaminophen in analgesic preparations containing up to 6 additional active components. The method uses a C18 reverse phase column, methanol–0.75% acetic acid (1 + 3) mobile phase, and photometric detection in the ultraviolet region. Acetaminophen was effectively separated from chlorpheniramine maleate, phenylephrine hydrochloride, caffeine, salicylamide, aspirin, and phenacetin, as well as from salicylic acid, a degradation product of aspirin. Typical chromatograms of the separation of acetaminophen from the above compounds in synthetic mixture and in commercial multicomponent analgesic preparations are presented, along with reproducibility and recovery data.

Liquid Chromatographic Determination of Coumarin Anticoagulants in Tablets: Collaborative Study

1987 ◽  
Vol 70 (5) ◽  
pp. 834-836
Author(s):  
Ella S Moore
Keyword(s):  
Mobile Phase ◽  
Collaborative Study ◽  
Chromatographic Determination ◽  
Content Uniformity ◽  
Photometric Detection ◽  
Warfarin Sodium ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method for the determination of coumarin anticoagulants in tablets was collaboratively studied by 7 laboratories. The method uses an octadecylsilane-bonded microparticulate column, tetrahydrofuran-methanol-water-acetic acid mobile phase, and photometric detection at 311 nm. Each collaborator received samples of warfarin sodium, phenprocoumon, and dicumarol as a synthetic composite and as commercial individual and composited tablets. Pooled average assay values for synthetic and commercial tablet samples of warfarin sodium were 101.6 and 99.5%, respectively, with a combined reproducibility SD of 2.38% (CV = 2.37%) and combined repeatability SD of 1.49% (CV = 1.49%). Pooled average (SD) assay values for dicumarol and phenprocoumon commercial samples were 98.0 (2.27) and 101.3% (4.00), respectively. The content uniformity determinations of 2 mg warfarin sodium and 25 mg dicumarol tablets indicated average tablet contents (range) of 99.5% (91.0-116.0) and 98.0% (89.8-108.8), respectively. The method has been approved interim official first action

Liquid Chromatographic Determination of Six Sympathomimetic Drugs in Dosage Forms

1991 ◽  
Vol 74 (2) ◽  
pp. 289-291
Author(s):  
Michael J Smela ◽  
Rona Stromberg
Keyword(s):  
Chromatographic Determination ◽  
Dosage Forms ◽  
Photometric Detection ◽  
Coefficients Of Variation ◽  
Acid Sodium Salt ◽  
Sympathomimetic Drugs ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A simple and rapid stability-Indicating liquid chromatographic method is described for quantitative determination of 6 sympathomimetic drugs In various liquid and solid formulations. Analyses were carried out on a C18 reverse phase column using 0.01M 1-octanesulfonlc acid, sodium salt In 0.2% acetic acid-methanol (70 + 30) as the mobile phase with photometric detection at 220 nm. Coefficients of variation for 5 consecutive injections of a mixed standards solution ranged from 0.62% for metaraminol to 1.40% for epinephrine. Standard recoveries ranged from 98.8 % for metaraminol to 100.8% for epinephrine. The method was linear between 0.2 and 10 μg of drug Injected and was used successfully to analyze 17 commercial products in a variety of dosage forms.

Liquid Chromatographic Determination of Atropine in Nerve Gas Antidotes and Other Dosage Forms

1995 ◽  
Vol 78 (2) ◽  
pp. 339-342 ◽  
Author(s):  
Gary J Lehr ◽  
Stella M Yuen ◽  
Glen D Lawrence
Keyword(s):  
Benzalkonium Chloride ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Dosage Forms ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Nerve Gas ◽  
Liquid Chromatographic ◽  
Ophthalmic Solutions

Abstract A simple and specific liquid chromatographic method was developed for the determination of atropine in nerve gas antidotes and several other dosage forms. The method is also used simultaneously to quantitate phenol, an antimicrobial agent present in nerve gas antidotes, and to monitor the level of tropic acid, a principal degradation product of atropine. The system uses a Spherisorb CN column and a mobile phase of acetonitrile–0.05M sodium phosphate monobasic (10 + 90), pH 4.0. The detection wavelength is 220 nm. The method was validated by testing for accuracy, linearity, reproducibility and precision. In addition, the proposed method was applied to 8 commercial preparations of atropine, including injectables, ophthalmic solutions, and ointments, and was found to be satisfactory and free from interferences from preservatives, such as benzyl alcohol, methylparaben, benzalkonium chloride and chlorobutanol, that are present in these formulations.

Liquid Chromatographic Determination of Methyldopa and Methyldopa-Thiazide Combinations in Dosage Forms

1983 ◽  
Vol 66 (6) ◽  
pp. 1436-1442
Author(s):  
Susan Ting
Keyword(s):  
Acetic Acid ◽  
Mobile Phase ◽  
Chromatographic Determination ◽  
Dosage Forms ◽  
Reverse Phase ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Standard Deviations ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method, using a reverse phase C18 column, an acetic acid-methanol-water mobile phase, and detection at 280 nm, was developed for the determination of methyldopa in tablets and oral suspensions and combinations of methyldopa with hydrochlorothiazide or chlorothiazide in tablets. A mixture of these 3 drugs was resolved in <8 min. Detector responses were linear for the following amounts (mg/mL) of drug injected: methyldopa 0.031-0.393, chlorothiazide 0.019-0.114, and hydrochlorothiazide 0.004-0.083. Recoveries from commercial dosage forms ranged from 99.1 to 100.9% for methyldopa, 99.2-100.4% for chlorothiazide, and 100.0-101.2% for hydrochlorothiazide. Replicate injections of methyldopa, chlorothiazide, and hydrochlorothiazide standard preparations alone or in combination gave overall relative standard deviations of <1.6% (n = 10). The results for methyldopa tablets by the proposed method were in agreement with those obtained by the USP XX method. The LC method detected as little as 0.6 μg 3-O-methylmethyldopa/mL and 0.5 μg 4-amino-6- chloro-l,3-benzenedisulfonamide/mL, which are sometimes found as contaminants of methyldopa and thiazides, respectively, and resolved methyldopa from its methyldopa glucose adduct, a substance found in methyldopa oral suspensions.

Improved liquid-chromatographic determination of haloperidol in plasma.

1984 ◽  
Vol 30 (7) ◽  
pp. 1228-1230 ◽  
Author(s):  
A K Dhar ◽  
H Kutt
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
Room Temperature ◽  
Internal Standard ◽  
Isoamyl Alcohol ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

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).

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