Liquid Chromatographic Determination of Clidinium Bromide and Clidinium Bromide-Chlordiazepoxide Hydrochloride Combinations in Capsules

1991 ◽  
Vol 74 (3) ◽  
pp. 461-464 ◽  
Author(s):  
Stella M Yuen ◽  
Gary Lehr
Keyword(s):  
Mobile Phase ◽  
Ammonium Phosphate ◽  
Chromatographic Determination ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds ◽  
Chlordiazepoxide Hydrochloride ◽  
Clidinium Bromide

Abstract A specific liquid chromatographic method was developed for determination of clidinium bromide and clidinium bromidechlordiazepoxide hydrochloride combinations in capsules. The procedure uses a Partisil 10 ODS-3 column and a mobile phase consisting of acetonitrile-0.3M ammonium phosphate (32 + 68) (pH = 4.3). The detection wavelength is 235 nm. Accuracy, reproducibility, and linearity were within accepted criteria. Four commercial samples of the single ingredient were tested; results compared favorably with the compendial method. Two commercial samples of the combination product were tested by the proposed method and results reported. The system was found to be free from any interferences from the 4 known related compounds of the 2 major components and Is useful as a screening procedure for 7- chloro-1,3-dihydro-5-phenyl-2H-1,4-benzodiazepin-2-one- 4-oxide, the principal degradation product of chlordiazepoxide hydrochloride.

Liquid Chromatographic Determination of Alprazolam and Related Impurities in the Drug Substance

1992 ◽  
Vol 75 (5) ◽  
pp. 801-803 ◽  
Author(s):  
Normand Beaulieu ◽  
Susan J Graham ◽  
Roger W Sears ◽  
Edward G Lovering
Keyword(s):  
Mobile Phase ◽  
Raw Materials ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract A liquid chromatographic method was developed for the determination of alprazolam and 5 known related compounds in drug raw materials. The method is based on a 3 µm cyano column (100 x 4.6 mm), a mobile phase of 0.01% phosphoric acidacetonitrile- methanol (6 + 3 +1), a flow rate of 1.5 mL/min, and detection at 230 nm. The method resolves the related compounds from the drug and from each other. The limit of quantitation for the impurities in drug raw material is less than 0.1%. Impurity levels in 4 drug raw materials were between 0.01 and 0.41 %. The corresponding mean assay values ranged from 98.3 to 100.6%.

Liquid Chromatographic Determination of Amiodarone Hydrochloride and Related Compounds in Raw Materials and Tablets

1994 ◽  
Vol 77 (6) ◽  
pp. 1447-1453 ◽  
Author(s):  
Pauline M Lacrok ◽  
Norman M Curran ◽  
Wing-Wah Sy ◽  
Dennis K J Goreck ◽  
Pierre Thibault ◽  
...  
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Amiodarone Hydrochloride ◽  
Related Compounds

Abstract A liquid chromatographic method for the determination of amiodarone hydrochloride and 10 related compounds in drug raw material and for assay of drug in tablets was developed. The method specifies a 3 jxm Hypersil nitrile column (150 × 4.6 mm), a mobile phase of 1 + 1 acetonitrile–ammonium acetate buffer (0.1 M adjusted to pH 6.0 with 0.1 M acetic acid), a flow rate of 1 mL/min, and detection at 240 nm. The lower limit of quantitation of the related compounds is 0.02% or less. Drug contents in 2 raw material samples were 100.1 and 99.9% and ranged from 98.2 to 99.4% in 3 tablet formulations. Impurity levels in 2 samples of raw material from different manufacturers were ca 0.4%. The presence of 3 of the known related compounds in these samples was confirmed by liquid chromatographymass spectrometry. The method applied to raw materials was evaluated by a second laboratory and found to be satisfactory.

Liquid Chromatographic Determination of Ergot Alkaloids in Wheat

1986 ◽  
Vol 69 (4) ◽  
pp. 697-699
Author(s):  
George M Ware ◽  
Allen S Carman ◽  
Octave J Francis ◽  
Shia S Kuan
Keyword(s):  
Mobile Phase ◽  
Ergot Alkaloids ◽  
Ammonium Phosphate ◽  
Ammonium Hydroxide ◽  
Chromatographic Determination ◽  
Resin Column ◽  
Fluorescence Detector ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A method is described for the determination of individual ergot alkaloids in wheat. The sample is extracted with ethyl acetate-4% ammonium hydroxide (100 + 10), and the extract is cleaned up by liquidliquid partition. The ergot alkaloids are resolved by liquid chromatography (LC), using a porous cross-linked polystyrene-divinylbenzene resin column and a mobile phase consisting of acetonitrile-0.05M dibasic ammonium phosphate (55 + 45) buffered at pH 10.0. The ergot alkaloids ergonovine, ergonovinine, ergotamine, ergotaminine, α-ergocryptine, α-ergocryptinine, ergocristine, and ergocristinine are separated by LC and detected with a fluorescence detector. Recovery of ergot alkaloids added to wheat at levels of 16-760 ng/g averaged 85.6% with a coefficient of variation of 11.1%.

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 pentobarbital in plasma with use of a resin column and an alkaline mobile phase.

1982 ◽  
Vol 28 (8) ◽  
pp. 1772-1774 ◽  
Author(s):  
R N Gupta ◽  
P T Smith ◽  
F Eng
Keyword(s):  
Mobile Phase ◽  
Internal Standard ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Enhanced Sensitivity ◽  
Acidic Drugs ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract We describe a liquid-chromatographic method involving a new, nonsilica column (XAD-2, Hamilton Co.) for pentobarbital in plasma. Plasma is extracted with chloroform after addition of the internal standard, 5-ethyl-5-p-tolyl-barbituric acid. Acidic drugs are back-extracted into alkali, then chromatographed on the resin-base reversed-phase column. The use of alkaline mobile phase allows enhanced sensitivity and detection of barbiturates at 240 nm. The within-run CV for 10 samples was 1.9%, the between-run CV 1.8%. Ten commonly used barbiturates are separated isocratically in less than 15 min. Other commonly prescribed acidic drugs do not interfere with determination of pentobarbital.

scholarly journals Liquid Chromatographic Determination of Scopolamine, Hyoscyamine, and Phenobarbital in Tablets

1997 ◽  
Vol 80 (2) ◽  
pp. 331-334 ◽  
Author(s):  
Susan Ting
Keyword(s):  
Mobile Phase ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Scopolamine Hydrobromide ◽  
Acid Sodium Salt ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic

Abstract A liquid chromatographic method using a reversed- phase C18 column and octanesulfonic acid sodium salt-methanol as the mobile phase was developed for the simultaneous determination of phenobarbi- tal, scopolamine, and hyoscyamine in tablets. The mixture of the 3 drugs was resolved in <8 min. Detector responses were linear for 10 μL injections of the following: scopolamine hydrobromide, 8.25-206.3 μg/mL; hyoscyamine sulfate, 15.01-750.76 μg/mL; and phenobarbital, 250-751 μg/mL. Recoveries from tablets were 100.8% for scopolamine hydrobromide, 100.1% for hyoscyamine sulfate, and 100.3% for phenobarbital. Replicate injections of scopolamine hydrobromide, hyoscyamine sulfate, and phenobarbital gave an overall relative standard deviation of <1.0% (n = 10). The method detected as little as 3.3 ng scopolamine hydrobromide.

Liquid Chromatographic Determination of Cromolyn Sodium and Related Compounds in Raw Materials

1994 ◽  
Vol 77 (6) ◽  
pp. 1439-1442 ◽  
Author(s):  
Randy M Duhaime ◽  
Lorna K Rollins ◽  
Dennis J K Gorecki ◽  
Edward G Lovering
Keyword(s):  
Mobile Phase ◽  
Raw Materials ◽  
Chromatographic Determination ◽  
Cromolyn Sodium ◽  
Raw Material ◽  
Assay Method ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract Liquid chromatographic methods for the assay of cromolyn sodium and 3 related compounds were developed. The methods, which differ only in the composition of the mobile phase, use an octadecylsilane bonded-phase column and an acetonitrile–water–cetyltrimethylammonium bromide mobile phase. Minimum quantitatable amounts of the related compounds were less than 0.05%; assay method precision was better than 1 %. Impurity levels in raw material samples from 4 manufacturers were less than 0.1 %.

Liquid Chromatographic Determination of Glyburide (Glibenclamide) and Its Related Compounds in Raw Materials

1993 ◽  
Vol 76 (5) ◽  
pp. 962-965
Author(s):  
Normand Beaulieu ◽  
Susan J Graham ◽  
Edward G Lovering
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Assay Method ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract A liquid chromatographic method has been developed for the determination of glyburide and 3 known related compounds in drug raw materials. The lower limit of quantitation of the related compounds is about 0.02%. Evaluation of 9 drug raw materials revealed total impurities ranging from 0.17 to 0.65%. The relative standard deviation of the assay method is <1%.

Liquid Chromatographic Determination of Tolrestat and Related Compounds in Raw Materials

1995 ◽  
Vol 78 (3) ◽  
pp. 647-650 ◽  
Author(s):  
Normand Beaulieu ◽  
Pauline M Lacrok ◽  
Roger W Sears ◽  
Edward G Loveremg
Keyword(s):  
Raw Materials ◽  
Chromatographic Determination ◽  
Raw Material ◽  
Liquid Chromatographic Method ◽  
Limit Of Quantitation ◽  
Liquid Chromatographic Determination ◽  
Liquid Chromatographic ◽  
Related Compounds ◽  
Different Sources

Abstract A liquid chromatographic method was developed for the determination of tolrestat and 7 related compounds. The lower limit of quantitation of the related compounds in the presence of the drug was <0.05%. The coefficient of variation on the assay of drug raw material analyzed on 5 different days was 0.75%. Total impurities found in 2 samples of tolrestat from different sources were 0.12 and 0.54%, respectively. The method was validated by a second laboratory.

Liquid Chromatographic Determination of Sodium Salinomycin in Feeds, with Post-Column Reaction

1984 ◽  
Vol 67 (4) ◽  
pp. 701-706 ◽  
Author(s):  
John T Goras ◽  
William R Lacourse
Keyword(s):  
Mobile Phase ◽  
Reaction System ◽  
Chromatographic Determination ◽  
Average Recovery ◽  
Commercial Scale ◽  
Liquid Chromatographic Determination ◽  
Effluent Stream ◽  
Liquid Chromatographic ◽  
Related Compounds

Abstract A method for the detection and quantitation of sodium salinomycin in feeds by a liquid chromatographic, post-column reaction system is presented. Sodium salinomycin is leached from feed with hexane, isolated as a dried residue, and dissolved in mobile phase for analysis. The drug is separated from interfering substances on a silica LC column, combined with vanillin reagent in a mixing tee, reacted with vanillin at elevated temperature in a coil, and detected in the effluent stream at 527 nm. Response, as peak area, is linear with concentration. Feed components, other common veterinary drugs, and closely related compounds do not interfere. Average recovery and coefficient of variation (CV) values for liquid spiked feeds and supplements were 101 ± 3.5% and 100 ± 0.3%, respectively. Results for laboratory blends and commercial scale feeds were within 6% of intent with CV values ranging from 0.4 to 5.1%.

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