scholarly journals Simultaneous Determination of Hyoscine Butylbromide and Ketoprofen in Pharmaceutical Preparations by Spectrophotometric and Liquid Chromatographic Methods

2007 ◽  
Vol 90 (1) ◽  
pp. 102-112 ◽  
Author(s):  
Yasser Shaker El-Saharty ◽  
Fadia H Metwally ◽  
Mohamed Refaat ◽  
Sonia Zaki El-Khateeb
Keyword(s):  
Pharmaceutical Preparations ◽  
Standard Addition ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Hyoscine Butylbromide ◽  
Mathematical Algorithm ◽  
Accuracy And Precision ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A binary mixture of hyoscine butylbromide and ketoprofen was determined by 4 different methods. The first involved determination of hyoscine butylbromide and ketoprofen using the ratio-spectra first-derivative spectrophotometric technique at 211 and 234 nm over the concentration ranges of 2-14 and 5-45 μg/mL with mean accuracies 99.84 ± 0.92 and 99.98 ± 0.64%, respectively. The second method utilized second-derivative spectrophotometry over the concentration ranges of 2-14 and 5-35 μg/mL with mean accuracies 99.32 ± 1.06 and 99.55 ± 1.15%, respectively. The third method was based on the resolution of the 2 components by bivariate calibration depending on a simple and rapid mathematical algorithm and quantitative evaluation of the absorbances at 206 and 254 nm over concentration ranges of 2-16 and 5-35 μg/mL; mean accuracies of 100.21 ± 1.30 and 100.19 ± 1.07% were obtained for hyoscine butylbromide and ketoprofen, respectively. The fourth method was reversed-phase liquid chromatography using 0.05 M ammonium dihydrogen phosphateacetonitrilemethanol (20 + 30 + 6, v/v) as the mobile phase with ultraviolet detection at 220 nm over concentration ranges of 1-90 and 5-70 μg/mL; mean accuracies were 99.92 ± 1.02 and 99.61 ± 0.98%, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical preparations. The methods retained their accuracy and precision when the standard addition technique was applied. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

Determination of Dicloxacillin Preparations by Liquid Chromatography

1992 ◽  
Vol 75 (1) ◽  
pp. 26-29 ◽  
Author(s):  
Mei-Chich Hsu ◽  
Yann-Jen Fann
Keyword(s):  
Internal Standard ◽  
Pharmaceutical Preparations ◽  
Standard Addition ◽  
Reversed Phase ◽  
Microbiological Method ◽  
Absorbance Detection ◽  
Liquid Chromatographic Method ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic method was developed for the assay of dicloxacillin In bulk drugs and pharmaceutical preparations. The samples were analyzed on a μBondapak (C18) column with a mobile phase of methanol-4% acetic acid (60 + 40) at a flow rate of 1.5 mL/mln, with UV absorbance detection at 254 nm. An equation was derived showing a linear relationship between peak area ratios of dicloxacillin to dimethylphthalate (internal standard) and the dicloxacillin concentration over a range of 2-30 μg (r = 0.9999). Standard addition recoveries ranged from 98.65 to 100.74% (mean 99.70%, n = 6). The coefficient of variation was less than 0.24%. The assay results were compared with those obtained by the official microbiological method, which indicated that the proposed method Is a suitable substitute for the microbiological method for potency assays and stability studies of dicloxacillin preparations.

scholarly journals Simultaneous Determination of Piracetam and Vincamine by Spectrophotometric and High-Performance Liquid Chromatographic Methods

2008 ◽  
Vol 91 (2) ◽  
pp. 311-321 ◽  
Author(s):  
Yasser Shaker Ibrahim El-Saharty
Keyword(s):  
High Performance ◽  
Pharmaceutical Preparation ◽  
Standard Addition ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Potassium Dihydrogen ◽  
Accuracy And Precision ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A mixture of piracetam and vincamine was determined by 3 different methods. The first was the determination of piracetam and vincamine using the ratio-spectra first-derivative (DD1) spectrophotometric technique at 209 and 293 nm in concentration ranges of 1045 and 214 g/mL with mean recoveries of 99.22 0.72 and 99.67 0.79, respectively. The second method was based on the resolution of the 2 components by bivariate calibration depending on a mathematic algorithm that provides simplicity and rapidity. The method depended on quantitative evaluation of the absorbencies at 210 and 225 nm in concentration ranges of 545 and 214 g/mL, with mean recoveries of 100.33 0.54 and 100.44 0.98 for piracetam and vincamine, respectively. The third method was reversed-phase liquid chromatography using 0.05 M potassium dihydrogen phosphatemethanol (50 + 50, v/v) as the mobile phase, with the pH adjusted to 3.5 with phosphoric acid. The eluent was monitored at 215 nm in concentration ranges of 5100 and 2200 g/mL, with mean recoveries of 99.62 0.67 and 99.32 0.85 for piracetam and vincamine, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparation. The methods retained their accuracy and precision when applying the standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

scholarly journals Application of Liquid Chromatography to the Simultaneous Determination of Acetylsalicylic Acid, Caffeine, Codeine, Paracetamol, Pyridoxine, and Thiamine in Pharmaceutical Preparations

2001 ◽  
Vol 84 (3) ◽  
pp. 676-683 ◽  
Author(s):  
Natividad Ramos-Martos ◽  
Francisco Aguirre-Gómez ◽  
Antonio Molina-Díaz ◽  
Luis F Capitán-Vallvey
Keyword(s):  
Salicylic Acid ◽  
Acetylsalicylic Acid ◽  
Simultaneous Determination ◽  
Pharmaceutical Preparations ◽  
Reversed Phase ◽  
Liquid Chromatographic Method ◽  
Relative Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract This paper describes a rapid reversed-phase liquid chromatographic method, with UV detection, for the simultaneous determination of acetylsalicylic acid, caffeine, codeine, paracetamol, pyridoxine, and thiamine in pharmaceutical preparations. A reversed-phase C18 Nucleosil column is used. The mobile phase consists of 2 successive eluants: water (5 min) and acetonitrile–water (75 + 25, v/v; 9 min), both adjusted to pH 2.1 with phosphoric acid. Before determination acetylsalicylic acid is completely converted to salicylic acid by alkaline hydrolysis. Salicylic acid, caffeine, paracetamol, pyridoxine, and thiamine are all detected at 285 nm, whereas codeine is detected at 240 nm. Calibration curves were linear for salicylic acid, caffeine, paracetamol, and pyridoxine in the range of 50–500 mg/L, and for codeine and thiamine in the range of 50–1000 mg/L. The method was applied to the analysis of 13 fortified commercial pharmaceutical preparations. Recoveries ranged from 92.6 to 105.5%, with relative standard deviations of 1.1–5.8%.

scholarly journals Liquid Chromatographic/Mass Spectrometric Determination of Desmedipham and Phenmedipham and Their Metabolites in Soil

2001 ◽  
Vol 84 (5) ◽  
pp. 1407-1412 ◽  
Author(s):  
Daniela Perret ◽  
Alessandra Gentili ◽  
Stefano Marchese ◽  
Aldo Marino ◽  
Federica Bruno
Keyword(s):  
Reversed Phase ◽  
Soil Types ◽  
Liquid Chromatography Mass Spectrometry ◽  
Reversed Phase Liquid Chromatography ◽  
Soil Suspension ◽  
Simple Method ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Chromatographic Mass

Abstract A simple method is described for the simultaneous determination of residues of 2 carbamate herbicides (phenmedipham and desmedipham) and related metabolites (m-aminophenol, aniline, and m-toluidine) in soil. The analytes are extracted from spiked soils with methanol. The solvent/soil suspension is centrifuged, and the supernatant is directly injected, without any further cleanup, into a reversed-phase liquid chromatography/mass spectrometry apparatus equipped with a TurboIonSpray interface. The method was tested on 5 soils having different physicochemical properties. Recoveries from the soil types, spiked over the range of 50–200 ppb, were essentially quantitative for each analyte. The detection limits of the method are ≤25 ng/g.

Liquid Chromatographic Determination of 2-Chloro-4-nitroaniline, 2-Naphthol, and 2,4-Dinitroaniline in D&C Red No. 36

1993 ◽  
Vol 76 (2) ◽  
pp. 287-291 ◽  
Author(s):  
Alan L Scher ◽  
Nicholas C Adamo
Keyword(s):  
Chromatographic Determination ◽  
Reversed Phase ◽  
Calibration Data ◽  
Reversed Phase Liquid Chromatography ◽  
Relative Standard ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic ◽  
Cellulose Column

Abstract A method is described for the determination of the intermediates and a related impurity in D&C Red No. 36 by reversed-phase liquid chromatography. This method may be used to ensure that limits set forth in the Code of Federal Regulations on the amounts of these 3 impurities in the color are not exceeded. The pigment is dissolved in boiling dioxane and then precipitated. The filtrate is chromatographed by isocratic elution, and then the column is washed and reequilibrated. Impurities were identified as 2-chloro-4-nitroaniline (2-CI-4-NA), 2-naphthol, and 2,4-dinitroaniline (2,4-DNA) by comparison of their retention times and spectra with those of standards. Peak area calibrations were linear to at least 0.375% 2-CI-4-NA, 1.25% 2-naphthol, and 0.025% 2,4-DNA, all with zero intercepts. At the specification levels, 99% confidence limits were 0.30 ± 0.006% for 2-CI-4-NA, 1.0 ± 0.03% for 2-naphthol, and 0.020 ± 0.0004% for 2,4-DNA. The limits of determination calculated from calibration data were 0.019% for 2-CI-4-NA, 0.10% for 2-naphthol, and 0.0014% for 2,4-DNA at the 99% confidence level. Recoveries were 100-104% for 2-CI-4-NA added to purified D&C Red No. 36,100% for 2-naphthol, and 100-110% for 2,4-DNA; relative standard deviations were 0.8-3.4%. A survey of certified D&C Red No. 36 samples showed that the batches contained higher levels of intermediates than were determined previously by a cellulose column method in which the pigment was not dissolved.

scholarly journals Determination of Four Fluoroquinolones in Milk by On-Line Immunoaffinity Capture Coupled with Reversed-Phase Liquid Chromatography

1999 ◽  
Vol 82 (3) ◽  
pp. 607-613 ◽  
Author(s):  
Carol K Holtzapple ◽  
Sandra A Buckley ◽  
Larry H Stanker
Keyword(s):  
Raw Milk ◽  
Reversed Phase ◽  
Immunoaffinity Column ◽  
Isocratic Elution ◽  
Reversed Phase Liquid Chromatography ◽  
Sample Matrix ◽  
On Line ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract An automated, on-line immunoaffinity extraction method was developed for the analysis of 4 fluoroquinolones in milk: ciprofloxacin, difloxacin, enrofloxacin, and sarafloxacin. This method involves analyte extraction using an immunoaffinity capture column containing anti-fluoroquinolone antibodies coupled on-line with reversed-phase column chromatography. Liquid chromatographic analyses were performed by isocratic elution using a mobile phase of 2% acetic acid-acetonitrile (85 + 15) and an Inertsil phenyl column with fluorescence detection at excitation and emission wavelengths of 278 and 444 nm, respectively. No significant interferences from the sample matrix were observed, indicating good selectivity with the immunoaffinity column. Recoveries from fortified raw milk samples (5–50 ppb of each fluoroquinolone) ranged from 72 to 90%, with standard deviations of ≤8%.

scholarly journals Determination of Methomyl in Insecticidal Formulations by Reversed-Phase Liquid Chromatography: Collaborative Study

1996 ◽  
Vol 79 (4) ◽  
pp. 941-948
Author(s):  
James E Conaway ◽  
J B Audino ◽  
E Bane ◽  
S K Carrigan ◽  
R Glinsky ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Coefficient Of Variation ◽  
Mobile Phase ◽  
Collaborative Study ◽  
Internal Standard ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A reversed-phase liquid chromatographic (LC) method for methomyl was studied. Twelve collaborators analyzed 3 solid and 4 liquid formulations on both a Zorbax octadecylsilane (ODS) column and a similar column of their choice. Methomyl and the internal standard were separated by using a mobile phase consisting of approximately 8% acetonitrile in water, which was monitored at 254 nm. The coefficient of variation on the Zorbax column ranged from 0.70 to 5.23%, while the range on the collaborators' house columns was 1.08 to 6.01%. Results with the Zorbax ODS column fell within the 5% 2-tail limits, and 10 of 11 collaborators' results fell within these limits on house columns. The LC method for determination of methomyl in insecticidal formulations has been adopted first action by AOAC INTERNATIONAL.

Liquid-chromatographic determination of cyclosporine in serum with use of a rapid extraction procedure.

1982 ◽  
Vol 28 (11) ◽  
pp. 2269-2271 ◽  
Author(s):  
G C Yee ◽  
D J Gmur ◽  
M S Kennedy
Keyword(s):  
Extraction Procedure ◽  
Chromatographic Determination ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Assay Methods ◽  
Liquid Chromatographic

Abstract In this procedure, reversed-phase liquid chromatography is used to measure cyclosporine, a fungal metabolite with immunosuppressive activity, in human serum. With a gradient elution, the retention times for cyclosporine and cyclosporin D were 14.1 and 15.7 min, respectively. Ultraviolet absorbance at 215 nm was used to detect cyclosporine; this wavelength improved assay accuracy without decreasing sensitivity, as compared with detection at 205 nm, which is near the absorption maximum. The major advantage of our procedure is the clean-up method, which involves use of disposable extraction columns. This extraction is simple and requires only 10 to 15 min per sample. Results by radioimmunoassay for cyclosporine were unpredictably greater than those measured by the present method. Dosing guidelines for cyclosporine need re-evaluation, based on more specific assay methods.

Chloramphenicol Extraction from Milk by Using the Diphasic Dialysis Method Followed by Liquid Chromatographic Determination

1994 ◽  
Vol 77 (4) ◽  
pp. 854-856 ◽  
Author(s):  
Javier Bayo ◽  
Miguel A Moreno ◽  
Javier Prieta ◽  
Susana Díaz ◽  
Guillermo Suárez ◽  
...  
Keyword(s):  
Working Conditions ◽  
Chromatographic Determination ◽  
Reversed Phase ◽  
Reversed Phase Liquid Chromatography ◽  
Simple Method ◽  
Dialysis Method ◽  
Liquid Chromatographic Determination ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract An economical, fast, and simple method for the extraction and liquid chromatographic determination of chloramphenicol (CAP) in milk is described. CAP is extracted by using a recently developed membrane-based method named “diphasic dialysis.” CAP is detected and quantitated in the organic solvent used in dialysis without additional cleanup steps by reversed-phase liquid chromatography and UV detection (270 nm). The determination imit of CAP in milk was about 5 μg/L, although as little as 1 μg/L could be detected under optimal working conditions.

Quantitation of Cyfluthrin in Liquid and Solid Formulations by Reversed-Phase Liquid Chromatography: Collaborative Study

1995 ◽  
Vol 78 (6) ◽  
pp. 1335-1338 ◽  
Author(s):  
Donald N Harbin
Keyword(s):  
Collaborative Study ◽  
Internal Standard ◽  
Reversed Phase ◽  
Matched Pair ◽  
Reversed Phase Liquid Chromatography ◽  
Pesticide Formulations ◽  
Relative Standard ◽  
Phase Liquid ◽  
Liquid Chromatographic

Abstract A liquid chromatographic (LC) method has been developed for quantitation of cyfluthrin (Baythroid®, Tempo®) in liquid and solid formulations. Cyfluthrin is a synthetic pyrethroid insecticide. Samples are dissolved in acetonitrile and analyzed by reversedphase LC with decanophenone as an internal standard. Seventeen laboratories from 7 countries participated in a collaborative study of the method. Each collaborator was provided with reference standard, internal standard, and matched pair samples of Tempo 20 wettable powder, Tempo 2 emulsifiable concentrate, and Tempo 2 flowable liquid formulations. Collaborators were instructed to use peak area measurements for quantitation. Relative standard deviations for reproducibility (RSDR) were 0.78,0.98, and 2.32, respectively. The LC method for determination of cyfluthrin in pesticide formulations has been adopted first action by AOAC INTERNATIONAL.

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