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

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%.

1993 ◽  
Vol 76 (6) ◽  
pp. 1187-1192
Author(s):  
Raj P Singh ◽  
Mikio Chiba

Abstract A liquid chromatographic (LC) method is reported for the simultaneous determination of benomyl, methyl {1 -[(butylamino)carbonyl]-1 H-benzimidazol-2-yl}carbamate and carbendazim, methyl 1H-benzimidazol-2-ylcarbamate (MBC), in wettable powder (WP) formulations. In this method, benomyl is converted to 3-butyl-2,4-dioxo-s-triaz-ino[1,2-a]benzimidazole (STB) in 0.125M sodium hydroxide. After conversion (at room temperature in 20 min), STB is determined simultaneously with MBC (which remains intact with the sodium hydroxide treatment) at 286 nm after LC separation on a C18 column. The method was accurate and showed good reproducibility, with relative standard deviations of 0.7 and 2.2% for benomyl and MBC determinations, respectively.


2008 ◽  
Vol 91 (6) ◽  
pp. 1271-1277 ◽  
Author(s):  
M Nurul Islam ◽  
Hye Hyun Yoo ◽  
Jun Lee ◽  
Joo Won Nam ◽  
Eun Kyoung Seo ◽  
...  

Abstract The rhizomes of Anemarrhena asphodeloides Bunge (Liliaceae) are prescribed as crude drugs in herbal medication for the treatment of various diseases such as diabetes, inflammation, and platelet aggregation inhibition. A simple, sensitive, and precise reversed-phase liquid chromatographic method was developed to study the quantitative determination of 5 bioactive compounds from these rhizomes, namely, neomangiferin, mangiferin, isomangiferin, nyasol, and methylnyasol. Chromatographic analysis was performed on Capcell Pak C18 column (150 4.6 mm, 3 m) with a mobile phase consisting of acetonitrile, methanol, and 0.1 formic acid at a flow rate of 1.00 mL/min. Quantitation was performed using a UV-visible detector at 260 nm. The method for the determination of reported medicinal agents was accurate and reproducible. Excellent linear behavior was observed over the investigated concentration range of 2.5100.0 g/mL for neomangiferin; 1.560.0 g/mL for mangiferin; 0.520.0 g/mL for nyasol; and 0.220.0 g/mL for methylnyasol; correlation coefficient >0.99. The intraday and interday precision over the concentration range of compounds was <6.6 (relative standard deviation) and accuracy was between 94.9 and 109.3. This method can be successfully applied for the analysis of medicinal compounds from the ethanolic extract of A. asphodeloides Bunge.


1993 ◽  
Vol 76 (2) ◽  
pp. 414-417 ◽  
Author(s):  
Henry S Kim ◽  
Gerald Angyal

Abstract A reversed-phase liquid chromatographic (LC) method coupled with precolumn derivatization of L-tryptophan with phenylisothiocyanate was compared to the AOAC microbiological method for determining L-tryptophan in tablets and capsules. For the microbiological method, the concentrations of L-tryptophan were 4-8% lower in autoclaved test samples (hot method) than in test samples that were not autoclaved (cold method). When L-tryptophan values obtained by the LC method were compared to those obtained by the cold microbiological method, no significant differences were observed (P > 0.05). The mean relative standard deviations were 2.9% for the LC method and 1.6% for the cold microbiological method. The mean recoveries of standard L-tryptophan added before analysis were 99% for the LC method and 101 % for the cold microbiological method. These results demonstrate that both methods are reliable for determining free L-tryptophan contained in tablets and capsules. However, the LC method has the advantages of using a smaller test portion and having a shorter analysis time.


1992 ◽  
Vol 75 (1) ◽  
pp. 26-29 ◽  
Author(s):  
Mei-Chich Hsu ◽  
Yann-Jen Fann

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.


1991 ◽  
Vol 5 (2) ◽  
pp. 78-82 ◽  
Author(s):  
E. Mendez-Alvarez ◽  
R. Soto-Otero ◽  
G. Sierra-Paredes ◽  
E. Aguilar-Veiga ◽  
J. Galan-Valiente ◽  
...  

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