scholarly journals Determination of Oxycodone Hydrochloride in Oral Solutions by High-Performance Thin-Layer Chromatography/Densitometry

2000 ◽  
Vol 83 (6) ◽  
pp. 1497-1501
Author(s):  
Hannele E M Salomies ◽  
Piia K Salo

Abstract A thin-layer chromatography/densitometry method was developed and validated for the determination of oxycodone hydrochloride in oral solutions by using silica gel plates. A horizontal technique was used for development of the plates. The optimum composition for the mobile phase, which provided a suitable Rf value of 0.6 for oxycodone, was propanol–acetic acid–water–25% ammonia–methanol (20 + 1 + 1 + 3 + 10). Detection was at 234 nm. Oxycodone hydrochloride was stable on the sorbent and was precisely and accurately measured in the range of 0.3–1.5 μg/band.

2000 ◽  
Vol 83 (6) ◽  
pp. 1480-1483 ◽  
Author(s):  
Sateesh K Chauhan ◽  
Brijpal Singh ◽  
Sudhakar Agrawal

Abstract A simple and reproducible high-performance thin-layer chromatographic method was developed for the simultaneous determination of bergenin and gallic acid in Bergenia ligulata. Water and methanol were used as the extracting solvents. The concentrations of bergenin and gallic acid in both of these solvents were found to be almost the same. The method involves separation of the components by thin-layer chromatography on a precoated Silica Gel 60 F254 plate with a solvent system of ethyl acetate–formic acid–acetic acid–water (100 + 11 + 11 + 27). The sensitivity of the method for bergenin was 0.30 μg, whereas for gallic acid it was 0.25 μg. The proposed method is precise and sensitive and can be used for the detection, monitoring, and simultaneous quantification of bergenin and gallic acid in B. ligulata.


2013 ◽  
Vol 8 ◽  
pp. ACI.S12349 ◽  
Author(s):  
Ola Mohamed El-Houssini

Two simple, accurate and reproducible methods were developed and validated for the simultaneous determination of paracetamol (PARA) and pamabrom (PAMB) in pure form and in tablets. The first method was based on reserved-phase high-performance liquid chromatography, on a Thermo Hypersil ODS column using methanol:0.01 M sodium hexane sulfonate:formic acid (67.5:212.5:1 v/v/v) as the mobile phase. The flow rate was 2 mL/min and the column temperature was adjusted to 35 °C. Quantification was achieved with UV detection at 277 nm over concentration range of 100-600 and 4-24 μg/mL, with mean percentage recoveries were found to be 99.90 ± 0.586 and 99.26 ± 0.901 for PARA and PAMB, respectively. The second method was based on thin-layer chromatography separation of PARA and PAMB followed by densitometric measurement of the spots at 254 nm and 277 nm for PARA and PAMB respectively. Separation was carried out on aluminum sheet of silica gel 60F254 using dichloromethane:methanol:glacial acetic acid (7.5:1:0.5 v/v/v) as the mobile phase over concentration range of 1-10 and 0.32-3.20 μg per spot, with mean percentage recovery of 100.52 ± 1.332 and 99.71 ± 1.478 for PARA and PAMB, respectively. The methods retained their accuracy in presence of up to 50% of P-aminophenol and could be successfully applied in tablets.


2005 ◽  
Vol 88 (5) ◽  
pp. 1537-1543 ◽  
Author(s):  
Caitlin Sullivan ◽  
Joseph Sherma

Abstract A new quantitative method using silica gel high-performance thin-layer chromatography plates with channels and a concentration zone, manual application of standards and samples, development with methanol–ethyl acetate (15 + 85) mobile phase, and ultraviolet absorption densitometry is reported for the determination of caffeine in diuretic pharmaceutical preparations. Tablet and capsule products containing potassium salicylate, acetaminophen, and salicylamide as active ingredients were analyzed to test the applicability of the new method, and precision, accuracy, linearity, limits of detection and quantitation, and selectivity were validated. The milligrams of caffeine in each tablet ranged from 48.0 to 51.0, and the milligrams in each capsule from 37.9 to 40.3. Within-day precision was 1.48 and 1.78% (n = 6), and interday precision 0.723 and 1.26% (n = 5) for analysis of 2 tablets and 2 capsules, respectively. Accuracy validation of the tablet and capsule results produced errors of 1.0 and 1.9% for spiked blank analyses and 2.6 and 3.5% for standard addition analyses, respectively. A comparative study using a caffeine standard solution and a multicomponent analgesic tablet solution containing caffeine, acetaminophen, and acetylsalicylic acid showed that manual application on the concentration zone, instrumental application on the concentration zone, and instrumental application on the silica gel gave quite similar results in terms of number of theoretical plates, resolution, limit of detection, and linearity.


2002 ◽  
Vol 85 (5) ◽  
pp. 1015-1020 ◽  
Author(s):  
Khadiga M Kelani ◽  
Azza M Aziz ◽  
Maha A Hegazy ◽  
Laila Abdel Fattah

Abstract A selective, precise, and accurate method was developed for the determination of cimetidine (C), famotidine (F), and ranitidine hydrochloride (R·HCI)in the presence of their sulfoxide derivatives. The method involves quantitative densitometric evaluation of mixtures of the drugs and their derivatives after separation by high-performance thin-layer chromatography on silica gel plates (10 × 20 cm) with ethyl acetate–isopropanol–20% ammonia (9 + 5 + 4, v/v) as the mobile phase for both C and F and ethyl acetate–methanol–20% ammonia (10 + 2 + 2, v/v) as the mobile phase for R·HCI; Rf values for C, F, and R·HCI and their corresponding derivatives were 0.85 and 0.59, 0.73 and 0.41, and 0.56 and 0.33, respectively. Developing time was approximately 20 min. For densitometric evaluation, peak areas were recorded at 218, 265, and 313 nm for C, F, and R·HCI, respectively. The relationship between concentration and the corresponding peak area was plotted for the ranges of 5–50 μg/spot for C and 2–20 μg/spot for F and R·HCl. Mean recoveries were 100.39 ± 1.33, 99.77 ± 1.30, and 100.09 ± 0.69% for C, F, and R·HCI, respectively. The proposed method was used successfully for stability testing of the pure drugs in the presence of up to 90% of their degradates, in bulk powder and dosage forms. The results obtained were analyzed statistically and compared with those obtained by the official methods.


1999 ◽  
Vol 82 (2) ◽  
pp. 244-247 ◽  
Author(s):  
M H Guermouche ◽  
D Habel ◽  
S Guermouche

Abstract Determination of tinidazole in human serum by high-performance thin-layer chromatography (HPTLC) is presented. It includes use of 10 × 10 cm plates coated with silica gel 60 and chloroform-acetonitrile-acetic acid (60 + 40 + 2) as mobile phase. Quantitation was performed by densitometry at 320 nm. The linearity (1-10 ng), precision (6%), reproducibility (5%), recovery (96%), and detection limit (1 mg/L) of tinidazole determination by HPTLC were comparable with corresponding method parameters by reversed-phase HPLC. A satisfactory correlation was found between the 2 analytical methods. The procedure was used to quantitate tinidazole in patient sera.


2019 ◽  
Vol 2019 ◽  
pp. 1-6 ◽  
Author(s):  
Andrzej Czyrski

The lipophilicity is an important parameter that influences the activity of the drugs in the human body. The reversed phase high performance thin layer chromatography was applied to determine the Log P values of ibuprofen, ketoprofen, naproxen, and flurbiprofen. The stationary phase used in the study was silica-gel coated plates. The mobile phase was the mixture of acetonitrile and water in different proportions. The content of acetonitrile varied in 5% increments from 50% to 80%. The Rm0 values were determined for the compounds with a known Log P and for the analyzed substances (ibuprofen, naproxen, ketoprofen, and flurbiprofen). The Log P values were calculated for the analyzed compounds using the regression curve Rm0 = f(Log P) parameters for the compounds with the known lipophilicity. Flurbiprofen is characterized by the highest Log P value: 3.82. The lowest one is noted for ketoprofen: 2.66. The determined Log P values of tested compounds were similar to the values calculated by the software.


2021 ◽  
Vol 10 (4) ◽  
pp. 2804-2809

Thymus species belong to the Lamiaceae family, of which 18 species in the flora of Iran, 6 are endemic to Iran. In the current research, high-performance thin-layer chromatography (HPTLC) technique as an easy, fast, reproducible, and low-cost method was used for the determination of rosmarinic acid and caffeic acid in Thymus lancifolius (T. lancifolius) and two species of Thymus daenensis (T. daenensis) from Iran. Toluene-ethyl acetate-formic acid with a ratio of 67.72-22.90 and 9.38% was selected as the mobile phase of rosmarinic acid, and ethyl acetate-methanol-formic acid-water with a ratio of 85-8-2 and 5% was designated as the mobile phase of caffeic acid. The highest and lowest amount of rosmarinic acid was observed for T. daenensis 1 (10.54±0.12 mg/g) and T. lancifolius (0.46±0.01 mg/g), respectively. The amount of rosmarinic acid for T. daenensis 2 was obtained as 7.85±0.02 mg/g for each of the dried plants. In the following, HPTLC analysis of caffeic acid for T. daenensis 1, T. daenensis 2, and T. lancifolius was acquired amounts of 0.78±0.007, 0.13±0.007, and 0.26±0.007 mg/g for each of dried plants, respectively. Therefore, regarding the special effects of phenolic acids and properties of the Thymus genus, the acquired results are suitable for application in pathogenic research, infections, immunology diseases, and evaluation of the antioxidant activity.


2006 ◽  
Vol 89 (4) ◽  
pp. 995-998 ◽  
Author(s):  
Magdalena Wójciak-Kosior ◽  
Agnieszka Skalska ◽  
Grażyna Matysik ◽  
Magdalena Kryska

Abstract In this paper, a high-performance thin-layer chromatography (HPTLC) method combined with densitometry has been described. Chromatography was performed on silica gel Si 60F254 plates using dichloromethaneethyl acetateformic acid (9.5 + 0.5 + 0.1, v/v) mobile phase. This method has been successfully applied for the determination of phenobarbital in pharmaceuticals. Obtained results were comparable with traditionally used column high-performance liquid chromatography (HPLC) methods. For the proposed procedure, linearity (r > 0.999), sensitivity (limit of detection 0.4 g/spot), recovery (97.8102.1%), and repeatability were found to be satisfactory. The HPTLC-densitometry method has many advantages, such as simplicity, reasonable sensitivity, rapidity, and low cost, and it can be successfully used in routine quality control of multidrug preparations containing barbiturates.


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