Determination of Bergapten in Fragrance Preparations by Thin Layer Chromatography and Spectrophotofluorometry

1976 ◽  
Vol 59 (3) ◽  
pp. 547-551
Author(s):  
Harris H Wisneski
Keyword(s):  
Acetic Acid ◽  
Carbon Tetrachloride ◽  
Thin Layer ◽  
Ethyl Acetate ◽  
Thin Layer Chromatography ◽  
Digital Integrator ◽  
Average Recovery ◽  
Tert Butylamine ◽  
Layer Chromatography

Abstract A method has been developed for the determination of bergapten (5-methoxypsoralen), a known phototoxin, in perfumes, colognes, and toilet waters. The bergapten and other lactonic compounds were first isolated from the sample by a series of extractions. The extract containing the bergapten was diluted to a known volume and an aliquot was spotted on a thin layer chromatographic (TLC) plate coated with silica gel G. After 2-dimensional development with hexane - carbon tetrachloride - tert - butylamine (180 + 12 + 9) and hexane-toluene-ethyl acetate-acetic acid (100+10+15+0.5), the TLC plate was dried and the emitted fluorescence of bergapten was measured, using a spectrophotofluorometer equipped with a TLC accessory and coupled to an automatic digital integrator. The amount of bergapten was determined by comparing its peak area to those of bergapten standards. The average recovery for levels of 0.001, 0.005, and 0.01% bergapten was 88%.

Improved Method for the Thin Layer Chromatographic Determination of Patulin in Apple Juice

1973 ◽  
Vol 56 (4) ◽  
pp. 813-816 ◽  
Author(s):  
Peter M Scott ◽  
Barry P C Kennedy
Keyword(s):  
Thin Layer ◽  
Ethyl Acetate ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Apple Juice ◽  
Chromatographic Determination ◽  
Improved Method ◽  
Layer Chromatography ◽  
Hydrochloride Solution

Abstract Apple juice from a freshly opened container is extracted 3 times with ethyl acetate. The extract is dried, concentrated, diluted with benzene, and added to a silica gel column. Patulin is eluted by benzene-ethyl acetate (75+25) and detected by thin layer chromatography, using a 3-methyl-2-benzothiazolinone hydrazone hydrochloride solution as the spray reagent. Satisfactory recoveries were obtained for patulin added to apple juice at levels of 25–400 μg/L.

Determination of 3-Methoxy-4-Hydroxymandelic Acid (VMA) in Urine by Thin-Layer Chromatography

1965 ◽  
Vol 11 (10) ◽  
pp. 905-913 ◽  
Author(s):  
J S Annino ◽  
M Lipson ◽  
L A Williams
Keyword(s):  
Thin Layer ◽  
Ethyl Acetate ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Potassium Carbonate ◽  
Several Variables ◽  
Fast Red ◽  
Layer Chromatography

Abstract From studies of several variables, a method has been developed for the separation and quantitation of 3-methoxy-4-hydroxymandelic acid (VMA) in urine by thin-layer chromatography. The urine is pretreated with acid and Florisil, and then extracted with ethyl acetate. Thin-layer chromatography is performed on silica gel with a butanol: acetic acid:water solution. The VMA spot is located by spraying with fast red GG and potassium carbonate. After removal from the plate, maximum color is developed and quantitated by reading in a spectrophotometer at 510 mµ.

Colorimetric Determination of Terreic Acid Produced by Aspergillus terreus

1978 ◽  
Vol 61 (3) ◽  
pp. 581-583
Author(s):  
Thirugnana Subramanian ◽  
Kuppuswamy Mohan Namasivayam ◽  
Edayathimangalam R B Shanmugasundaram
Keyword(s):  
Thin Layer ◽  
Ethyl Acetate ◽  
Thin Layer Chromatography ◽  
Lower Limit ◽  
Minimal Medium ◽  
Aspergillus Terreus ◽  
Limit Of Detection ◽  
Colorimetric Determination ◽  
Layer Chromatography

Abstract Two methods have been developed for determining terreic acid, which is a mycotoxin produced by Aspergillus terreus, a common food contaminant. The organism was grown independently in synthetic minimal medium, bread, and rice. After 15 days of growth, the toxin was extracted with ethyl acetate, cleaned up by thin layer chromatography, and determined colorimetrically, using Folin's reagent or 2,4- dinitrophenylhydrazine. The production of terreic acid was greater on bread than on rice or minimal medium. Recoveries of 200–400 ≧g terreic acid/100 g bread and rice ranged from 62 to 98%. The lower limit of detection was 200 ≧g/100 g.

Determination of Cimetidine, Famotidine, and Ranitidine Hydrochloride in the Presence of Their Sulfoxide Derivatives in Pure and Dosage Forms by High-Performance Thin-Layer Chromatography and Scanning Densitometry

2002 ◽  
Vol 85 (5) ◽  
pp. 1015-1020 ◽  
Author(s):  
Khadiga M Kelani ◽  
Azza M Aziz ◽  
Maha A Hegazy ◽  
Laila Abdel Fattah
Keyword(s):  
Thin Layer ◽  
Ethyl Acetate ◽  
Thin Layer Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Accurate Method ◽  
Dosage Forms ◽  
Ranitidine Hydrochloride ◽  
Layer Chromatography

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.

Preparing a New Chromatographic support from Local Syrian Clay and using it in Thin Layer Chromatography for Simultaneous Determination of Paracetamol, Caffeine and Aspirin in Tablets

2021 ◽  
pp. 2119-2124
Author(s):  
Amir Alhaj Sakur ◽  
Firas Mannaa ◽  
Mahamed Yahia Zein Eddin
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Mobile Phase ◽  
Dosage Forms ◽  
Thin Layers ◽  
Raw Material ◽  
Average Recovery ◽  
Layer Chromatography ◽  
Chloroform Methanol

A new chromatographic support was prepared from Local Syrian Clay (Bentonite), using thermal and acid treated Clay (B500AW) for utilizing it in thin layer chromatography (0.25mm thickness) to separate and determine of Paracetamol, Caffeine, and Aspirin in raw material and in tablets. The separation carried out using mobile phase consisted of Cyclohexane-Chloroform- Methanol - acetic acid (14:5: 0.25:0.75) v/v. The specific surface area of treated bentonite was 45m2/g. Quantification was carried out densitometerically at λ = 250nm for Paracetamol, λ = 275nm for Caffeine, and at λ = 200 nm for Aspirin. The retardation factors (Rf) of Paracetamol, Caffeine, and Aspirin were 0.10, 0.21, and 0.40 respectively. Calibration curves were obtained in the concentration ranges of 5.0-40.0µg/spot, 2.0-16.0µg/spot and 3.0-24.0µg/spot for standard solutions of Paracetamol, Caffeine and Aspirin respectively. The New Prepared Chromatographic Thin Layers were successfully applied for analysis of commercial dosage forms (tablets) containing the drugs with average recovery 98.33 –101.83% with RSD not more than 3.86%.

scholarly journals Determination of Rosmarinic Acid and Caffeic Acid in Thymus daenensis and Thymus lancifolius Extracts by High-Performance Thin Layer Chromatography

2021 ◽  
Vol 10 (4) ◽  
pp. 2804-2809
Keyword(s):  
Thin Layer ◽  
Formic Acid ◽  
Ethyl Acetate ◽  
Thin Layer Chromatography ◽  
Caffeic Acid ◽  
Rosmarinic Acid ◽  
Mobile Phase ◽  
High Performance ◽  
Layer Chromatography

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.

Thin Layer Chromatographic Determination of Aflatoxins in Dry Ginger Root and Ginger Oleoresin

1980 ◽  
Vol 63 (5) ◽  
pp. 1052-1054 ◽  
Author(s):  
Mary W Trucksess ◽  
Leonard Stoloff
Keyword(s):  
Carbon Tetrachloride ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Fish Meal ◽  
Chromatographic Determination ◽  
Adsorption Column ◽  
Mixed Feeds ◽  
Layer Chromatography

Abstract A method for determining aflatoxins in dry ginger root and ginger oleoresin, using 1-dimensional thin layer chromatography (TLC) for the determinative step, has been developed. The key cleanup steps that permit this change from the 2-dimensional TLC previously required are partitioning of the extract with carbon tetrachloride and use of an improved eluting system for the silica gel adsorption column. Recoveries of aflatoxins B1, B2, G1, and G2 added to samples of ground ginger were 82, 101, 106, and 110%, respectively; recoveries of these aflatoxins added to ginger oleoresin were 75, 100, 93, and 125%, respectively. The method is applicable to fish meal and a number of mixed feeds.

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
Keyword(s):  
Acetic Acid ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
Mobile Phase ◽  
High Performance ◽  
Acetic Acid Water ◽  
Oxycodone Hydrochloride ◽  
Layer Chromatography

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.

scholarly journals High-Performance Thin-Layer Chromatography Determination of Some Antimycotic Imidazole Derivatives and Preservatives in Medicinal Creams and a Gel

2005 ◽  
Vol 88 (5) ◽  
pp. 1544-1548 ◽  
Author(s):  
Mira Čakar ◽  
Gordana Popović ◽  
Danica Agbaba
Keyword(s):  
Carbon Tetrachloride ◽  
Benzoic Acid ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Benzyl Alcohol ◽  
High Performance ◽  
Butyl Acetate ◽  
Mobile Phases ◽  
Layer Chromatography

Abstract Simple and reliable thin-layer chromatography-densitometry methods for determination of antimycotics (bifonazole, clotrimazole, and miconazole) and preservatives (benzyl alcohol and benzoic acid) were developed. The pairs bifonazole/benzyl alcohol, clotrimazole/benzyl alcohol, and miconazole/benzoic acid were determined simultaneously. The following mobile phases were used: ethyl acetate–n-heptane–methanol–diethylamine (3 + 4.5 + 1 + 0.2, v/v/v/v) for bifonazole and benzyl alcohol; n-butyl acetate–n-heptane–methanol–dietylamine (3 + 4.5 + 1 + 0.2, v/v/v/v) for clotrimazole and benzyl alcohol; and n-butyl acetate–carbon tetrachloride–methanol–diethylamine (3 + 6 + 2.5 + 0.5, v/v/v/v) for miconazole and benzoic acid. The chromatographic zones on silica gel plates were scanned in the reflectance/absorbance mode at 230 nm (bifonazole, benzyl alcohol, miconazole, and benzoic acid) and 210 nm (clotrimazole and benzyl alcohol). The recovery for all substances ranged from 98.7 to 100.7%. The limits of detection and quantitation were 0.03 to 0.2 μg and 0.1 to 0.5 μg/spot, respectively. The proposed methods were applied for determination of antimycotics and preservatives in commercially available pharmaceuticals.

Fluorometric and Thin Layer Chromatographic Determination of Aminacrine and Its Salts in Drug Preparations

1966 ◽  
Vol 49 (4) ◽  
pp. 837-840
Author(s):  
Laura A Roberts
Keyword(s):  
Carbon Tetrachloride ◽  
Thin Layer ◽  
Quantitative Determination ◽  
Thin Layer Chromatography ◽  
Chromatographic Determination ◽  
Basic Solution ◽  
Antimony Pentachloride ◽  
Fluorometric Method ◽  
Layer Chromatography

Abstract A fluorometric method has been developed for the quantitative determination of aminacrine (USAN name for 9-aminoacridine) and its salts in a wide variety of drug preparations. Aminacrine is extracted with chloroform from basic solution, the chloroform is evaporated, and the residue is dissolved in acidic ethanol. Aminacrine is identified by thin layer chromatography; travel of sample and standard spots is compared under ultraviolet light. Aminacrine is confirmed by spraying the plate with a solution of antimony pentachloride in carbon tetrachloride to produce a yellow spot.

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