scholarly journals Rapid Identification and Quantitation of Clotrimazole, Miconazole, and Ketokonazole in Pharmaceutical Creams and Ointments by Thin-Layer Chromatography–Densitometry

1996 ◽  
Vol 79 (3) ◽  
pp. 656-660 ◽  
Author(s):  
Utpal Roychowdhury ◽  
Saroj K Das
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Uv Light ◽  
Internal Standard ◽  
Solvent System ◽  
Short Wave ◽  
Rapid Identification ◽  
Pharmaceutical Creams ◽  
Liquid Chromatographic ◽  
Layer Chromatography

Abstract Thin-layer chromatography (TLC)–densitometry was used to separate, identify, and quantitate clotrimazole, miconazole, and ketokonazole (alone or combined with other drugs) in various pharmacopoeial or proprietary creams and ointments. Clotrimazole was extracted from the cream or ointment with ethyl alcohol, and miconazole and ketokonazole were extracted with a mixture of equal volumes of chloroform and isopropyl alcohol. Active ingredients were separated from excipients and other drugs by TLC on a precoated silica gel F254 plate with a solvent system of n-hexane–chloroform–methanol–diethylamine (50 + 40 + 10 + 1, v/v). The 3 azoles were well separated and easily identified in this chromatographic system. The separated azoles were visualized under short-wave UV light and quantitated by scanning densitometry at 220 nm by comparing the integrated areas of samples with those of standard (one azole was used as internal standard for the other). Recoveries from samples spiked with known amounts of azoles were excellent. The method was validated further by comparison with official liquid chromatographic methods.

OPTIMIZATION OF THIN LAYER CHROMATOGRAPHY METHODS FOR SEPARATION AND IDENTIFICATION OF ANTIDEPRESSANTS IN THEIR MIXTURE

2014 ◽  
Vol 21 (1) ◽  
pp. 11-15
Author(s):  
Daiva Kazlauskienė ◽  
Guoda Kiliuvienė ◽  
Palma Nenortienė ◽  
Giedrė Kasparavičienė ◽  
Ieva Matukaitytė
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Solvent System ◽  
Ammonia Solution ◽  
Relative Standard ◽  
Rf Values ◽  
Solvent Systems ◽  
Paroxetine Hydrochloride ◽  
Fluvoxamine Maleate ◽  
Layer Chromatography

By conducting the toxicological analysis it is meaningful to determine the analytical system that could identify simultaneously several medicinal preparations quickly and precisely. The purpose of this work was to create and validate the method of thin-layer chromatography that would be suitable to separate the components of antidepressant mixture (amitriptyline hydrochloride, paroxetine hydrochloride, sertraline hydrochloride, fluvoxamine maleate and buspirone hydrochloride) and to identify them. The system was validated with regard to the sensitivity, repetition of data, resistance and particularity. The solvent systems with potential of high separation of components in their mixture were created: acetonitrile, methanol, ammonia solution 25 percent (85:10:5); acetonitrile, methanol, ammonia solution 25 percent (75:20:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (50:45:5); dichlormethane, 1,4-dioxane, ammonia solution 25 percent (42:55:3); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (25:70:5); trichlormethane, 1,4-dioxane, ammonia solution 25 percent (60:36:4). One of the most suitable solvent systems for separation of the analyzed mixture (sertraline, amitriptyline, paroxetine, buspirone, fluvoxamine) was determined – acetonitrile, methanol, ammonia solution 25 percent (85:10:5). When this solvent system was used, the average Rf values of the analyzed compounds differed the most. Validation was conducted – the relative standard deviation (RSD, percent) of the average Rf value of the analyzed compounds varied from 0,6 to 1,8 percent and did not exceed the permissible error of 5 percent. The sensitivity of methodology was determined by assessing the intensity of the mixture’s spots on the chromatographic plate. The detection limit of buspirone was 0,0012 µg; sertraline – 0,0008 µg; amitriptyline – 0,0004 µg; fluvoxamine – 0,0004 µg; paroxetine – 0,0008 µg. The resistance of results to the changed conditions – it was determined that when the amounts of the solvents acetonitrile and methanol were increased or decreased to two milliliters, the average Rf values of the analyzed compounds did not change statistically significantly

DEVELOPMENT OF HPTLC METHOD FOR THE ESTIMATION OF ONDANSETRON AND RANITIDINE IN COMBINED DOSAGE FORM

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (12) ◽  
pp. 42-48
Author(s):  
P. J. Patel ◽  
◽  
D. A Shah ◽  
F. A. Mehta ◽  
U. K. Chhalotiya
Keyword(s):  
Thin Layer ◽  
Stationary Phase ◽  
Thin Layer Chromatography ◽  
Silica Gel ◽  
High Performance ◽  
Dosage Form ◽  
Solvent System ◽  
Rf Values ◽  
Layer Chromatography ◽  
Hptlc Method

A simple, sensitive and precise high performance thin layer chromatographic (HPTLC)method has been developed for the estimation of ondansetron (OND) and ranitidine (RAN) in combination. The method was employed on thin layer chromatography (TLC) and aluminium plates were precoated with silica gel 60 F254 as the stationary phase, while the solvent system was methanol. The Rf values were observed to be 0.5 ± 0.02, and 0.3 ± 0.02 for OND and RAN, respectively. The separated spots were densitometrically analyzed in absorbance mode at 299 nm. This method was linear in the range of 25-300 ng/band for OND and 50-600 ng/band for RAN. The limits of detection for OND and RAN were found to be 3.47 and 1.83 ng/band, respectively. The limits of quantification for OND and RAN were found to be 10.53 and 5.55 ng/band, respectively. The proposed method was validated with respect to linearity, accuracy, precision and robustness. The method was successfully applied to the estimation of OND and RAN in combined dosage form.

EXPERIMENTAL PRODUCTION OF AFLATOXIN ON BRICK CHEESE1

1972 ◽  
Vol 35 (10) ◽  
pp. 585-587 ◽  
Author(s):  
C. N. Shih ◽  
E. H. Marth
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Aspergillus Flavus ◽  
Aspergillus Parasiticus ◽  
Solvent System ◽  
Experimental Production ◽  
Mold Growth ◽  
Layer Chromatography ◽  
Plastic Containers ◽  
Chloroform Methanol

Brick cheese was placed in plastic containers and all surfaces except the top were sealed with wax. The top was inoculated with Aspergillus flavus or Aspergillus parasiticus and cheese was incubated in a humid chamber at 7.2, 12.8, and 23.9 C for up to 14 weeks after mold growth was evident. After incubation each cheese was cut horizontally into four layers, each approximately 1 cm thick. Each layer of cheese was extracted with a monophasic-biphasic solvent system (chloroform, methanol, and water). The extract was purified, concentrated, and aflatoxins were measured by thin-layer chromatography and fluorometry. No aflatoxins were produced by either mold at 7.2 C. At 12.8 C, A. parastticus developed aflatoxins B1 and G1 after 1 week of incubation. Aflatoxin produced by this mold persisted through 4 weeks of storage and then was not detectable. Aspergillus flavus did not form aflatoxin at 12.8 C. Both molds produced aflatoxin on cheese at 23.9 C; A. parasiticus did so after 1 week and A. flavus after 14 weeks. In some instances, aflatoxin was found in cheese 4 cm from the surface. It is reasonable to assume that cheese will not become contaminated with aflatoxin if the food is held at or below 7 C.

Determination of Biphenyl in Citrus Fruits by Thin Layer Chromatography and Ultraviolet Spectrophotometry

1967 ◽  
Vol 50 (4) ◽  
pp. 934-938
Author(s):  
Paul E Corneliussen
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Uv Light ◽  
Preparative Thin Layer Chromatography ◽  
Mean Deviation ◽  
Citrus Fruits ◽  
Ultraviolet Spectrophotometry ◽  
Spectrophotometric Measurement ◽  
Layer Chromatography

Abstract A rapid method for determining biphenyl in citrus fruits has been developed and was studied collaboratively. Biphenyl is separated from fruit tissue by steam liquidliquid extraction. The ra-heptane extract is subjected to preparative thin layer chromatography (TLC) on plates coated with silica gel containing phosphors for ready visibility of the biphenyl spots under UV light. The spots are removed from the plate and extracted with alcohol for spectrophotometric measurement at 248 mμ. The TLC cleanup adds specificity to the method; o-phenylphenol, if present, does not interfere and crop blanks are insignificant. The average of 36 recoveries (12 each at abovit 100, 50, and 10 ppm) was 96.7% with a mean deviation of 10.7%. It is recommended that the method be adopted as official, first action.

Porpidia irrigua, a new species related to P. contraponenda

2014 ◽  
Vol 46 (3) ◽  
pp. 269-284 ◽  
Author(s):  
Alan ORANGE
Keyword(s):  
New Species ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Solvent System ◽  
Siliceous Rocks ◽  
Layer Chromatography ◽  
A New Species

AbstractPorpidia irrigua is described as a new species; it has a white thallus, sessile apothecia, contains the depside methyl 2'-O-methylmicrophyllinate, and grows on damp siliceous rocks. It was previously included in a wide concept of P. contraponenda, but that species differs in the thicker thallus, partly immersed apothecia, and the possession of an unidentified depside in addition to methyl 2′-O-methylmicrophyllinate, which can be separated by thin-layer chromatography using Solvent System G.

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