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.

DDT-Type Compounds: Separation and Identification by a System Combining Thin Layer Chromatography, Gas Chromatography, and Infrared Spectroscopy

1968 ◽  
Vol 51 (6) ◽  
pp. 1247-1260
Author(s):  
M B Abou-Donia ◽  
D B Menzel
Keyword(s):  
Gas Chromatography ◽  
Infrared Spectroscopy ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Electron Capture ◽  
Structural Changes ◽  
Effective Technique ◽  
Rf Values ◽  
Solvent Systems ◽  
Layer Chromatography

Abstract Infrared spectroscopy, in combination with TLC and GLC, offers an effective technique for isolation, separation, and identification of DDT-type compounds. Rf values for DDT and 13 other compounds, most of which have been reported as DDT breakdown products, have been determined in 27 solvent systems, using TLC techniques. Three columns, in combination with the electron capture detector, have been experimentally studied to analyze the 13 DDT-like compounds. The positions and intensities of the infrared bands of the 14 compounds have been measured in KBr. The variations of these measurements have been discussed in relation to the structural changes of DDT-type compounds.

Thin Layer Chromatography of Some Carbamate and Phenylurea Pesticides

1967 ◽  
Vol 50 (4) ◽  
pp. 888-896
Author(s):  
Josephine M Finocchiaro ◽  
Walter R Benson
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Tertiary Amines ◽  
Carbamate Pesticides ◽  
Cleanup Procedure ◽  
Rf Values ◽  
Solvent Systems ◽  
Layer Chromatography

Abstract Nineteen carbamate pesticides and three structurally related phenylureas were examined on thin layer chromatographic plates. These compounds have been divided into 4 groups, based on their Rf values and their responses to chromogenic agents: 8 aryl N-methylcarbamates; 2 aryl N-methylcarbamates containing tertiary amines; compounds containing chlorine, i.e., 4 carbamates and 3 phenylureas; and 5 other carbamates. Two adsorbents, two solvent systems, and four chromogenic sprays were used to separate and distinguish these compounds. Some compounds qualitatively came through a cleanup procedure previously reported for carbaryl.

Thin-Layer Chromatography for Insecticide Analysis

1963 ◽  
Vol 46 (2) ◽  
pp. 250-261
Author(s):  
Kenneth C Walker ◽  
Morton Beroza
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Simple Procedure ◽  
Rf Values ◽  
Solvent Systems ◽  
Layer Chromatography

Abstract A single, simple procedure has been worked out for the analysis of 62 pesticides by thin-layer chromatography. Rf values in 19 different solvent systems and chromogenic reagents for making the pesticides visible are presented, together with Rf values of dyes that may be used as standards.

Simplified Qualitative Analysis of Glycerides Derived from Coconut Oil Using Thin Layer Chromatography

2012 ◽  
Vol 506 ◽  
pp. 182-185 ◽  
Author(s):  
Sirikarn Pengon ◽  
Chutima Limmatvapirat ◽  
Sontaya Limmatvapirat
Keyword(s):  
Acetic Acid ◽  
Qualitative Analysis ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Cocos Nucifera ◽  
Coconut Oil ◽  
Solvent System ◽  
Tlc Plates ◽  
Solvent Systems ◽  
Layer Chromatography

Coconut (Cocos nucifera L.) oil is composed predominately of medium-chain triglycerides which have been reported to be beneficial to human health. It also contains free fatty acids (FFAs) which can combine with glycerol to form monoglycerides, diglycerides, and triglycerides. The analysis of FFAs and their glycerides has been proposed to assess the quality of coconut oil used as raw materials in various industrial fields. The aim of this study was to develop the qualitative method for investigation of FFA and their glycerides in coconut oil using thin layer chromatography (TLC). Coconut oil and standards of FFA and their glycerides were chromatographed separately on Silica gel 60 F254 TLC plates using hexane: ether: acetic acid (60:40:1) and hexane: ethyl acetate: acetic acid (60:40:0.5) as solvent systems A and B, respectively. The spots on developing TLC plates were detected and compared using 254-nm UV light and iodine vapor. The results showed that the resolution of solvent system A was better than that of solvent system B. However, both solvent systems were used to confirm the results. The retention factor (Rf) values of the components were in good agreement with their polarity. This method should provide a guideline for qualitative analysis of coconut oil.

Reverse Phase Thin Layer Chromatography of Some Aroclors, Halowaxes, and Pesticides

1973 ◽  
Vol 56 (2) ◽  
pp. 367-372
Author(s):  
David L Stalling ◽  
James N Huckins
Keyword(s):  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Mobile Phase ◽  
Gas Liquid Chromatography ◽  
Chlorinated Pesticides ◽  
Reverse Phase ◽  
Mobile Phases ◽  
Rf Values ◽  
Solvent Systems ◽  
Layer Chromatography

Abstract The components of Aroclors® 1232, 1248, 1254, and 1260; Halowaxes® 1099, 1013, and 1014; and several chlorinated pesticides are resolved by reverse phase thin layer chromatography (RPTLC), which permits component separation by partition between a nonpolar stationary phase and a polar mobile phase. Rf values of resulting spots were calculated for 2 of 4 new solvent systems (mobile phases). RPTLC patterns were reproducible and characteristic of each material examined. The spots were recovered from the plates and characterized by gas-liquid chromatography (GLC) and/or GLC-mass spectrometry. In some cases, single GLC peaks of Aroclor standards were resolved into more than one component by RPTLC, whereas some RPTLC spots of Halowaxes were resolved into as many as 4 GLC peaks. The analysis of environmental residues of chlorinated compounds was facilitated by this technique.

Aflatoxins: Improved Resolution by Thin Layer Chromatography

1969 ◽  
Vol 52 (4) ◽  
pp. 669-672 ◽  
Author(s):  
R D Stubblefield ◽  
G M Shannon ◽  
O L Shotwell
Keyword(s):  
Quantitative Analysis ◽  
Relative Humidity ◽  
Qualitative Analysis ◽  
Thin Layer ◽  
Thin Layer Chromatography ◽  
Water Concentration ◽  
Solvent System ◽  
Solvent Systems ◽  
Layer Chromatography ◽  
System Water

Abstract Water was added to solvent systems for TLC of aflatoxins to achieve more reproducible results in laboratories where temperature and relative humidity vary. Resolution of the toxins also improved. Increments of water were added to solvent systems composed of acetone-chloroform (10 + 90, 12 + 88, and 15 + 85, v/v). As the water concentration was increased, separation of aflatoxins B2 and G1 improved. These two toxins are usually the most difficult to resolve in these solvent systems. Separations were the best with wateracetone-chloroform (1.5 + 12 + 88, v/v/v). Water added to methanol-chloroform (3 + 97, v/v) improved resolution of this solvent system but not enough for quantitative analysis, or at times, qualitative analysis. The solvent system water-methanol-ether (1 + 3 + 96, v/v/v) separated aflatoxins as well as water-acetone-chloroform (1.5 + 12 + 88, v/v/v).

Sign in / Sign up

Export Citation Format

Share Document