Simple, Sensitive Technique for Detection and Separation of Halogenated Synthetic Pyrethroids by Thin Layer Chromatography

1983 ◽  
Vol 66 (4) ◽  
pp. 1009-1012
Author(s):  
Radhakrishnan Sundararajan ◽  
Ram Parkash Chawla

Abstract Thin layer chromatography employing silver nitrate-impregnated alumina G plates has been extended for the routine detection and confirmation of the identity of halogenated synthetic pyrethroid insecticides. Of the solvent systems tried, maximum resolution was achieved by using n-hexane-benzene (45+ 55) and n-hexane-chloroform (60 + 40), which gave distinct separations of the cis- and trans-isomers of permethrin and cypermethrin from fenvalerate and decamethrin. Possible interference of HCH isomers and DDT and its analogs can also be checked by a concurrent run of the sample mixture in these 2 systems. A minimum of 50 ng each of cis- and trans-permethrin and cypermethrin isomers and fenvalerate and decamethrin can be positively detected. Using this technique, the minimum detectable limit of permethrin was 0.1 ppm in the cleaned up extracts of tomato plant and fruit and soil samples.

2014 ◽  
Vol 21 (1) ◽  
pp. 11-15
Author(s):  
Daiva Kazlauskienė ◽  
Guoda Kiliuvienė ◽  
Palma Nenortienė ◽  
Giedrė Kasparavičienė ◽  
Ieva Matukaitytė

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


1968 ◽  
Vol 51 (6) ◽  
pp. 1247-1260
Author(s):  
M B Abou-Donia ◽  
D B Menzel

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.


1965 ◽  
Vol 48 (4) ◽  
pp. 838-843 ◽  
Author(s):  
Rachel S Silk

Abstract Thin-layer chromatographic procedures have been developed by which most of the colors present in current commercial lipsticks can be separated. Most lipstick colors are separated on one plate with two solvent systems, but the presence of D&C Red No. 7 requires a slightly altered procedure. A plate with a buffered zone is added and an additional development step is used. The color recovery was determined by the analyses of 16 lipsticks from four manufacturers.


1972 ◽  
Vol 55 (6) ◽  
pp. 1345-1353
Author(s):  
Marshall T Jeffus ◽  
Charles T Kenner

Abstract A method for the determination of diethylstibestrol in feeds, which is based on official first action method 38.048–38.051, is proposed. Interfering feed extractives are removed by using a tripotassium phosphate-Celite column prior to measurement at 415 nm before and after irradiation. Recoveries of equilibrated standards added to Soxhlet extracts of several samples averaged 94.3% compared to 86.3% by the official method. The background absorbance at 415 nm obtained by using the proposed method was approximately 6% of the background by the official method for solutions containing equivalent amounts of sample. A thin layer chromatographic method is also included for the confirmation and identification of the cis and trans isomers of the drug. The proposed method has been found satisfactory for the quantitative determination of 0.55–44 ppm diethylstilbestrol and the thin layer chromatographic procedure can detect as little as 0.07 ppm.


1968 ◽  
Vol 42 (12) ◽  
pp. 735-739
Author(s):  
Hiromu TANAKA ◽  
Kiyoshi YOSHIKAWA ◽  
Hiromu SHIMOMURA

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