Use of Nonionic Tween-80 Surfactant Mobile Phase in Thin Layer Chromatography of Heavy Metal Cations

Author(s):  
Sarang Dhote ◽  
Lata Deshmukh ◽  
L. Paliwal

The possibility of separation of oleic and stearic acids with mobile phases on the basis of surfactants was estimated by the method of a thin-layer chromatography. The influence of surfactant's type and concentration on the retention parameters of the studied acids when using of normal-phase plates for a thin-layer chromatography of Sorbfil UV-254 is investigated in the work. The influence on mobility of oleic and stearic acids of the anionic sodium n-dodecylsulphate, cationic cetylpyridinium chloride and non-ionic Tween-80 in the range of concentration from 1·10-5 mol/l to 0.1 mol/l is estimated. The mixed mobile phases on the basis of two last surfactants taken in various concentrations are also investigated. The рН of eluents was varied in the range from 1 to 9. The addition of 2-propanol into the mobile phase containing surfactant didn't lead to improvement of acids' distribution efficiency. The best results have been received with the eluent, containing 1·10-5 mol/l of cetylpyridinium chloride and boric buffer solution with pH 9. Preliminary modification of silica gel surface with cetylpyridinium chloride did not change the results of chromatography. For clarification of relation of acids' retention with a length of a hydrophobic fragment, and, therefore, a contribution of hydrophobic interactions, in system with the mixed mobile phase on the basis of cetylpyridinium chloride and Tween-80 at pH 3 formic acid, acetic acid, propionic acid, hexanoic acid and myristic acid were analyzed. The smallest mobility was observed for myristic acid (lgPo/w=6.09±0.19) that indicates very strong hydrophobic interactions of acid with the surface of silica gel modified by surfactants. Such interactions are the main reason of bad mobility of studied oleic (lgPo/w=7.7±0.2) and stearic (lgPo/w=8.22±0.19) acids in system with the surfactant-containing eluents. For the manifestation of acidic zones after chromatography, a solution of phosphomolybdic acid, a solution of rhodamine B, a solution of sulfuric acid and an iodine chamber were tested. The best visualization of TLC-сhromatogram is obtained after sprinkle the plates by 6% solution of sulfuric acid in ethanol with their subsequent heating at 110 °C.


2021 ◽  
Vol 5 (1) ◽  
pp. 013-018
Author(s):  
Verushkin Aleksey G ◽  
Kulikov Artem Yu ◽  
Kutsanyan Andranik A

A micellar thin-layer chromatography method for the quantitative determination and validation of coumarin in Meliloti herba and its ethanolic extracts was developed and validated. For achieving good determination, the mobile phase of 5 x 10-4 mol/L Tween-80 in a mixture propanol-2 – water (5:95 v/v) was used. Densitometric determination was carried out at 275 nm. The calibration curve was linear in the range of 0.1-2.5 μg per band. The proposed method is simple, rapid, precise and accurate; replacing hazardous solvents by greener ones correspond to the modern requirements in “Green chemistry” concepts. The obtained data can be used for the routine analysis of coumarin in medical plant and extracts.


Talanta ◽  
1992 ◽  
Vol 39 (8) ◽  
pp. 953-958 ◽  
Author(s):  
I POLITZER ◽  
K CRAGO ◽  
K AMOS ◽  
K MITCHELL ◽  
T HOLLIN

2018 ◽  
Vol 1 (1) ◽  
pp. 264-270
Author(s):  
Hady Wiraputra ◽  
Marline Nainggolan ◽  
Panal Sitorus

Tanaman buni (Antidesma bunius (L.) Spreng.) secara tradisional telah digunakan untuk hipertensi, takikardia, anemia, sifilis, antikanker, antioksidan, sumber pewarna alami dan antidiabetes. Saponin merupakan senyawa fitokimia yang mempunyai kemampuan membentuk busa dan mengandung aglikon polisiklik yang berikatan dengan satu atau lebih gula. Penelitian ini bertujuan untuk melakukan karakterisasi senyawa saponin hasil isolasi dari daun buni dengan spektrofotometer ultraviolet dan inframerah. Simplisia daun buni dilakukan karakterisasi kemudian diekstraksi dengan cara maserasi bertingkat menggunakan pelarut n-heksana dan etanol 80%. Selanjutnya ekstrak etanol dihidrolisis dengan HCl 2N kemudian difraksi dengan pelarut kloroform. Isolasi dilakukan terhadap fraksi kloroform dengan cara kromatografi lapis tipis preparatif menggunakan fase diam silika gel GF254 dan fase gerak yang sesuai. Isolat yang diperoleh diuji kemurnian dengan KLT 2 arah dan dikarakterisasi menggunakan spektrofotometer ultraviolet dan inframerah. Hasil pemeriksaan karakterisasi simplisia diperoleh kadar air 7,32%, kadar sari larut dalam etanol 52,70%, kadar sari larut dalam air 23,25%, kadar abu total 6,86% dan kadar abu tidak larut dalam asam 0,94%. Pemisahan fraksi kloroform dengan KLT menggunakan fase gerak n-heksana-etilasetat perbandingan 5:5 diperoleh noda 13 dan hasil KLT preparatif diperoleh 2 isolat murni yaitu isolat 1 (ungu merah) dengan Rf 0,92 dan isolat 2 (biru) dengan Rf 0,78. Hasil karakterisasi isolat 1 diperoleh panjang gelombang maksimum pada 208 nm dan dijumpai adanya gugus hidroksil, gugus -CH alifatis, ikatan C=C, gugus –CH2, gugus –CH3, dan gugus C-O. Hasil karakterisasi isolat 2 diperoleh panjang gelombang maksimum pada 204 nm dan adanya gugus hidroksil, gugus -CH alifatis, gugus –CH2, gugus –CH3, dan gugus C-O. Buni (Antidesmabunius (L.) Spreng.) has been traditionally used for the treatment of hypertension, tachycardia, anemia, syphilis, and used asanti-cancer, anti-oxidant, natural dye, and anti-diabetic. Saponin is a phytochemical compound which has capability in forming foam and contains polycyclic aglycone that binds with one or more glucose. This research aimed to conduct the characterization of saponin compound from buni leaves with ultraviolet spectrophotometer and infrared. Buni leaves simplicia was characterizedand extracted using sequential maceration method with n-hexane and 80% ethanol. The ethanol extract was hydrolyzed with HCl 2N and fractionized using chloroform solvent. Isolation of chloroform fraction was done using preparative thin-layer chromatography using silent phase of silica gel GF 254 and suitable mobile phase. Isolates obtained was taken into purity test with two dimensions thin-layer chromatography and characterized using ultraviolet spectrophotometer and infrared. The characterized simplicia resulted with 7.32% of water content, 52.70% of dissolved content in ethanol, 23.25% of dissolvedcontent in water, 6.86% of total ash content, and 0.94% of undissolved ash content in acid. Fractinationof chloroform fraction with thin-layer chromatography using mobile phase ofn-hexane-ethyl acetate with 5:5 ration resulted with 13 spotsand the result of the preparative thin-layer chromatography resulted 2 pure isolates which are isolate 1 (purple-red) with Rf 0.92 and isolate 2 (blue) with Rf 0.78. The characterization of isolate 1 resulted that the maximum wave lengthwas 208 nm with hydroxyl group, –CH aliphatic group, C=C bond, –CH2 group, –CH3 group, and C–O group. The characterization of isolate 2 resulted that the maximum wave lengthwas204 nm with hydroxyl group, –CH aliphatic group, –CH2 group, –CH3 group, and C–O group.


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