scholarly journals Some Observations on Thin Layer Chromatography Technique

2019 ◽  
Vol 8 (2) ◽  
pp. 1700-1702

The present study is to report the various problems faced during TLC methodology. Although used regularly some technical aspects must be kept in mind to get better and uniform results. During our experiments with TLC methods we came across some problems and here these aspects of TLC methodology are being highlighted. It is suggested that the solvent use as mobile phase should also be used for extraction of any particular phytochemical. TLC plates should be 3 to 4 mm thick, to be dried for at least 72 hrs. It is also suggested that potassium permanganate solution gives better clarity in visualizing the spots

2010 ◽  
Vol 93 (3) ◽  
pp. 778-782 ◽  
Author(s):  
Tatána Gondová ◽  
Iveta Petríková

Abstract A new and simple TLC-densitometry method has been developed for the simultaneous separation of the two noradrenergic and specific serotonergic antidepressants mirtazapine and mianserine and validated for their determination in commercially available tablets. The method used TLC plates precoated with silica gel 60F254 as the stationary phase, and the mobile phase consisted of hexaneisopropanol25 ammonia (70 + 25 + 5, v/v/v). Densitometric analysis was carried out in the absorbance mode at 280 nm. The method was validated in accordance with International Conference on Harmonization guidelines in terms of linearity, LOD, LOQ, precision, and accuracy. Calibration curves were linear (R2 > 0.9970) with respect to peak area in the concentration range of 5002500 and 5005000 ng/spot for mirtazapine and mianserine, respectively. The LODs were 20 and 35 ng/spot for mirtazapine and mianserine, respectively. The described method was successfully applied to the determination of mirtazapine and mianserine in their pharmaceutical formulations with recovery ranging from 99.83 to 101.20 of the labeled amount of the compounds. The proposed method can be used in routine QC of these drugs in pharmaceutical formulations.


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.


1966 ◽  
Vol 49 (4) ◽  
pp. 795-800
Author(s):  
William A Moats

Abstract Butterfat and milk samples were analyzed for chlorinated insecticides by thin layer chromatography (TLC) on aluminum oxide or silica gel plates containing a small amount of silver nitrate. The adsorbent was washed with distilled water before preparing the plates. A one-step cleanup on a partially inactivated Florisil column was performed prior to TLC analysis. For color development, the TLC plates were sprayed lightly with hydrogen peroxide to suppress possible interference from fat and then steamed before exposure to ultraviolet light to accelerate and intensify the color reaction. Rf values for a number of solvent systems on aluminum oxide and silica gel plates are given. With this procedure, 0.05 μg or less of insecticide can be detected in a 0.4 g butterfat sample or the extract from 10 ml milk.


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