Cumulative CAMAG Bibliography Service CCBS
Our CCBS database includes more than 11,000 abstracts of publications. Perform your own detailed search of TLC/HPTLC literature and find relevant information.
The Cumulative CAMAG Bibliography Service CCBS contains all abstracts of CBS issues beginning with CBS 51. The database is updated after the publication of every other CBS edition. Currently the Cumulative CAMAG Bibliography Service includes more than 11'000 abstracts of publications between 1983 and today. With the online version you can perform your own detailed TLC/HPTLC literature search:
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Chem. Asian J. 15(19), 3044-3049 (2020). The studied rotaxane combines a dibenzocrown of 8 ethers (DB24C8) with an axle chain (Ax) containing two amines, one of them in an aniline group, allowing stability of the rotaxane even when the other one is unprotonated. TLC on silica gel in 4 steps, with detection under UV light or after derivatization with phosphomolybdic acid in ethanol. (1) Before the synthesis of the rotaxane, unprotonated Ax was isolated by preparative TLC of the protonated Ax obtained by addition of HCl or toluenesulfonic acid (TsOH); the mobile phases were chloroform – methanol 10:1 and toluene – tetrahydrofurane 3:2, respectively. The isolated molecules were confirmed as totally unprotonated Ax by NMR, suggesting a complete loss of HCl and TsOH on the silica gel layer. (2) After synthesis, unprotonated rotaxane, pure vs. monoprotonated by the addition of 10 different acids (and purified by column chromatography CC), was applied on TLC plates and developed with dichloromethane – acetone – water 3:16:1; the hRF values were very different, depending on the counter-anions from the used acids. (3) The same behavior (except with sulfuric acid) was observed under the same conditions when CC was omitted (unprotonated rotaxane samples were mixed with each of the acids, or with two acids at the same time for acid-competitive TLC analysis). (4) When unprotonated rotaxane was applied under the same conditions as in step (3) with the sodium salts instead of the acids, the behavior was similar (except for the shapes of the spots, due to the salts in excess). The rotaxane can thus be used for the TLC separation and detection of sodium salts, by forming salts of protonated rotaxane with the anion afforded by these sodium salts. The rotaxane protonation seems to be promoted by the methanol of the spotting mixture; indeed, when step (3) was performed with the mobile phase chloroform – methanol 10:1, a second zone appeared because methanol formed a salt with the rotaxane (identified by NMR).
Planta Med. 84(18), 1348-1354 (2018). A subfraction (obtained through liquid-liquid partition and column chromatography) of the ethanolic extract of whole Vernonia cinerea plants (Asteraceae, subf. Cichorioideae) was further fractioned by reverse-phase SPE (solid-phase extraction) followed by preparative TLC on silica gel layer (eluent not given). For verification, zones were detected by spraying with anisaldehyde solution with 10 % sulfuric acid, followed by heating at 100 °C. Further purification by reverse-phase HPLC allowed the isolation of 6 hirsutinolide-type sesquiterpenoids (all with a oxacyclonane forming an ether bridge), including vernolides A and B.
Planta Med. 84(18), 1340-1347 (2018). Preparative TLC on silica gel for the final purification of 15 phenylethyl-chromenone derivatives (including 3 with epoxide functions), 4 sesquiterpenoids (neopetasane, dehydrokaranone, dioxoselinene, ligudicin C) and a steroid (ergostatetraenone), all isolated through multi-step column chromatography from the ethyl-acetate fraction of a methanolic extract of Aquilaria sinensis resinous wood (Thymelaeaceae). For each compound, mobile phase, RF value and yield are given.
Planta Medica 84(11), 813-819 (2018). Fluorinated analogues of epigallocatechin-gallate were purified after synthesis by extraction with ethyl acetate from the synthesis mixtures, followed by column chromatography or (for two pairs of isomers) by preparative TLC. This isolation (as well as monitoring of column elution for the other compounds) was performed by TLC on silica gel with mixtures of n-hexane and (less) ethyl acetate in several concentrations, allowing the separation of diastereoisomers (RF values and yields are given). No derivatisation, visualisation because of fluorescing agent in the layers. Structures were identified by NMR and HR-MS, but apart from the TLC.
Planta Medica 84(9/10), 729-735 (2018). The chloroform fraction of a methanolic extract of Euphorbia taurinensis whole plant (Euphorbiaceae) was submitted to a multi-step fractionation through column chromatography. Monitoring by TLC on silica gel (mobile phases see below) followed by derivatization with concentrated sulfuric acid and heating at 105°C. The fractions obtained were purified by repeated cycles of preparative TLC alone or alternating with preparative HPLC, leading to the isolation of segetane, ingenane, and jatrophane diterpenes. Depending on the subfractions, preparative TLC silica gel and reverse-phase C18 layers were used, with cyclohexane – ethyl acetate – ethanol 25:15:1 for normal phase, and with mixtures of acetonitrile (or methanol) and water for RP.
Planta Medica 84(2), 129-134 (2018). TLC of subfractions obtained from normal-phase LC and size-exclusion chromatography of an ethanolic extract of Bougainvillea spectabilis (Nyctaginaceae) stem-bark on RP-18 with methanol – water 2:3 and 1:1 to isolate six flavones (bougainvinones J, K, L, M, and two dimethylflavone derivatives).
Planta Medica 84(1), 26-33 (2018). For the monitoring of the multi-step fractionation through VLC (vacuum liquid chromatography) of the chloroform-soluble parts of a methanol – water 7:3 percolate of Hippophae rhamnoides (Eleagnaceae) fruit peels, TLC on silica gel and RP-18, detection by spraying with sulfuric acid and heating. Preparative TLC on silica gel with cyclohexane – dichloromethane – methanol 5:15:1 to isolate, from VLC subfractions, three lignans (nectandrin B, fragransin A2, saucernetindiol) that are diastereoisomers of each other.
Planta Medica 83(17), 1329-1334 (2017). Two acetone-soluble subfractions of an n-hexane maceration of Hypericum denudatum aerial parts (Hypericaceae) were submitted to repeated centrifugal planar chromatography (CPC) on silica gel using n-hexane – ethyl acetate (gradient from 100:0 to 90:10), obtaining four dimeric acylphloroglucinols (denudatin A, hyperbrasilol A, uliginosin B and isouliginosin B), which were purified by crystallisation with n-hexane – dichloromethane 9:1. From the most apolar CPC eluates, a monomer (selancin A) was isolated on preparative TLC silica gel layer by elution with n-hexane – ethyl acetate 97:3. Furthermore, all the purification steps were monitored through TLC on silica gel with n-hexane – ethyl acetate 19:1 or with n-hexane – dichloromethane 1:1. Detection under UV light after derivatization with anisaldehyde – sulfuric acid, monomeric acylphloroglucinols appeared purple, whereas dimers appeared yellow-orange.