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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      130 143
      Estimation of withaferin-A by HPLC and standardization of the Ashwagandhadi lehyam formulation
      A. K. MEENA*, P. REKHA, A. PERUMAL, M. GOKUL, K.N. SWATHI, R. ILAVARASAN (*Captain Srinivasa Murthy Regional Ayurveda Drug Development Institute, Central Council for Research in Ayurvedic Sciences, Arumbakkam, Chennai, India; ajaysheera@gmail.com)

      Heliyon 7(2), e06116 (2021). Samples were a methanolic extract of a semi-solid ayurvedic conserve (ashwagandhadi lehyam) prepared with Withania somnifera roots (Solanaceae) and five other plants, as well as standards: withaferin A and withanolide A (= withaniol), two ergostane triterpene steroids with lactone cycle and epoxide. HPTLC on silica gel with toluene – ethyl acetate – formic acid 6:4:1. Visualization and densitometric scanning at UV 254 nm and 366 nm (deuterium lamps). Derivatization by immersion into vanillin – sulfuric acid reagent, followed by oven heating at 105 °C until optimal coloration. Documentation under white light and densitometry scanning at 540 nm (tungsten lamp). Both analytes (hRF 35 and 45 respectively) were shown at 254 nm and 540 nm (but not at 366 nm), in the standards and in the extract.

      Classification: 8b, 9, 13c, 15a, 32e
      130 147
      Globotriaosylceramide-related biomarkers of Fabry disease identified in plasma by high-performance thin-layer chromatography – densitometry – mass spectrometry
      C. JARNE, L. MEMBRADO, M. SAVIRÓN, J. VELA, J. ORDUNA, R. GARRIGA, J. GALBÁN, V. L. CEBOLLA* (*Institute of Carbon Chemistry, Spanish National Research Council (CSIC), Saragossa, Spain; vcebolla@icb.csic.es)

      J Chromatogr A 1638, 461895 (2021). Samples were sphingolipid-rich fractions of unproteinated blood plasma from healthy humans or from Fabry’s disease patients, as well as standards of sphingomyelin (SM) and of globotriaosylceramides (Gb3 = ceramide trihexosides), and related compounds (lyso-ceramide trihexosides, lactosyl ceramide, glucosyl ceramide). HPTLC on silica gel (Lichrosphere with spherical particles) by automated multiple development with a 9-step gradient, starting with pure methanol and ending with dichloromethane – methanol 9:1. Visualization and densitometry under UV 190 nm. Derivatization for Gb3 and derivatives (but not for SM) by immersion into orcinol solution (0.2 %, with sulfuric acid 10 %), followed by 15 min heating at 100 °C and by densitometry under visible light 550 nm. Bands of interest were directly eluted with methanol from underivatized plates into an ion-trap MS, through the oval head of a TLC-MS interface (with stainless steel frit to remove silica gel particles). Two different ionization processes were used: (A) electrospray ionization (ESI, capillary voltage 4 kV, endplate offset voltage -0.5 kV, nebulizer pressure 40 psi, drying gas 9 mL/min at 350 °C); (B) atmospheric pressure chemical ionization (APCI, capillary voltage 2–3 kV, current intensity 4.5 µA, nebulizer pressure 45 psi, drying gas 5 mL/min at 350 °C; vaporization at 450 °C). Full MS spectra were recorded up to m/z 1500 in positive ion mode. The relative ion intensities were used to quantify the detected species. Previous to this study, the precision of the elution head positioning was tested on Gb3 standard zones, comparing 3 positions for analyte elution: from the centre and from each higher or lower side of the band. The same main m/z peaks were observed in the 3 positions, but in different proportions. This was explained by the presence of coeluting Gb3 subclasses (the ceramide moiety CM being either saturated, mono-unsaturated fatty acyl with a slightly higher migration distance, or polar hydroxyl fatty acyl with the opposite effect on migration) and of coeluting Gb3 isoforms (the hexoside moiety consisting of glucose and/or galactose units). This resulted in the broadening and partial splitting of the standard band. In the plasma samples, 19 molecular species of Gb3 were identified (depending on the CM, the sugar isoforms being undistinguishable by MS): 5 with a saturated CM, 7 with two additional double bonds on the CM, 7 with a methylated CM. In case of Fabry’s disease, most Gb3 species with saturated CM were highly increased, whereas other species were decreased.

      Classification: 4e, 11c, 11e, 32f
      130 146
      Development of a thin-layer chromatography bioautographic assay for neuraminidase inhibitors hyphenated with electrostatic field induced spray ionisation-mass spectrometry for identification of active Isatis indigotica root compounds
      Y. ZANG (Zang Yichao), Y. MIAO (Miao Yu), T. WU (Wu Tao)*, Z. CHENG (Cheng Zhihong)** (*Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai, China, laurawu2000@163.com; **Department of Natural Medicine, School of Pharmacy, Fudan University, Shanghai, China, chengzhh@fudan.edu.cn)

      J Chromatogr A 1638, 461597 (2021). Samples were Isatis tinctoria (= I. indigotica) root extracts (Brassicaceae) and their fractions. Standards were oseltamivir acid (OA), a neuraminidase (NA) inhibitor; pinoresinol (PR, a lignan), β-sitosterol (SS, a sterol), and dihydro-neoascorbigen (DHNA, an alkaloid). HPTLC / TLC on silica gel with (1) petroleum ether – ethyl acetate – acetic acid 48:8:1 for petroleum ether extracts and SS, or 30:40:1 for ethyl acetate extracts, or 10:30:1 for PR; (2) with toluene – ethyl acetate – methanol – formic acid 16:3:1:2 or 10:4:1:2 also for ethyl acetate extracts and DHNA; (3) with n-butanol – acetic acid – water 25:4:3 for butanol extracts. OA was applied but not developed. RP-18, polyamide, cellulose, alumina layers were tested, but the resolution was lower. Derivatization by spraying with sulfuric acid (10 % in ethanol). Enzymatic assay by immersion of the plates into neuraminidase solution (6 U/mL), followed by 1 h incubation at 37 °C and by immersion into chromogenic substrate solution (1.75 mM 5-bromo-4-chloro-3-indolyl-α-D-N-acetylneuraminic acid). After 5 min, NA inhibitors were seen as white zones on blue background. The experiment was previously improved for the following parameters: incubation times, substrate and enzyme concentrations, followed by statistical evaluation and calculations using Box-Behnken design. Quantification by absorbance measurement (detection wavelength 605 nm, reference wavelength 420 nm). In optimal conditions, OA had LOD 300 ng/zone. Zones of interest on underivatized plates were directly submitted to MS, using EFISI (electrostatic-field-induced spray ionisation), as follows. Chromatograms were immersed 1–3 s into dimethicone – n-hexane 1:1 to form a hydrophobic film, and dried 30 min at room temperature; on the analyte spot, a hydrophilic droplet was formed with 5 µL methanol – water 1:1, extracting the analyte from the layer; the analyte was further attracted through a capillary tube (3–4 cm long, made of non-deactivated fused silica) under a strong electrostatic field, into the in-let orifice of the triple-quadrupole ­– linear ion-trap MS (induction voltage 4 kV; capillary voltage 40 V; tube lens voltage 100 V; capillary temperature 200 °C). Full-scan spectra were recorded in m/z range 50 – 1000, helium was used for collision-induced dissociation. 11 active compounds were identified in the extract: SS, 6 alkaloids (including cycloanthranilylproline, DHNA, hydroxy-indirubin, isatindigodiphindoside, isatindinoline A and), 3 lignans (including PR and isolariciresinol), 1 fatty acid (trihydroxy-octadecenoic acid).

      Classification: 4e, 8a, 8b, 11a, 13c, 22
      130 149
      HPTLC/HPLC-mass spectrometry identification and NMR characterization of major flavonoids of wild lemongrass (Cymbopogon giganteus) collected in Burkina Faso
      R.K. BATIONO*, C.M. DABIRÉ, A. HEMA, R.H.CH. NÉBIÉ, E. PALÉ, M. NACRO (*Laboratory of Applied Organic Chemistry and Physics, Joseph Ki-Zerbo University, Ouagadougou, Burkina Faso; kindanloun@gmail.com)

      Heliyon 8(8), e10103 (2022). Samples were a methanolic extract of Cymbopogon giganteus leaves (= C. caesius subsp. giganteus, Poaceae), as well as flavones as standards: isorhamnetin, luteolin and orientin (=luteolin 8-C-glucoside). HPTLC on silica gel with ethyl acetate – acetic acid – formic acid – water 100:11:11:26. Derivatization for flavones with Neu’s reagent (ethanolamine diphenylborate – PEG). Visualization under UV 365 nm. The standards (hRF 75, 70-72 and 96, respectively) were not detected in the extract. Some analytes detected by the reagent were scraped from the underivatized plate into a tube, and injected through a TLC-MS interface into a double-quadrupole – time-of-flight MS (electrospray ionization). Full mass scan spectra were recorded in positive and negative ionization modes in m/z range 150–550. For 3 of the compounds, isolated through MPLC columns, the HPTLC-MS results, combined to the NMR and HPLC-MS analyses, allowed the identification as epicatechin (hRF 86, a flavanol, not coloured by Neu’s reagent) and as luteolin 8-C- and 6-C-glucosides (hRF 67-70).

      Classification: 4e, 8a, 32e
      130 036
      Propolis from Nariño: Physicochemical properties and biological activity of Propolis
      G. SALAMANCA*, M. OSORIO, J. CABRERA (* Department of Chemistry, University of Tolima, Ibague, Colombia, gsalaman@ut.edu.co)

      Biotecnologia en el Sector Agropecuario y Agroindustrial. 20, 152-154 (2022). HPTLC of propolis on silica gel with toluene - ethyl acetate - formic acid 30:12:5. Detection under UV light at 254 and 366 nm. The method allowed the identification of apigenin, naringenin, quercetin, caffeic acid, galangin, feruloyl and derivatives of coumaric acid.

      Classification: 8a
      130 038
      Molecular and morphological diversity, qualitative chemical profile and antioxidant activity of filamentous fungi of the digestive tract of Phylloicus sp. (Trichoptera: Calamoceratidae)
      T. ROMAO*, A. FILHO, R. HARAVAKA, C. CASTRO, P. MORAIS (* Goiano Federal Institute, Departament of Agrochemistry, Rio Verde, GO, Brasil, tiago.romao@ifgoiano.edu.br)

      Braz. J. Biol. 45, e13764 (2021). HPTLC of filamentous fungi (Endomelanconiopsis endophytica, Myxospora musae, Neopestalotiopsis cubana and Fusarium pseudocircinatum) isolated from the digestive tract of Phylloicus sp, on silica gel with acetone - chloroform 5:3 and acetone - petroleum ether 5:2. Detection with iodine vapor, ferric chloride solution, sulfuric vanillin solution, green bromocresol solution and chromic acid solution. Qualitative identification under UV light at 254 and 366 nm. 

      Classification: 8b
      130 040
      Partial characterization of novel inulin-like prebiotic fructooligosaccharides of Sechium edule (Jacq.) Sw. (Cucurbitaceae) tuberous roots
      B. BANDYOPADHYAY, V. MANDAL, N. MANDAL* (*Plant and Microbial Physiology and Biochemistry Laboratory, Department of Botany, University of Gour Banga, Malda –732 103, WB, India, mandalvivek@gmail.com)

      J. Food. Biochem. 45, e13764 (2021). HPTLC of L-arabinose, D-fructose, D-fucose, D-galactose, D-glucose, D-mannose, D-rhamnose, D-xylose in the roots of Sechium edule on silica gel with chloroform - n-butanol - methanol - water - acetic acid 9:15:10:3:3. Detection by spraying with 5 % sulfuric acid in methanol containing 0.1 % orcinol, followed by heating at 80 °C for 5-10 min.

      Classification: 10a
      130 045
      Investigation of market herbal products regulated under different categories: How can HPTLC help to detect quality problems?
      Debora FROMMENWILER, E. REICH*, M. SHARAF, S. CAÑIGUERAL, C. ETHERIDGE (*CAMAG Laboratory, Muttenz, Switzerland, eike.reich@camag.com)

      Front. Pharmacol. 13, 925298 (2022). HPTLC of milk thistle on silica gel with toluene - ethyl formate - formic acid 8:10:1. Detection by dipping in NP reagent and subsequently in PEG reagent, followed by heating at 100 °C for 5 min. Qualitative analysis under UV light at 254 and 366 nm. HPTLC of alkylamides in coneflower on silica gel with ethyl acetate - ethyl methyl ketone - water - formic acid 5:3:1. Detection by dipping in NP reagent and subsequently in PEG reagent, followed by heating at 100 °C for 5 min. Qualitative analysis under UV light at 254 and 366 nm. HPTLC of black cohosh on silica gel with toluene - ethyl formate - formic acid 5:3:2. Detection by dipping into sulfuric acid reagent (20 mL of sulfuric acid in 180 mL of methanol), followed by heating at 100 °C for 5 min. 

      Classification: 32e
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