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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      130 144
      Combining multivariate image analysis with high-performance thin-layer chromatography for development of a reliable tool for saffron authentication and adulteration detection
      A. AMIRVARESI, M. RASHIDI, M. KAMYAR, M. AMIRAHMADI, B. DARAEI, H. PARASTAR* (*Department of Chemistry, Sharif University of Technology, Tehran, Iran; h.parastar@sharif.edu)

      J Chromatogr A, 1628, 461461 (2020). Samples were hydro-methanolic extracts of 100 genuine saffron samples (Crocus sativus stigmata, Iridaceae) from South Khorasan (SK) and Razavi Khorasan (RK) provinces (Iran), pure or mixed in several proportions with common vegetal adulterants: C. sativus style, Calendula officinalis petals (Asteraceae, Asteroideae), Carthamus tinctorius petals (Asteraceae, Carduoideae), Rubia tinctorum rhizomes (Rubiaceae). Commercial saffron samples (containing artificial adulterants) were also tested. TLC on silica gel with ethyl acetate – methanol – water – acetic acid 66:23:11:1. Evaluation at 254 nm, 366 nm, and 440 nm. Crocin (carotenoid, hRF 38) was used for optimization of extraction (parameters being first calculated by chemometry), using multilinear regression and ANOVA. Image data (pixel intensities and colors of each sample under the three selected wavelengths) were unfolded into a data matrix and transformed into a vector, used for multivariate image analysis of the chromatogram fingerprints. This allowed: A) separation of genuine samples by principal component analysis (PCA) into 2 clusters according to origin (cold climate in Northern half of RK vs. warm climate in SK and Southern part of RK) with 92 % prediction accuracy; B) separation of samples according to purity / vegetal adulterant groups by partial least squares – discriminant analysis (PLS-DA) with 98 % accuracy (if 10 µL extract applied); C) separation with 100 % prediction accuracy by PCA between genuine, mixed, and commercial samples.

      Classification: 4c, 4e, 8b, 14, 32e
      130 005
      Multiobjective optimization of microemulsion – thin layer chromatography with image processing as analytical platform for determination of drugs in plasma using desirability functions
      Noura H. ABOU-TALEB*, D. T. EL-SHERBINY, N. M. EL-ENANY, H. I. EL-SUBBAGH (*Medicinal Chemistry Department, Faculty of Pharmacy, Mansoura University, Mansoura, Egypt; nourahemdan@yahoo.com)

      J Chromatogr A, 1619, 460945 (2020). Samples were lamotrigin as standard, or extracted with an oil-in-water microemulsion (10 µL butyl acetate, 4 mL n-butanol, 925 mg sodium dodecyl sulphate, 8.6 mL water) either from patients’ raw plasma (for separation from blood proteins) after spiking, or from commercial tablets dissolved in methanol. TLC on silica gel with a water-in-oil microemulsion of 9 mL butyl acetate, 1 mL n-butanol, 250 mg sodium dodecyl sulphate, 250 µL water. Both optimal microemulsions were predicted using Taguchi orthogonal array and Plackett-Burman design. Evaluation in UV 254 nm, quantification from the digital picture using four image processing software programs. For lamotrigin (hRF 24), limits of quantification were 170 ng for pure drug and 10 ng for spiked plasma. Linearity (in range 20–200 ng/spot) was directly obtained for the calibration curve in spiked plasma; however, for pure drug, linearity was obtained only when using log values of the calculated densities (300–3000 ng/spot).

      Classification: 3a, 3d, 5c, 23e, 32c
      130 008
      High performance thin-layer chromatography–mass spectrometry methods on diol stationary phase for the analyses of flavan-3-ols and proanthocyanidins in invasive Japanese knotweed
      V. GLAVNIK, Irena VOVK* (*National Institute of Chemistry, Ljubljana, Slovenia; irena.vovk@ki.si)

      J Chromatogr A, 1598, 196-208 (2019). Samples were acertone – water 7:3 extracts of Reynoutria japonica (= Fallopia japonica = Polygonum cuspidatum) rhizomes (Polygonaceae) as well as flavanols (catechin, epicatechin, epicatechin gallate, epigallocatechin gallate) and procyanidins (A1, A2, B1–B3 and C1) as standards. HPTLC on diol silica gel with: (MP1) acetonitrile; (MP2) ethyl acetate; (MP3) ethyl acetate – formic acid 90:1; or (MP4) toluene – acetone – formic acid 3:6:1. Prewashing of the plates with mobile phase was needed only with MP1. After drying under hot air stream, derivatization by automated immersion into DMACA (dimethylaminocinnamaldehyde) – HCl solution (60 mg in 13 mL HCl + 187 mL ethanol), followed by 2 min drying under warm air stream. Visualization under UV 366 nm and white light, densitometry in absorption/reflectance mode at 280 nm (before derivatization) or 655 nm (10 min after derivatization). Bands of interest were eluted from layer with acetonitrile – methanol 2:1 through the oval elution head of a TLC-MS interface pump, into a RP18 liquid chromatography guard column, followed by a quadrupole ion trap mass spectrometer. Full scan mass spectra (m/z 150–2000) were recorded in negative mode using electrospray ionization (spray voltage 4 kV, capillary temperature 200◦C, capillary voltage -38.8 V). Monomer gallates to hexamer gallates were detected, separated with MP1, MP2 or MP4; monomers and oligomers (not gallates) were separated with MP3 (up to hexamers) and with MP1 and MP4 (up to decamers). Moreover, enhanced absorption of standards was also studied for influence of mobile phases, of layers (diol silica gel vs. classical silica gel vs. cellulose) and of luminosity (light vs. dark).

      Classification: 4e, 8a, 8b, 32e
      130 007
      Planar chromatography-bioassays for the parallel and sensitive detection of androgenicity, anti-androgenicity and cytotoxicity
      C. RIEGRAF, A.M. BELL, M. OHLIG, G. REIFFERSCHEID, S. BUCHINGER* (*Federal Institute of Hydrology, Koblenz, Germany; buchinger@bafg.de)

      J Chromatogr A, 1684, 463582 (2022). Samples were concentrated filtrates of leachates of waste deposition sites, as well as testosterone, flutamide, bisphenol A (BPA) and nitroquinoline oxide (NQO) as standards. Automated Multiple Development on HPTLC silica gel (prewashed with methanol and dried 30 min at 110 °C) with 1) methanol up to 20 mm; 2A) chloroform – ethyl acetate –petroleum ether 11:4:5 or 2B) ethyl acetate – n-hexane 1:1 for flutamide and testosterone, up to 90 mm. Effect-directed analysis was performed by automated spraying 3 mL suspension of BJ1991 yeast (transfected Saccharomyces cerevisiae strain, pure for androgenic activity, with 50 ng/mL testosterone for anti-androgenic assay), followed by 20 h incubation at 30 °C in a closed chamber (90 % relative humidity), by 5 min drying under cold air stream, by spraying 2.5 mL MUG solution (4-methylumbelliferyl-galactopyranoside) and by 15 min incubation at 37 °C in an open chamber. Agonistic and antagonistic activities were detected qualitatively under UV 366 nm (light or dark blue bands, respectively, on blue background) and quantitatively documented using automated scanning at excitation wavelength 320 nm (deuterium lamp), with cut-off filter at 400 nm. Dose-response curves for model compounds were established by regression analysis. Anti-androgenic effective doses at 10 % were 28 ng/zone for flutamide and 20 ng/zone for BPA, without toxicity for the yeast. To exclude cytotoxicity where anti-androgenic activity was observed, the HPTLC layers (either without or after the spraying with MUG) were sprayed with 3 mL resazurin solution (0.01 % in water) and incubated 30 min at 30 °C and 90 % humidity. Cytotoxicity bands appeared as pink zones of resorufin on a colorless background (dihydroresorufin) under white light. Densitometric evaluation in absorption mode at 575 nm (under deuterium and halogen-tungsten lamps, no filter applied). NQO was cytotoxic at its lowest tested dose (1 ng/zone).

      Classification: 4b, 4e, 32d, 37c, 37d
      130 002
      An improved method for a fast screening of α-glucosidase inhibitors in cherimoya fruit (Annona cherimola Mill.) applying effect-directed analysis via high-performance thin-layer chromatography-bioassay-mass spectrometry
      O. GALARCE-BUSTOS, J. PAVÓN-PÉREZ, K. HENRÍQUEZ-AEDO, M. ARANDA*
      (*Department of Food Science and Technology, Faculty of Pharmacy, University of Concepción, Concepción, Chile; maranda@udec.cl, maranda@gmx.net)

      J Chromatogr A, 1608, 460415 (2019). Samples were acetonitrile extracts of Annona cherimola fruit peel, pulp and seeds (Annonaceae), as well as caffeic acid as standards. HPTLC on silica gel with chloroform – ethyl acetate – propanol 21:2:2 for peel extracts, with chloroform – methanol 9:1 for seed extracts. Derivatization by spraying Dragendorff’s reagent for alkaloids, secondary amines and non-nitrogenous oxygenated compounds.  Effect-directed assay was performed for inhibitors of α-glucosidase. Before sample application, plates were developed with enzyme substrate (2-naphthyl-α-D-glucopyranoside 0.1 % in methanol) and dried 20 min at 60 °C. Then, samples were applied and separated, and mobile phase was removed by heating 10 min at 60 °C. The chromatogram was sprayed with 4 mL enzyme solution (5 unit/mL in 100 mM phosphate buffer,  pH 7.4), liquid excess was removed under lukewarm air stream, the plate was incubated 10 min at 37 °C in a moisture box, followed by spraying chromogenic reagent Fast Blue salt B 0.1 % in water, giving after 2 min white inhibition bands visible on purple background under white light. Plate image was documented under illumination (reflectance mode) with white light. The bands of 3 inhibiting compounds were analyzed in a triple quadrupole mass spectrometer. 1) Full scan mass spectra (m/z 50−1000) in the positive ionization mode were recorded using electrospray ionization (ESI, spray voltage 3 kV, desolvation line temperature 250 °C, block temperature 400 °C) for compounds directly eluted with methanol – acetonitrile through the oval elution head of a TLC-MS interface pump. 2) Compounds were also isolated (either eluted directly from the plate into a vial through the same interface, or scraped from the plate and extracted with methanol – chloroform into a vial), dried, and submitted to HPLC-DAD-MS/MS; MS-MS spectra were recorded in the same conditions, using argon as collision gas and collision cell voltages from -20 and -40 V. Inhibitors were identified as phenolamides (phenylethyl cinnamides): moupinamide (hRF 66 in peels, 56 in seeds), N-trans-feruloyl phenethylamine (hRF 76 in peels), N-trans-p-coumaroyl tyramine (hRF 44 in seeds).

      Classification: 4d, 4e, 7, 17c, 32e
      130 009
      Development of a high performance thin layer chromatography method for the rapid qualification and quantification of phenolic compounds and abscisic acid in honeys
      N. STANEK, P. KAFARSKI, Izabela JASICKA-MISIAK* (*Faculty of Chemistry, Opole University, Opole, Poland; izajm@uni.opole.pl)

      J Chromatogr A, 1598, 209-215 (2019). Samples were methanolic extracts of honeys from Robinia pseudoacacia (Fabaceae) or from Tilia spp. (Tiliaceae / Malvaceae), as well as standards: abscisic acid (sesquiterpenoid), caffeic acid, chlorogenic acid, cinnamic acid, ferulic acid (phenolic acids), chrysin (flavone), myricetin, quercetin (flavonols), naringenin (flavanone). HPTLC on silica gel with chloroform – ethyl acetate – formic acid 5:4:1. Visualization under UV 254 nm and 366 nm, before and after derivatization by spraying with aluminium chloride (1 % in methanol), which rendered flavone bands bright yellow. Quantitative absorbance measuremet by densitometry at 366 nm. Linearity was in the range of 12,5–200 µg/mL for most standards (25–400 µg/mL for chrysin). Main differences observed in samples: 1) abscisic acid (hRF 56) and chrysin (hRF 82) were present only in Tilia honey samples, quercetin (hRF 55) only in Robinia honey; 2) ferulic acid (hRF 60) was the most prominent blue band in Tilia honey samples (1.35–18.73 g/kg of honey), and less intense in Robinia honey (0–1.24 g/kg of honey). Multivariate analysis was performed in two different ways with principal component analysis.

      Classification: 7, 8a, 15a, 32e
      130 020
      Versatile TLC-densitometric methods for the synchronous estimation of cinnarizine and acefylline heptaminol in the presence of potential impurity and their reported degradation products
      O.M. EL-HOUSSINI*, M.A. MOHAMMAD (*Nat. Organ. for Drug Contr. & Res. (NODCAR), 51 wezerat El- Zeraa Street St, Agouza P.O. Box 12553 Giza 35521, Egypt, olamha23@hotmail.com)

      J Chromatogr Sci, 60 (9), 832-839 (2022). Establishment of two TLC methods for the synchronous estimation of cinnarizine (Cinn) and acefyline heptaminol (Acef) in the presence of reported Cinn/Acef degradation products, as well as theophylline (Theo) as potential impurity of Acef. TLC on silica gel (1) for Cinn with dichloromethane - methanol - formic acid 30:2:1 and (2) for Acef with the same solvents in ratio 150:7.5:4. Quantitative determination by densitometry at 254 nm showed that Cinn and Acef are well separated from their degradation products. The concentration range was 0.2 - 1.8 and 2 - 18 μg/zone for Cinn and Acef, respectively, with mean percentage recoveries of 99.2 / 99.8 and 99.2 / 99.7 for method 1 and method 2, respectively. The method is selective, robust and retained its accuracy in up to 50 % of Cinn/Acef reported degradation products and Theo. Application of the two methods to a coformulated drug product comprising Cinn and Acef with satisfactory results showing statistically no significant differences compared with those obtained by reference ones.

      Classification: 32a
      129 054
      The authentication of Java turmeric (Curcuma xanthorrhiza) using thin layer chromatography and 1H-NMR based-metabolite fingerprinting coupled with multivariate analysis
      A. ROHMAN*, T. WIJAYANTI, A. WINDARSIH, S. RIYANTO (*Department of Pharmaceutical Chemistry, Faculty of Pharmacy, Universitas Gadjah Mada, Yogyakarta, Indonesia; abdulkimfar@gmail.com)

      Molecules 25 (17), E3928 (2020). Samples were curcumin (as standard) and methanolic extracts of Curcuma xanthorrhiza and C. aeruginosa (Zingiberaceae) rhizomes, both separately and in mixtures. Separation on TLC silica gel with chloroform – methanol – formic acid 94:3:3. Densitometry of curcumin (hRF 50) in absorption mode at UV 427 nm. This method was validated with curcumin standard for selectivity (vs. demethoxycurcumin hRF 32), linearity range (250 - 450 ng), LOD (21 ng) and LOQ (69 ng), accuracy and precision. Curcumin contents were between 0.74 and 1.23 % in pure C. xanthorrhiza extracts, but decreased when adulterated with C. aeruginosa.

       

      Classification: 7, 32e
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