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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      130 112
      Separation of acetylferrocene from synthetic mixtures by countercurrent chromatography
      X. LI (Li Xiaoyuan), H. YOU (You Haibo), H. QIU (Qiu Huiyun), M. WEN (Wen Mengyi), C. ZHENG (Zheng Chuncui), S. TONG* (Tong Shengqiang) (*College of Pharmaceutical Science, Zhejiang University of Technology, Moganshan Campus, Gongda Road 1, Deqing, Huzhou, China, sqtong@zjut.edu.cn)

      J. Liq. Chromatogr. Relat. Technol. https://doi.org/10.1080/10826076.2022.2143798 (2022). HPTLC of ferrocene and acetyl ferrocene from their synthetic mixtures on silica gel with ethyl acetate - petroleum ether 1:9. Detection by exposure to iodine vapor.

      Classification: 26a
      130 003
      Purification and characterization of a novel endolytic alginate lyase from Microbulbifer sp. SH-1 and its agricultural application
      J. YANG, D. CUI, D. CHEN, W. CHEN, S. MA, H. SHEN* (*College of Natural Resources and Environment, South China Agricultural University, Guangzhou, and Guangdong Provincial Key Laboratory of Eco-Circular Agriculture, Guangzhou, China; hshen@scau.edu.cn)

      Marine Drugs 18(4), 184 (2020). A new alginate lyase (AlgSH7), isolated from marine bacterium Microbulbifer sp. strain SH1 (Alteromonadaceae), was incubated (24 h at 40 °C) with sodium alginate from brown algae (1 % in TRIS-HCl buffer, pH 9), or with related mannuronate and guluronate polymers (polyM and polyG), or with related saccharides with different polymerisation degrees (PD 1 – 4). TLC of reaction products as well as saccharides, on silica gel with n-butanol ­– acetic acid – water 3:2:2. Derivatization by spraying sulfuric acid (10 % in ethanol), followed by 5 min heating at 130 °C. The enzyme was active only on alginate and on polyM, cleaving them into oligomeric fragments (PD 2 – 4); it was inactive on polyG or on oligomers.

      Classification: 4e, 10
      130 028
      The effect of extractive lacto-fermentation on the bioactivity and natural products content of Pittosporum angustifolium (gumbi gumbi) extracts
      Snezana AGATONOVIC-KUSTRIN*, V. GEGECHKORI, D.W. MORTON
      (*Department of Pharmaceutical and Toxicological Chemistry, Institute of Pharmacy, Sechenov University, Moscow, Russia, and School of Pharmacy and Biomedical Sciences, La Trobe Institute for Molecular Sciences, La Trobe University, Bendigo, Australia; s.kustrin@latrobe.edu.au)

      J Chromatogr A, 1647, 462153 (2021). Samples were extracts of Pittosporum angustifolium leaves (Pittosporaceae), either pure or fermented 1-4 weeks in NaCl solution, as well as acarbose, gallic acid, β-sitosterol, caffeic and chlorogenic acids, as standards. HPTLC on silica gel (prewashed with methanol and dried 15 min at 105 °C) with n-hexane – ethyl acetate – acetic acid 15:9:1. Derivatization by immersion (speed 5 cm/s, time 1 s): (A) into DPPH• 0.2 % solution, to detect radical scavengers; (B) into neutralized ferric chloride (3 % in ethanol), followed by 5 min heating at 110 °C, for detection of phenolic compounds; (C) into anisaldehyde – sulphuric acid reagent, followed by 10 min heating at 110 °C, to detect terpenes and steroids. Effect-directed analysis (EDA) for α-amylase inhibition assay (D) by immersion into enzyme solution, incubation 15 min at 37 °C, immersion into substrate solution (starch 2 % in water), incubation 20 min at 37 °C and immersion into Gram’s iodine solution for detection (inhibition zones appear blue on white background). In all cases, visualization under white light. Quantification was performed on pictures using image processing software, and expressed as equivalents to the respective standards used for calibration curves: (A) and (B) gallic acid (LOQ 250 and 740 ng/band, respectively), (C) β-sitosterol (LOQ 1.5 µg/band), (D) acarbose (LOQ 8 µg/band). Zones of interest, scraped from untreated plates and washed with ethyl acetate, were submitted by ATR-FTIR analysis. An amylase inhibiting zone (hRF 85) present in all extracts was identified as fatty acid esters: ethyl palmitate in unfermented and methyl linoleate in fermented extracts. Moreover, fermented extracts contained antioxidant zones (hRF 15 – 20), identified as monomers and oligomers (including hydroxycinnamic, guaiacyl, syringyl derivatives) from decomposed lignin.

      Classification: 4e, 7, 8b, 11a, 32e
      130 013
      Characterization of natural herbal medicines by thin-layer chromatography combined with laser ablation-assisted direct analysis in real-time mass spectrometry
      Y. CHEN (Chen Yilin), L. LI (Li Linnan)*, R. XU (Xu Rui), F. LI (Li Fan), L. GU (Gu Lihua), H. LIU (Liu Huwei), Z. WANG (Wang Zhengtao), L. YANG (Yang Li)** (*Shanghai Key Laboratory of Compound Chinese Medicines, and Institute of Chinese Materia Medica, Shanghai University of Traditional Chinese Medicine, Shanghai, China; **Institute of Interdisciplinary Integrative Medicine Research, Shanghai University of Traditional Chinese Medicine, Shanghai, China; *linnanli@shutcm.edu.cn, **yl7@shutcm.edu.cn)

      J Chromatogr A, 1625, 461230 (2020). Samples were extracts of Chinese plants: Acorus tatarinowii (= Acorus calamus var. angustatus) rhizomes (Araceae / Acoraceae) (1), Angelica sinensis roots (Apiaceae) (2), Gynura japonica rhizomes (Asteraceae) (3), Phellodendron chinense bark (Rutaceae) (4), Picrasma quassioides twigs and leaves (Simaroubaceae) (5), Rheum sp. roots and rhizomes (R. palmatum, R. tanguticum and/or R. officinale) (Polygonaceae) (6), Sophora flavescens roots (Fabaceae) (7), Dendrobium stems (D. aphyllum, D. aurantiacum var. dennaeanum, D. chrysanthum, D. chrysotoxum, D. gratiosissimum, D. hercoglossum, D. thyrsiflorum, D. trigonopus and D. williamsonii) (Orchidaceae) (8). Standards were: gigantol (from D. sonia); methoxycarbonyl-β-carboline (MCC from (5)); caffeic acid, emodin; senecionine and β-asarone; crategolic acid (= maslinic acid), corosolic acid, oleanic acid, ursolic acid; sesquiterpenoids (atractylenolides I – III) from Atractylodes macrocephala (Asteraceae); flavonoids (baicalein, baicalin, daidzin, hesperidin, wogonin) from Scutellaria baicalensis roots (Lamiaceae). HPTLC on silica gel with 10 mobile phases, depending on the samples. Detection under UV 254 nm and white light. For (3), derivatization with Dragendorff’s reagent (bismuth potassium iodide solution) for visualization of alkaloids. Zones of interest on underivatized plates were identified by a triple-quadrupole ­– linear ion-trap MS, the compounds being removed from the layer by a continuous-wave (445 nm) diode laser pointer through a DART interface (Direct Analysis in Real-Time, helium as gas for plasma-based ambient ionization, discharge needle voltage 1.5 kV, grid voltage 350 V, capillary temperature 300 °C and voltage 40 V, full scan in positive ionization mode in m/z range 150-800). Pigment standards were used for validation of this laser-assisted HPTLC-DART-MS method: malachite green, crystal violet, chrysoidin, auramine O, rhodamine B, Sudan red I – IV, Sudan red G, dimethyl yellow. Afterwards, the same HPTLC-MS method was applied to the origin / species determination of Dendrobium samples, based on the presence of four bibenzyl compounds erianin, gigantol, moscatilin, tristin. Erianin was present only in D. chrysotoxum, whereas none of these were detected in D. hercoglossum. Several components of the extracts were thus identified: asarone (a phenylpropanoid) in (1); phthalide lactones (butenylphthalide, ligustilide and chuanxiong lactone) in (2); co-eluting pyrrolizidine alkaloids (senecionine and seneciphylline) in (3); benzylisoquinoline alkaloid berberine in (4); alkaloids (canthinone alkaloids and MCC) in (5); anthraquinones (rhein, aloe-emodin, emodin, emodin methyl ether, chrysophanol) and (in negative mode) caffeic acid (a hydroxycinnamic acid) and corosolic, maslinic and oleanic acids (triterpenoids) in (6); quinolizidine alkaloids (matrine, oxymatrine, oxysophocarpine, sophoridine) in (7).

      Classification: 4e, 7, 8a, 8b, 15a, 22, 32e
      130 027
      Thin-layer chromatographic quantification of magnolol and honokiol in dietary supplements and selected biological properties of these preparations
      E. LATA, A. FULCZYK, P.G; OTT, T. KOWALSKA, M. SAJEWICZ, Ágnes M. MÓRICZ* (*Plant Protection Institute, Centre for Agricultural Research, 1022 Budapest, Hungary; moricz.agnes@agrar.mta.hu)

      J Chromatogr A, 1625, 461230 (2020). Samples were methanolic extracts of commercial supplements containing Magnolia sp. bark (Magnoliaceae), as well as honokiol (1) and magnolol (2) (biphenyl neolignans) as separated or mixed standards. TLC and HPTLC on silica gel with n-hexane – ethyl acetate – ethanol 16:3:1. Visualization under UV 254 nm. Quantification of (1) and (2) by densitometric scanning in absorbance mode at 290 nm (hRF were 34 and 39, LOQ 200 ng and 280 ng/spot, respectively). Variability between samples from the same brand supplement was also determined, as well as extraction yields. Effect-directed analysis with 3 assays: A) to detect radical scavengers, immersion into DPPH• 0.02 % solution; B) to detect activity against Gram-negative bacteria, immersion into Aliivibrio fischeri suspension, followed by recording the bioluminescence; C) to detect activity against Gram-positive bacteria, immersion into Bacillus subtilis, followed by incubation 2 h at 28 °C and immersion into MTT 1 g/L. Compounds (1) and (2) were active in all assays. Identification of zones of interest by eluting with methanol from untreated TLC layer through the oval elution head of a TLC-MS interface directly to a single Quadrupole MS (electrospray ionization, interface temperature 350°C, heat block temperature 400°C, desolvation line temperature 250°C, detector voltage 4.5kV). Full mass scan spectra were recorded in the positive and negative ionization modes in m/z range 150–800. Other molecules (from other ingredients) were identified: piperine (alkaloid) and/or its geometrical isomers (active on A, hRF 29-30); and daidzein (active on A and B, hRF 18), isoflavone from Pueraria montana root (Fabaceae). Stability was assessed through 2D-HPTLC, by repeating the same development method in the orthogonal direction 4 h or 20 h after the first separation. Degradation products of (1) and (2) appeared after 20 h (but not at 4 h), including a honokiol dimer (formed in tracks of (1) and of (2)).

      Classification: 4e, 7, 8a, 22, 32e
      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
      130 142
      Bioassay-guided identification of α-amylase inhibitors in herbal extracts
      Snezana AGATONOVIC-KUSTRIN*, E. KUSTRIN, V. GEGECHKORI, D. W. MORTON (*Department of Pharmaceutical and Toxicological Chemistry, Institute of Pharmacy, Sechenov University, Moscow, Russia, and School of Pharmacy and Biomedical Sciences, La Trobe Institute for Molecular Sciences, La Trobe University, Bendigo, Australia; s.kustrin@latrobe.edu.au)

      J Chromatogr A, 1620, 460970 (2020). Samples were ethyl acetate extracts of Lavandula angustifolia herb and flowers and of aerial parts of other Lamiaceae (Ocimum basilicum, Origanum vulgare, Thymus vulgaris, Rosmarinus officinalis, Salvia officinalis), as well as standards. HPTLC on silica gel (pre-washed with methanol and heated 30 min at 105 °C) with n-hexane – ethyl acetate – acetic acid 70:27:3. Documentation at UV 254 nm and 365 nm and white light before and after A) derivatization with anisaldehyde – sulfuric acid reagent, followed by 10 min heating at 110 °C; B) spraying with DPPH• (0.2 % in methanol), followed by 30 min incubation in the dark; C) α-amylase inhibition assay by immersion into enzyme solution, incubation 30 min at 37 °C, immersion into substrate solution (starch 1 % in water), incubation 20 min at 37 °C and immersion into Gram’s iodine solution for detection (inhibition zones appear blue on white background). Quantification was performed on pictures using image processing software, and expressed as equivalents to the respective standards used for calibration curves: A) β-sitosterol (LOQ 1.5 µg/band), B) gallic acid (LOQ 60 ng/band), C) acarbose (LOQ 8 µg/band). An amylase inhibiting zone (hRF 68) present in all samples (except L. angustifolia), scraped from untreated plates and washed with ethyl acetate, was tentatively identified by ATR-FTIR analysis as oleanolic acid (pentacyclic triterpene).

      Classification: 4e, 15a, 32e
      130 004
      Identification of acetylcholinesterase inhibitors in water by combining two-dimensional thin-layer chromatography and high-resolution mass spectrometry
      Lena STÜTZ*, W. SCHULZ, R. WINZENBACHER (*Laboratory for Operation Control and Research, Zweckverband Landeswasserversorgung, Langenau, Germany; stuetz.l@lw-online.de)

      J Chromatogr A, 1624, 461239 (2020). Samples were chemical standards of acetylcholinesterase (AChE) inhibitors (azamethiphos, caffeine, donepezil, galanthamine, methiocarb-sulfoxide, paraoxon-ethyl) and of neurotoxic compounds, as well as drinking or contaminated water samples enriched through solid phase extraction. HPTLC on spherical silica gel (pre-washed twice by 20 min immersion in isopropanol, heated 20 min at 120 °C before and after pre-washing with acetonitrile). First separation (preparative TLC) with automated multiple development (16 steps). Effect-directed analysis for AChE inhibitors by immersion (speed 5 cm/s, time 1 s) into enzyme solution, incubation 5 min at 37 °C and immersion into substrate solution (indoxyl acetate 2 % in methanol); visualization under UV 366 nm. Active zones from untreated layers were eluted through the oval head of a TLC-MS interface to a second plate for a second separation with a panel of other mobile phases. Bands of interest were eluted from the second layer with water through the oval elution head of the TLC-MS interface pump, into a RP18 liquid chromatography guard column, followed by a quadrupole time-of-flight mass spectrometer. Full scan mass spectra (m/z 100–1200) were recorded in negative and positive modes using electrospray ionization (and collision-induced dissociation for MS2). Among the water contaminants, lumichrome (riboflavin photolysis product), paraxanthine and linear alkylbenzene sulfonates were identified as AChE inhibitors.

      Classification: 3d, 4d, 4e, 22, 29b, 35d, 37c
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