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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      131 007
      Principal component analysis and DoE-Based AQbD Approach to Multipurpose HPTLC method for synchronous estimation of multiple FDCs of metformin HCl, repaglinide, glibenclamide and pioglitazone HCl
      P. PRAJAPATI*, K. RADADIYA, S. SHAH (*Department of Quality Assurance, Maliba Pharmacy College, Uka Tarsadia University, Tarsadi, Gujarat, India; pintu.prajapati@utu.ac.in)

      J Chrom Sci, bmad055 (2022). Standards of antiglycemic drugs were metformin hydrochloride (S1, a biguanide), glibenclamide (S2 = glyburide, a sulfonylurea), pioglitazone hydrochloride (S3, a thiazolidinedione), repaglinide (S4, a glinide). Samples were methanolic solutions of commercial tablets of S1 with each of the other molecules. The following method was developed by a software-assisted AQbD approach (analytical quality by design): (1) Several TLC separations were tried with toluene together with other solvents and with acidic or basic modifiers, with also variations of 24 method or instrumental parameters. (2) Principal component analysis (PCA) was performed in order to identify two principal components (PCs) responsible for 98 % of the observed variations: namely, resolution and tailing factor. Three critical method parameters (CMPs) had a statistically significant impact on the PCs: mobile phase (MP) composition, ammonium acetate concentration in MP, and saturation time. (3) To optimize these CMPs, the Box–Behnken design was implemented in 15 software-proposed experiments; the impacts of the 3 CMPs on the 2 PCs were evaluated by ANOVA, multiple regression analysis, and 2D and 3D contour plots. (4) The optimal CMPs ranges were determined by defining a MODR (method operable design region) on the superposed contour plots, and one TLC condition was selected as analytical control point.
      TLC on silica gel pre-washed with 10 mL methanol, dried and activated 10 min at 100° C. Separation with toluene – ethyl acetate – methanolic solution of 4 % ammonium acetate 7:7:6 after 15 min pre-saturation with 35 % relative humidity. Absorption emasurement at UV 254 nm. The hRF values were 13 for S1, 72 for S2, 82 for S3, 38 for S4. LOQ were 263, 387, 73 and 35 ng/zone, respectively. Linearity range was 25–75 µg/zone for S1, 100–300 ng/zone for S2 and S4, 750–2250 ng/zone for S3. Intermediate precision was below 2 %. For accuracy tests, recovery rates were between 97.6–101.4 %.

      Classification: 2e, 5c, 7, 8b, 17a, 17c, 23d, 23e, 24, 32a
      131 006
      Application of Taguchi OA and Box–Behnken design for the implementation of DoE-based AQbD approach to HPTLC method for simultaneous estimation of azilsartan and cilnidipine
      P. PRAJAPATI*, P. TAILOR, A. SHAHI, A. ACHARYA, S. SHAH
      (*Department of Quality Assurance, Maliba Pharmacy College, Uka Tarsadia University, Tarsadi, Mahuva, Surat, Gujarat, India; pintu21083@gmail.com)

      J Chrom Sci, bmad045 (2022). Standards were azilsartan medoxomil (AZL) and cilnidipine (CLN). Samples were acetonitrile solutions of commercial tablets of AZL and CLN, and purified human blood plasma as biological fluid spiked with AZL and CLN. The following method was developed by a software-assisted AQbD approach (analytical quality by design): (1) Taguchi orthogonal array design was implemented in 8 screening experiments in order to identify the 3 critical method variables (CMVs), which were: volume ratio of toluene – ethyl acetate, volume of methanol and saturation time. These CMVs had statistically significant impact (one-way ANOVA and Pareto charts) on the 3 critical analytical attributes (CAAs, they were: resolution between AZL and CLN and their hRF values). (2) To optimize these CMVs, the Box–Behnken design was implemented in 15 software-proposed experiments; the impacts of the 3 CMVs on the 3 CAAs were evaluated by ANOVA, multiple regression analysis, and 2D and 3D contour plots; the response surface analysis allowed the software to find a mathematical (quadratic or linear) equation for each CAA, based on the CMVs values. (3) The optimal CMVs ranges were determined by defining an analytical design space (ADS) on the superposed contour plots, and one TLC condition was selected as analytical control point.
      TLC on silica gel pre-washed with 10 mL methanol, dried and activated 15 min at 110° C. Separation with toluene – ethyl acetate – methanol 13:3:4 after 15 min pre-saturation with 35 % relative humidity. Absorption measurement at UV 254 nm. The hRF values were 49–51 for AZL and 70–71 for LRT. Linearity range was 400–2000 ng/zone for AZL and 100–500 ng/zone for CLN. Intermediate precision was below 1.6 % (n=3). LOQ were 121 ng/zone for AZL and 34 ng/zone for CLN. Recovery rates were 99.3–99.7 % for AZL and 98.1–99.5 % for CLN. Recovery rates from spiked plasma were 83.3 % for both molecules.

      Classification: 2e, 7, 8b, 16, 23d, 23e, 32a
      131 004
      Simultaneous determination of montelukast sodium and loratadine by eco-friendly densitometry and spectrophotometric methods
      Shimaa A. MAHMOUD*, A.M. EL-KOSASY, F.A. FOUAD
      (*Pharmaceutical Analytical Chemistry Department, Faculty of Pharmacy, Al-Azhar University, Cairo, Egypt; shimaa.ahmed22@azhar.edu.eg)

      J Chrom Sci, bmad025 (2023). Standards (separated and mixed) were montelukast sodium (MKT) and loratadine (LRT). Samples were methanolic solutions of commercial tablets, and purified blood plasma as biological fluid, from patients taking MKT or LRT as oral treatment. TLC on silica gel with ethyl acetate – ethanol 9:1. Visualization under UV 254nm. The hRF values were 80 for MKT and 71 for LRT. Densitometric absorbance measurement at 260 nm (20 mm/s scanning speed). System suitability was verified by resolution, selectivity, capacity and absence of tailing. The method was validated for linearity range (0.3–3.6 μg/zone for MKT, 0.2–4 µg/zone for LRT), for precision, for reproducibility, for robustness, and for accuracy expressed as average recovery values (100 % overall mean) at different concentrations. The TLC-densitometric method was also found statistically equivalent (Student’s t-test and F-test) to a previously described method (HPLC – spectrophotometry), but was better in terms of environmental and health impacts, using green analytical procedure index (GAPI) and analytical eco-scale (scores based on solvents/reagents, energy consumption, occupational hazard and waste generation). The TLC method was also compared to three (equally “green”) different analytical methods of spectrophotometry (without chromatography): response correlation, absorptivity-centering and LRT-MKT ratio derivatives. The TLC method was more sensitive (LOQ values were 82 ng/zone for MKT, 20 ng/zone for LRT).

      Classification: 5c, 7, 17c, 23d, 23e, 24, 32a, 32c
      129 060
      Detection of low levels of genotoxic compounds in food contact materials using an alternative HPTLC-SOS-Umu-C assay
      D. MEYER, M. MARIN-KUAN, E. DEBON, P. SERRANT, C. COTTET-FONTANNAZ, B. SCHILTER, Gertrud E. MORLOCK*
      (*Institute of Nutritional Science, Justus Liebig University Giessen, and TransMIT Center of Effect-Directed Analysis, Giessen, Germany; gertrud.morlock@uni-giessen.de)

      ALTEX - Alternatives to animal experimentation, 38(3), 387-397 (2021). Samples were standards of food contact contaminants with genotoxicity (4-nitroquinoline-1-oxide (NQO), aflatoxin B1, hexachloroethane, nitroso-ethylurea, phenformin, PhIP) or negative controls (alosetron, mannitol), and extracts of coated tin cans (extracted with n-hexane – acetone at 25°C for 16 h or by heating at 60 °C with ethanol 95 % for 240 h). HPTLC on RP18W layer, pretreated to harden the binder by heating 1 h at 120 °C, prewashed with methanol and with ethyl acetate and dried 4 min in cold air stream after each development. Application areas were focused to their upper edges by a two-fold elution with ethyl acetate, followed by 1 min drying in cold air stream. Development with toluene – ethyl acetate 8:5, followed by 5 min drying, neutralization with citrate buffer (pH 12) and 4 min drying. Effect-directed analysis for genotoxicity (SOS response – UMU-C test, using NQO as positive control) by immersion (speed 3.5 cm/s, time 3 s) into Salmonella typhimurium suspension and, after 3 h incubation at 37 °C and 4 min drying in cold air stream, into one of two fluorogenic substrate solutions (methylumbelliferyl- vs. resorufin-galactopyranoside). After 1 h incubation at 37 °C, visualization of mutagenic compounds as (blue vs. red) fluorescent zones at FLD 366 nm, and densitometry performed with mercury lamp for fluorescence (at  366 / >400nm vs. 550 / >580 nm, respectively). Further validation experiments, including spiking extracts with NQO, were performed showing good mean reproducibility, no quenching or other matrix effects. Lowest effective concentration of NQO was 0.53 nM (20 pg/band), 176 times lower than in the corresponding microtiter plate assays.

      Classification: 4e, 5c, 8b, 16, 23d, 23e, 32d
      56 107
      Chromatographic study of various acridine-glycosides by TLC and HPLC methods
      J. JAVOR, I. KISS

      Budapest Chromatography Symposium June 13, 1985. Optimization of TLC separation of biologically active acridine glycosides; more than 50 solvent systems and 10 "straight" and reversed-phase layers investigated. Best results with MERCK silica gel and isobutanol - ethanol - water - NH3 55:20:20:5.

      Classification: 23d, 32a
      57 105
      Determination of methyl nicotimate in pharmaceutical creams by high-performance thin-layer chromatography
      B. DE SPIEGELEER, W. VAN DEN BOSSCHE, P. DE MOERLOOSE

      Chromatographia 20, 249-252 (1985). HPTLC of methyl nicotinate on silica with ether - dichloromethane - hexane 5:3:2. Detection by spraying with 0.1 % solution of the ammonium salt of 8-anilino-naphthalene-1-sulfonic acid in water. Quantification by densitometry at 263 nm. 1) 3-pyridine carboxaldehyde was used as internal standard. 2) After quantification of methyl nicotinate the same plate was used for the identification of the cream base excipients with methanol - chloroform 3:2.

      Classification: 23d, 32c
      58 032
      Preparative separation of bipyridyl isomers using sequential centrifugal layer chromatography (SCLC)
      SZ. NYIREDY, C.A.J. ERDELMEIER, O. STICHER

      Fresenius Z. Anal. Chem. 321, 556-558 (1985). Description of sequential centrifugal layer chromatography (SCLC), a new technique for preparative separation of isomers and other substances. TLC of 5 bipyridyl isomers on silica with 1.9 % tetrahydrofuran -1.59 % dioxane -1.39 % methoxyethanol -95.12 % hexane. Detection by UV 254 nm.

      Keywords:
      Classification: 3d, 23d
      61 242
      Synthesis and anticonvulsant properties of N-methyl-pyridyl derivatives of m- and p-bromophenylsuccinimides
      A. ZEJC*, J. OBNISKA, E. CHOJNACKA-WOJCIK, E. TATARCZYNSKA, B. WICZYNSKA, (*Dep. of Pharmaceutical Chemistry, Medical Academy, Skaleczna 10, 31-065 Kraków, Poland)

      Polish Journal of Pharmacology and Pharmacy 39, 91-95 (1987). TLC or N-methylpyridyl derivatives of bromophenylsuccinimide on silica with chloroform - acetone 9:1. Visualization with 0.05M iodine in 10% HCL.

      Classification: 23d, 32a