PLoS ONE 18(11), e0295012 (2023). TLC on silica gel to monitor the synthesis of 15 new camphene-based thiosemicarbazones produced by the reaction of camphene thiosemicarbazide either with benzaldehydes, or with acetophenones, or with one of the following molecules: benzophenone, cinnamic aldehyde, ethyl pyruvate, furaldehyde, menthone, pyrrole carboxaldehyde or thiophene-carboxaldehyde. Development with n-hexane – ethyl acetate 3:7 in the case of benzaldehydes, except vanillin; or 7:3 for the vanillin derivative and all others, followed by visualization of products with resublimated iodine. The aldehyde used for compound 15 is in fact vanillin.

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 %.

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).

J. Planar Chromatogr. 35, 473-479 (2022). HPTLC of capsaicin and dihydrocapsaicin as capsaicinoids in Habanero pepper pods on silica gel with cyclohexane - chloroform - acetic acid 7:2:1. Quantitative determination by absorbance measurement at 254 nm. The hRF value for capsaicinoids was 29. Linearity was between 0.5 and 4.0 µg/zone. Interday and intra-day precisions were below 6 % (n=6). The LOD and LOQ were 251 and 750 ng/zone, respectively. 

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).

J. Planar Chromatogr. 35, 61-71 (2022). HPTLC of empagliflozin (1) in the presence of metformin HCl (2) on silica gel with toluene - methanol - ammonia - glacial acetic acid 72:26:1:1. Quantitative determination by absorbance measurement at 230 nm. The hRF values for (1) and (2) were 15 and 48, respectively. Linearity was between 11 and 112 ng/zone for (1) and 85 and 850 ng/zone for (2). Interday and intra-day precisions were below 2 % (n=3). The LOD and LOQ were 0.6 and 1,7 ng/zone for (1) and 5 and 15 ng/zone for (2), respectively. Recovery was found to be in the range of 99.4-101.0 % for (1) and 100.3-101.4 % for (2). Degradation products were characterized by liquid chromatography coupled with electrospray ionization‒quadrupole-time of flight‒tandem mass spectrometry (LC‒ESI‒QTOF‒MS/MS).

Rapid Commun. Mass Spectrom. 34, 8755 (2020). HPTLC of a synthetic formulated gasoline (diluting polypropylene glycol and polyisobutylene succinimide polyamine surfactant at a mass ratio of 1 % in gasoline) on silica gel with methanol - toluene 2:3. Detection under UV light. Samples were scratched for analysis by atmospheric solids analysis probe mass spectrometry (ASAP-MS).

J. Sep. Sci. 43, 2981-2988 (2020). HPTLC of citicoline (1) and piracetam (2) in presence of their degradation products on silica gel with methanol - chloroform - ammonium chloride buffer 9:1:2. Quantitative determination by absorbance measurement at 230 nm. The hRF values for (1) and (2) were 15 and 85, respectively. Linearity was between 0.2 and 4 µg/zone for both (1) and (2). Intermediate precision was below 2 % (n=3). The LOD and LOQ were 56 and 180 ng/zone for (1) and 53 and 170 ng/zone for (2), respectively. Average recovery was 100.9 % for (1) and 99.8 % for (2).