Authors:Danijela Ašperger, Lidija Ćurković, Alka Horvat and Marija Kaštelan-Macan
Qualitative identification of Cu, Sn, Pb, Ni, and Fe in Cu-alloys is presented. The method involves anodic sampling of alloys, separation and identification by thin-layer chromatography (TLC). The powerful desktop-computer tool makes it easy to optimize ternary solvent mixtures. Optimization was performed graphically by means of Rsi≥1 as a selected separation criterion. Mobile phase composition for optimal separation was determined as MeOH−HCl−H2O (60:35:5, v/v). The method was applied to Persian helmet as real sample.
Authors:Vesna Glavnik, Breda Simonovska, Irena Vovk, Dragana Pavlović, Danijela Ašperger and Sandra Babić
Validation of a method for the quantification of (−)-epicatechin and procyanidin B2 in chocolates is reported. After a simple preparation of the chocolate test solution, thin-layer chromatography (TLC) on high-performance thin-layer chromatographic (HPTLC) cellulose plates with n-propanol-water-acetic acid (20:80:1, ν/ν) and derivatization with 4-dimethylaminocinnamaldehyde (DMACA) were performed. Densitometry at 655 nm enabled accurate quantification of both analytes in chocolates. The milk chocolate sample which served for precision and recovery experiments contained 13.0 mg/100 g of (−)-epicatechin (relative standard deviation (RSD)) 5.8%, n = 6) and 13.2 mg/100 g of procyanidin B2 (RSD 4.2%, n = 6). Usable polynomial curves were 2–30 ng for (−)-epicatechin and 4–60 ng for procyanidin B2. The validated TLC method can be applied for routine quality control of the two major polyphenolic compounds in different chocolate samples.
Authors:Dragana Mutavdžić, Sandra Babić, Danijela Ašperger, Alka Horvat and Marija Kaštelan-Macan
This paper focuses on the study of different types of SPE material that can be used for preconcentration of eight pharmaceuticals from water samples. The compounds studied were enrofloxacine, norfloxacine, oxytetracycline, trimethoprim, sulfamethazine, sulfadiazine, sulfaguanidine, and penicillin G/procaine. Cartridges were tested on spiked water samples and extraction efficiency was determined by thin-layer chromatography (TLC) CN-modified chromatographic plates with 0.05 m
-methanol, 81 + 19, as mobile phase. Strata-X cartridges were proved to be the best type of SPE material for this group of pharmaceutical compounds. For this reason an SPE-TLC method with Strata-X cartridges and HPTLC plates was validated. The method has been applied to the determination of pharmaceutical products in production wastewater samples from the pharmaceutical industry.
Authors:Sandra Babić, Danijela Ašperger, Dragana Mutavdžić, Alka Horvat and Marija Kaštelan-Macan
This paper describes a method for separation and quantification of a mixture of antibiotics extracted from spiked water samples. The method involves SPE of the analytes from water then analysis of the extract by TLC. Excellent separation of sulfadimidine, sulfadiazine, sulfaguanidine, and trimethoprim (TMP) was achieved by HPTLC on silica gel F
plates with chloroform-methanol, 89 + 11, as mobile phase. Videodensitometric quantification was validated for linearity, precision, limit of detection, and limit of quantification. Limit of detection (
) was 0.05 µg per spot for sulfadimidine, sulfadiazine, and sulfaguanidine, and 0.1 µg per spot for TMP. Limit of quantification (
) was 0.1 µg per spot for sulfadimidine, sulfadiazine, and sulfaguanidine, and 0.2 µg per spot for TMP. The TLC method was tested on extracts obtained, by use of solid-phase extraction, from spiked water samples. The best recovery of these antibiotics was achieved by use of HLB cartridges and elution with acetonitrile. Apparent recoveries were 87.1 ± 8.4 for sulfadiazine, 93.1 ± 6.4 for sulfadimidine, 16.1 ± 7.2 for sulfaguanidine, and 108.7 ± 23.7 for trimethoprim.
Authors:Danijela Ašperger, Dragana Mutavdžić, Sandra Babić, Alka Horvat and Marija Kaštelan-Macan
Quantitative determination of the antibiotics enrofloxacin, oxytetracycline, and trimethoprim in aquatic samples is reported. The method involves solid-phase extraction (SPE) and preconcentration of the antibiotics, separation by thin-layer chromatography (TLC) and quantification by video densitometry. TLC separation was performed on HPTLC CN F
s plates with H
-methanol as mobile phase. Spots were detected and quantified at
= 254 nm by videodensitometry. Limits of detection (
) and limits of quantification (
) for TLC determination were calculated. The method was evaluated for spiked water samples. Antibiotics were extracted by solid-phase extraction (SPE) on a polystyrene-divinyl-benzene (SDB) Empore extraction disk. The extraction efficiency was checked by recovery experiments.