Determination of Organic Sulfur Contaminants Using Hollow Fibre-protected Liquid-phase Micro-extraction Coupled with Gas Chromatography
ANALYTICAL AND BIOANALYTICAL CHEMISTRY RESEARCH
Authors: Hojjati, Mohammad; Haghighi, Tarlan
Abstract
A simple and solvent-minimized sample preparation technique based on hollow fibre-protected liquid-phase micro-extraction has been developed for extraction of fifteen organic sulfur compounds (OSCs) from aqueous samples. The analysis of the extracted OSCs was performed by gas chromatography equipped with mass spectrometry and/or flame photometric detectors. 3.3 mu l of organic solvent located in the lumen of hollow fibre was used to extract OSCs from 8 ml of an aqueous sample. Several parameters influencing extraction efficiency such as salt concentration, stirring speed, temperature, sample volume, organic phase volume and extraction time were studied and optimized using super-modified simplex method. Under optimized conditions, including extraction solvent (toluene) extraction time (15 min), salt addition (4% w/v), stirring rate (1200 rpm), sample volume (8 ml SV), organic solvent volume (3.3 mu l) and extraction temperature (35 degrees C), the limits of detection varied from 0.1 to 8.7 mu g l(-1) and 0.7 to 99.4 mu g l(-1) for GC-FPD and GC-MS, respectively. The calibration graphs were linear over three orders of magnitude for most of the studied OSCs. The relative standard deviations for inter- and intra- day analysis were in the range of 5-10%, and the relative recoveries of the analytes from three different real water samples were more than 83%. The results were compared with those obtained using direct single drop micro-extraction and headspace single drop micro-methods. The proposed method is reliable and can be considered useful for routine monitoring of the organic sulfur compounds in surface water samples.
Biological activity, and volatile and phenolic compounds from five Lamiaceae species
FLAVOUR AND FRAGRANCE JOURNAL
Authors: Celik, Gonca; Kilic, Gozde; Kanbolat, Seyda; ozlem Sener, Sila; Karakose, Mustafa; Yayli, Nurettin; Karaoglu, Sengul Alpay
Abstract
Lamiaceae, a family of flowering plants, have been historically used as culinary herbs, shrubs and medicinal plants. With this study, the volatile organic compounds (VOCs) of the five species of the Lamiaceae family (Thymus cilicicus, Clinopodium nepeta L., Nepeta italica L., Thymbra spicata L. and Ziziphora clinopodioides) that grow in Turkey were identified by the SPME/GC-FID/MS method. The five species were screened in order to reveal their antibacterial and antioxidant activities. Phenolic compound analyses of five species were performed by using RP-HPLC with diode array detection. Among the total number of 73 compounds that were identified, alpha-pinene (2.2%-13.8%), beta-pinene (0.3%-25.9%), p-cymene (0.7%-17.9%), gamma-terpinene (0.4%-22.0%), carvacrol (0.1%-40.2%), sabinene (1.2%-34.2%), terpinen-4-ol (0.2%-27.5%), (E)-beta-caryophyllene (0.1%-13.8%) and (E)-beta-farnesene (0.4%-19.7%) were found to be the most plentiful ones. The minimal inhibitory concentration (MIC) values of the methanol extracts of the five species of the Lamiaceae family were investigated, and the results were in the range of 23-959 mu g/mL; the most pronounced antibacterial activities were determined to be against Mycobacterium smegmatis (23-291 mu g/mL). All of the methanol extracts possessed effective antioxidant capacity (IC50: 1.82-28.18 mu mol/L Trolox/g sample) as estimated from the 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical-scavenging assays. Additionally, the effect of phenolics, especially benzoic acid (86.27, 27.85, -, 13.11, 9.59 mg/g extract, respectively), on the biological properties of the methanol extracts of the five species of the Lamiaceae family, was investigated.