According to the Scopus database, using “phthalate” and “GC” as keywords, 758 papers have been found between 1990 and 2014, showing strong and increasing interest in this class of compounds from the scientific community.
A solid-phase extraction (SPE) method was developed for extraction and analysis of six phthalate esters in wine samples using Carbograph 1 sorbent. The SPE procedure allowed efficient recovery of the investigated phthalates ranging between 78% and 105% with a relative standard deviation (RSD) ≤6.5 for an ethanolic phthalic acid ester (PAE) standard solution and between 73-71% and 96-99% with a RSD ≤8.4 for red wine samples spiked with 20 and 50 ng mL(-1) of PAE, respectively. The adsorption isotherms and breakthrough curves for Carbograph 1/water solution were reported. Gas chromatography coupled with an ion-trap mass spectrometer detector (GC/IT-MS) was used for analysis. The instrumental analytical protocol was found to yield a linear calibration in the range 0.01-10.0 μg mL(-1) with R(2) values ≥0.9992. The limits of detection in GC/IT-MS (SIM mode) vary between 0.2 and 14 ng mL(-1) (RSD ≤5.6) whereas the limits of quantification range between 0.5 and 25 ng mL(-1) (RSD ≤5.9); the intra- and inter-day repeatabilities calculated as RSD for wine samples, were between 0.9-7.8 and 1.0-10.5, respectively. The analytical method developed was applied to several commercial wine samples. Furthermore, the investigated methods are simple, reliable, reproducible, and not expensive.
Phthalates (or phthalate esters, PAEs) and bisphenol A (BPA) are widely used in various industries, particularly in the fields of cosmetics and packaging, and they increase the malleability and workability of materials. As a result of their use, some international health organizations have begun to study them. In this study, the authors developed a methodology for the simultaneous determination of dimethyl phthalate (DMP), diethyl phthalate (DEP), diisobutyl phthalate (DiBP); dibutyl phthalate (DBP), bis(2-ethylhexyl) phthalate (DEHP); di-n-octyl-phthalate (DnOP) and bisphenol A (BPA) from drinking and non-potable waters. The extraction of PAEs and BPA was performed using a solvent-based dispersive liquid–liquid microextraction (SB-DLLME) method. The analytical determination was performed using a gas chromatography–ion trap mass spectrometry (GC-IT/MS) analysis. The entire procedure was validated as recoveries were studied according to the volume and the extraction solvent used, pH, and ionic strength. Dynamic linearity ranges and linear equations of all the compounds were experimentally determined as well as the limit of detection (LOD) (1–8 ng mL−1) and the limit of quantification (LOQ) (5–14 ng mL−1), reproducibility, and sensitivity. The method was applied to 15 water samples (mineral water and tap water) for determining PAEs and BPA released from the plastic container. After the release simulation, four PAEs (i.e., DiBP, DBP, DHEP, and DnOP) were determined at very low concentrations (below 1.2 ng mL−1) in two water samples from (sport) bottles.
An analytical method based on solid phase extraction (SPE) with XAD-2 for the enrichment of seven phthalate esters in light alcoholic drinks (alcohol content below 6% alc vol À1 ) and in soft drinks has been developed using gas chromatography coupled with an ion-trap mass spectrometer detector (GC/IT-MS).The instrumental analytical protocol was found to yield a linear calibration in the range of 1-800 ng mL À1 with r 2 values $ 0.912; the limits of detection (LOD) vary between 0.2 pg mL À1 and 20 pg mL À1 , whereas the limits of quantification (LOQ) range between 0.6 pg mL À1 and 41 pg mL À1 with relative standard deviations (RSDs) of #4.8 and #5.5, respectively. The interday precision ranges between 3.6 and 6.3%, whereas the intraday accuracy is between 7.9 and 12.4%. This simple, reliable, reproducible and low-cost analytical method has been applied to several commercial light alcoholic samples such as beers and soft drinks. DEP (0.1-1.0 ng mL À1 ), DiBP (0.2-2.5 ng mL À1 ), DBP (1.9-4.4 ng mL À1 ), BBP (0.08-0.8 ng mL À1 ), DEHP (3.6-101 ng mL À1 ) are present in every sample analyzed, whereas DMP (1.9 ng mL À1 ) and iBcEP (0.08 ng mL À1 ) are found only in one sample of beer.
In this paper, an analytical protocol was developed for the simultaneous determination of phthalates (di-methyl phthalate DMP, di-ethyl phthalate DEP, di-isobutyl phthalate DiBP, di-n-butyl phthalate DBP, bis-(2-ethylhexyl) phthalate DEHP, di-n-octyl phthalate DNOP) and bisphenol A (BPA). The extraction technique used was the ultrasound vortex assisted dispersive liquid–liquid microextraction (UVA-DLLME). The method involves analyte extraction using 75 µL of benzene and subsequent analysis by gas chromatography combined with ion trap mass spectrometry (GC-IT/MS). The method is sensitive, reliable, and reproducible with a limit of detection (LOD) below 13 ng g−1 and limit of quantification (LOQ) below 22 ng g−1 and the intra- and inter-day errors below 7.2 and 9.3, respectively. The method developed and validated was applied to six honey samples (i.e., four single-use commercial ones and two home-made ones. Some phthalates were found in the samples at concentrations below the specific migration limits (SMLs). Furthermore, the commercial samples were subjected to two different thermal stresses (24 h and 48 h at 40 °C) for evidence of the release of plastic from the containers. An increase in the phthalate concentrations was observed, especially during the first phase of the shock, but the levels were still within the limits of the regulations.
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