Analytical Scheme for Simultaneous Determination of Phthalates and Bisphenol A in Honey Samples Based on Dispersive Liquid–Liquid Microextraction Followed by GC-IT/MS. Effect of the Thermal Stress on PAE/BP-A Levels

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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A Method Validation for Simultaneous Determination of Phthalates and Bisphenol A Released from Plastic Water Containers

Applied Sciences ◽

10.3390/app9142945 ◽

2019 ◽

Vol 9 (14) ◽

pp. 2945 ◽

Cited By ~ 7

Author(s):

Ivan Notardonato ◽

Carmela Protano ◽

Matteo Vitali ◽

Badal Bhattacharya ◽

Pasquale Avino

Keyword(s):

Bisphenol A ◽

Simultaneous Determination ◽

Water Samples ◽

Limit Of Detection ◽

Tap Water ◽

Phthalate Esters ◽

Analytical Determination ◽

Limit Of Quantification ◽

Plastic Container

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.

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Spectrophotometric Determination of Zirconium by Dispersive Liquid-Liquid Microextraction based on Solidification of Floating Organic Droplets

Asian Journal of Chemistry ◽

10.14233/ajchem.2020.22863 ◽

2020 ◽

Vol 32 (12) ◽

pp. 3191-3196

Author(s):

Intizam Ahmadov

Keyword(s):

Spectrophotometric Determination ◽

Limit Of Detection ◽

Ph Effect ◽

Ionic Surfactant ◽

Ligand Effect ◽

Limit Of Quantification ◽

Relative Standard ◽

Dispersive Liquid Liquid Microextraction ◽

Liquid Microextraction

In this study, a new method was developed for the spectrophotometric determination of zirconium by the procedure of dispersive liquid-liquid microextraction based on the solidification of floating organic droplets (DLLME-SFO). o-Nitrobenzene-azopyrocatechol (o-NBAP) and non-ionic surfactant (OP-10) were used in the complex formation. At the first stage, a separation and solidification processes were carried out, after which the solidified samples were examined by spectrophotometric method. The effect of various parameters viz. pH effect, ion resistance, ligand effect, volume and type of extraction and dispersion solution, extraction time and temperature effect were studied. The results of the experiment were optimized with design programs. The calibration curve was linear ranging from 0.5 to70 μg L-1, with a correlation coefficient of 0.998. The limit of detection (LOD) is 0.12 μg L-1, the limit of quantification (LOQ) is 0.40 μg L-1 and the relative standard deviation (RSD) at 60 μg L-1 is 1.6% (n=6). This method was also applied to determine zirconium in various water samples. The obtained reextraction amount was 98-110%.

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