scholarly journals Evaluation of method for phthalate extraction from milk related to milk dilution ratio

2015 ◽  
Vol 80 (8) ◽  
pp. 983-996 ◽  
Author(s):  
Danica Milojkovic ◽  
Darko Andjelkovic ◽  
Gordana Kocic ◽  
Tatjana Andjelkovic
Keyword(s):  
Salt Effect ◽  
Gas Chromatography Mass Spectrometry ◽  
Extraction Techniques ◽  
Selected Ion Monitoring ◽  
Benzyl Butyl Phthalate ◽  
Liquid Liquid Extraction ◽  
Solvent Type ◽  
Butyl Phthalate ◽  
Ethylhexyl Phthalate

Liquid-liquid extraction techniques were compared coupled with gas chromatography-mass spectrometry (GC-MS), for the extraction and the determination of four phthalates: dimethyl phthalate (DMP), di-n-butyl phthalate (DBP), benzyl butyl phthalate (BBP) and di-(2-ethylhexyl) phthalate (DEHP) in six different kinds of milk-based samples. Extraction factors: sample preparation, organic solvent type and volume, salt effect, agitation and the extraction time were optimized. The ion of base peaks (m/z 149 for DBP, BBP and DEHP and m/z 163 for DMP) for investigated phthalates were selected for the screening studies. The acquisition was performed at the selected ion monitoring mode. The MSD response for GC-MS phthalate calibration standards was linear between 0.25 and 2.50 ?g mL-1 with calculated LODs between 0.01 ?g mL-1 to 0.04 ?g mL-1 and LOQs of 0.05 ?g mL-1 to 0.12 ?g mL-1, while repeatability was between 1.7 % to 4.9 % RSD. The study demonstrated an increase of the recovery of less polar phthalates in matrix milk standards by matrix dilution. Recovery for hydrophilic phthalates, like DMP, was not changed by matrix dilution and it was continuously low for the investigated method. Two spiking levels were tested for influence of matrix dilution on phthalate recovery, showed the same trend.

scholarly journals Transfer of phthalates from c-polyvinyl chloride and cross-linked polyethylene pipe (PEX-b) into drinking water

2016 ◽  
Vol 17 (2) ◽  
pp. 588-596
Author(s):  
Derek R. Faust ◽  
Kimberly J. Wooten ◽  
Philip N. Smith
Keyword(s):  
Drinking Water ◽  
Polyvinyl Chloride ◽  
Cold Water ◽  
Endocrine Disrupting Compounds ◽  
Gas Chromatography Mass Spectrometry ◽  
Domestic Water ◽  
Benzyl Butyl Phthalate ◽  
Endocrine Disrupting ◽  
Butyl Phthalate ◽  
Ethylhexyl Phthalate

Several different materials have been used for production of domestic water pipes throughout history. In recent years, the use of cross-linked polyethylene (PEX) pipe has increased dramatically, yet the potential for leaching of phthalates, which are endocrine disrupting compounds associated with adverse reproductive effects in humans, has not been examined. In this study, the potential of chlorinated polyvinyl chloride (cPVC) and red, blue, and heat PEX piping to leach phthalates into static hot and cold water after 2, 8, and 48 hours was evaluated. Concentrations of six phthalates, dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), benzyl-butyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), and di(n-octyl) phthalate (DNOP), were determined by gas chromatography-mass spectrometry. Pipe type (F3,71 = 15.6, P = 0.001) contributed significantly to phthalate concentrations in water, while temperature (F4,71 = 1.74, P = 0.106) and time (F4,71 = 1.02, P = 0.427) were not significant factors. Significantly higher concentrations of DEP, DBP, and BBP were observed in cPVC pipe (<method detection limits (MDL) to 466 ng L−1, 252–4,219 ng L−1, 473–18,400 ng L−1, respectively) compared to blue PEX (T2 = 12.2, P < 0.001; <MDL, <MDL − 140 ng L−1, <MDL − 459 ng L−1, respectively), red PEX (T2 = 19.3, P < 0.001; <MDL, <MDL − 188 ng L−1, <MDL − 881 ng L−1, respectively), and heat PEX (T2 = 19.9, P < 0.001; <MDL, <MDL − 162 ng L−1, <MDL − 169 ng L−1, respectively). Phthalate exposure from drinking water via cPVC or PEX is low when compared to other dietary sources. Nonetheless, a shift from cPVC to PEX pipes in households would decrease potential exposure to phthalates.

scholarly journals Determination of Organic Micropollutants in Water Using Gas Chromatography-Mass Spectrometry

Proceedings ◽  
2019 ◽  
Vol 16 (1) ◽  
pp. 57
Author(s):  
Marek Król ◽  
Mariusz Dudziak
Keyword(s):  
Mass Spectrometry ◽  
Detection Sensitivity ◽  
Gas Chromatography Mass Spectrometry ◽  
Determination Method ◽  
Organic Micropollutants ◽  
Selected Ion Monitoring ◽  
Detection Mode ◽  
Full Scan ◽  
Ethylhexyl Phthalate

In this study a determination method has been developed for seven different micropollutants, that were selected to represent different compound groups. The selected compounds were: 4-nonylphenol (4-NP), 4-octylphenol (4-OP), anthracene (Ant), alachlor (Ac), heptachlor (Hc), heptachlor epoxide (Hce), and bis(2-ethylhexyl)phthalate (DEHP). Chromatographic separation and mass spectrometer detection conditions were optimized to achieve the best micropollutants separation and the best detection sensitivity. A calibration curves were created at different calibration levels suited of each type of detection mode (Full Scan and Selected Ion Monitoring) and limits of detection (LOD) and limits of quantification (LOQ) were calculated. Furthermore, recovery values were determined for each compound in spiked water samples at levels equal to 10%, 50%, and 90% of the calibration curve range and compared to other studies in which similar methods of determination were used.

scholarly journals Application of Bar Adsorptive Microextraction for the Determination of Levels of Tricyclic Antidepressants in Urine Samples

Molecules ◽  
2021 ◽  
Vol 26 (11) ◽  
pp. 3101
Author(s):  
Mariana N. Oliveira ◽  
Oriana C. Gonçalves ◽  
Samir M. Ahmad ◽  
Jaderson K. Schneider ◽  
Laiza C. Krause ◽  
...  
Keyword(s):  
Tricyclic Antidepressants ◽  
Matrix Effects ◽  
Activated Carbons ◽  
Process Efficiency ◽  
Gas Chromatography Mass Spectrometry ◽  
Selected Ion Monitoring ◽  
Experimental Conditions ◽  
Analytical Methodology ◽  
Low Efficiency

This work entailed the development, optimization, validation, and application of a novel analytical approach, using the bar adsorptive microextraction technique (BAμE), for the determination of the six most common tricyclic antidepressants (TCAs; amitriptyline, mianserin, trimipramine, imipramine, mirtazapine and dosulepin) in urine matrices. To achieve this goal, we employed, for the first time, new generation microextraction devices coated with convenient sorbent phases, polymers and novel activated carbons prepared from biomaterial waste, in combination with large-volume-injection gas chromatography-mass spectrometry operating in selected-ion monitoring mode (LVI-GC-MS(SIM)). Preliminary assays on sorbent coatings, showed that the polymeric phases present a much more effective performance, as the tested biosorbents exhibited low efficiency for application in microextraction techniques. By using BAμE coated with C18 polymer, under optimized experimental conditions, the detection limits achieved for the six TCAs ranged from 0.2 to 1.6 μg L−1 and, weighted linear regressions resulted in remarkable linearity (r2 > 0.9960) between 10.0 and 1000.0 μg L−1. The developed analytical methodology (BAμE(C18)/LVI-GC-MS(SIM)) provided suitable matrix effects (90.2–112.9%, RSD ≤ 13.9%), high recovery yields (92.3–111.5%, RSD ≤ 12.3%) and a remarkable overall process efficiency (ranging from 84.9% to 124.3%, RSD ≤ 13.9%). The developed and validated methodology was successfully applied for screening the six TCAs in real urine matrices. The proposed analytical methodology proved to be an eco-user-friendly approach to monitor trace levels of TCAs in complex urine matrices and an outstanding analytical alternative in comparison with other microextraction-based techniques.

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