Fast Chromatographic Separation of Plasticizers on Thin Layers of an Inorganic Ion-Exchanger: Quantitative Determination of Di(2-ethylhexyl)phthalate (original) (raw)
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Revisiting analysis of phthalate plasticizers concentration in poly(vinyl chloride)
Journal of Vinyl & Additive Technology, 2014
The method of the efficient analysis of di(2-diethylhexyl) phthalate, tri(2-ethylhexyl) trimellitate, di(2-ethylhexyl) terephthalate, and other phthalate plasticizers concentrations in plasticized poly(vinyl chloride) (PVC) was developed. The method is based on quantitative dissolution of the PVC sample in methyl ethyl ketone with the consequent precipitation of PVC with hexane and concentration of phthalate in an organic layer. A capillary column-based gas chromatographic technique for phthalates separation and quantification was developed and used in conjunction with the PVC and phthalates dissolution technique. The developed method of phthalate plasticizers analysis proved to be relatively fast, reproducible, and straightforward. J.
TrAC Trends in Analytical Chemistry, 2017
Phthalate esters are widely used in production of polymer materials (approximately five millions tones annually), therefore they occur in final products (food packages, cosmetics, vinyl products) and undergo emission into the environment. Phthalates have a negative impact on living organisms (e.g. disturbing function of endocrine/reproductive systems) and some of them are restricted (REACH, U.S. CPSC). Investigating their occurrence in the environment, especially indoor/outdoor air, is very important. After several improvements in recent years (e.g. heating/cooling efficiency), sorption of analytes on sorbent followed by thermal desorption (TD) and GC-MS seems to be the best suited protocol to determine phthalates in air samples. It is a straightforward technique, without dilution of samples and use of toxic solvents. However, it cannot be applied to compounds which are thermally unstable and have a low vapor pressure. Overall, TD it is one of the best available technique for desorption of phthalates from a sorbent.
Solid-phase microextraction of phthalates from water
Journal of Chromatography A, 2001
Solid-phase microextraction (SPME) with six different non-polar and polar fibres was used to extract seven phthalate esters from water samples for analysis by gas chromatography-mass spectrometry. With regard to extraction efficiency and repeatability of the extractions, the 70-mm Carbowax-divinylbenzene fibre was especially suitable for the selected phthalates 21 21
Microextraction methods for the determination of phthalate esters in liquid samples: A review
Journal of Separation Science, 2015
1,2-Benzenedicarboxylic acid esters, commonly referred to as phthalate esters, form a group of compounds that are mainly used as plasticizers in polymers. Because phthalate esters are not chemically bound to the plastics, they can be released easily from products and migrate into the food or water that comes into direct contact. Due to their widespread use, they are considered as ubiquitous environmental pollutants. Phthalate esters are regarded as endocrine disrupting compounds by means of their carcinogenic effect. Phthalate esters can be analyzed by gas chromatography or highperformance liquid chromatography, however, their sensitivity and selectivity limit their direct use for determination of PEs at very low level of concentrations exist in environmental samples with complex matrices. Therefore a sample pretreatment prior to their analysis is necessary. In this review, the historical development and overview of sample preparation methodologies have briefly been discussed and a comprehensive application of the these methods in combination with different analytical techniques for preconcentration and determination of phthalate esters in various matrices have been summarized. Finally, a critical comparison of the different approaches in terms of enrichment factors achieved, extraction efficiency, precision, selectivity and simplicity of operation is provided.
Analytical Sciences, 2018
In this study, a solid-phase extraction-type collection device, with styrene-divinylbenzene polymer particles (Sunpak-H) as the adsorbent, was used for the quantitative determination of phthalate esters in air samples. The collection and elution recoveries of eight volatile phthalate esters, i.e., dimethyl phthalate, diethyl phthalate, dipropyl phthalate, diisobutyl phthalate, dibutyl phthalate, butyl-benzyl phthalate, di(2-ethylhexyl) phthalate, and dioctyl phthalate, were quantitatively evaluated. All analytes were collected using the device up to a sampling volume of 10000 L at a sampling temperature of 35 C without breakthrough. During air collection, moisture was not trapped on the adsorbent. The collected analytes were completely eluted from the device by passing 3 mL of acetone. The eluted solvent was injected into a gas chromatography-mass spectrometry system after the eluted solvent was concentrated, if necessary. After washing the adsorbent using acetone, the device could be reused more than 50 times. The limit of quantification for the analytes was less than 1 ng L-1 in air at a sampling volume of 600 L with solvent concentration. This device was successfully applied for the quantitative determination of phthalate esters in real air samples, including indoor and in-car air.
Migration of phthalate-based plasticizers from PVC and non-PVC containers and medical devices
Journal of the Brazilian Chemical Society, 2012
A presença de cinco plastificantes derivados de ftalatos em equipamentos para administração intravenosa de soluções e em hemodialisadores (HD), que são feitos tanto de policloreto de vinila (PVC) quanto de outros materiais poliméricos, foi investigada. Destes ftalatos, o único autorizado por agências reguladoras é o di-(2-etilhexil) ftalato (DEHP) em equipamentos de PVC. A determinação foi feita por chromatografia líquida de alta eficiência (HPLC) com detecção UV. Os resultados mostraram que as bolsas para infusão que são feitas tanto de PVC quanto de etil vinil acetato (EVA) contêm apenas DEHP. Entretanto, as mangueiras dos equipos de infusão e dos HD, bem como as fibras capilares dos HD feitas de celulose, contêm não só DEHP, mas também ftalato de dibutila (DBP). Todos os cinco ftalatos investigados foram encontrados nos capilares dos HD feitos de polisulfona. A migração de DEHP para soluções (aminoácidos, glicose e salina) armazenadas em bolsas ocorreu com taxas diferentes para os dois polímeros. Enquanto que para as bolsas de PVC o DEHP foi encontrado em soluções já nos primeiros dias de contato, para as bolsas de EVA a migração iniciou após aproximadamente 6 meses de armazenamento. Como os dispositivos analisados, com exceção das bolsas, contém, além do DHEP, outros ftalatos, o risco posto aos pacientes deve ser motivo de preocupação. The presence of five plasticizer phthalates in bags and sets for intravenous administration and hemodialyzers (HD), which are made of polyvinyl chloride (PVC) and of other polymeric materials, was investigated. Di-(2-ethylhexyl) phthalate (DEHP) in PVC is the only authorized phthalate by regulatory agencies. Phthalate determination was carried out by high resolution liquid chromatograph (HPLC) with UV detection. The results showed that the infusion bags that are made of both PVC and ethylene vinyl acetate (EVA) contained only DEHP. In contrast, the tubing of infusion sets and of HD (as well as the cellulose capillaries of HD) contained not only DEHP but also dibutyl phthalate (DBP). Moreover, all five investigated phthalates were found in HD polysulfone capillaries. Migration of DEHP into the stored solutions (amino acids, glucose and saline) in bags occurred at different rates from one polymer to another. While DEHP from PVC bags was found in solutions within the first days of contact, the migration from EVA bags started only after approximately 6 months of solution storage. Since PVC and non-PVC devices (as well as capillaries of HD sets) contain DEHP and other phthalate-based plasticizers, the extent of the risk that they pose to patients remains a matter of concern.
BPB Reports, 2019
Phthalic acid esters (PAEs) are the most abundantly produced, and the most widely used plasticizers in the world. PAEs are contained in many kinds of industrial products used in indoor environments, such as polyvinyl chloride covering for floors and walls, outer casings of computer monitors and TV sets, synthetic-leather products, and electrical cables. PAEs are released from these products into the indoor environment, existing as ubiquitous pollutants. Consequently, house dust is identified as an important source of human exposure to PAEs, in addition to food and drinking water. 1-3) Although PAEs are substances with low acute and chronic toxicity, they are often mentioned as suspected endocrine disruptors, mainly because of their testicular toxicity. 4-6) Since 2000-2001, the Japan Ministry of Health, Labor, and Welfare (MHLW) has set indoor guidelines for din -butyl phthalate (DBP) and di(2-ethylhexyl) phthalate (DEHP) based on their reproductive toxicity. Recently, the guidelines values were made more stringent, decreasing the permissible values from 220 μg/m 3 to 17 μg/m 3 , and from 120 μg/m 3 to 100 μg/m 3 , for DBP and DEHP, respectively. 7) MHLW also set two different standard sampling/analytical protocols for DBP and DEHP in indoor air in 2001: solid phase adsorption followed by solvent extraction or thermal desorption, and determination by a combination of gas chromatography (GC) and mass spectrometry (MS). 8) Another method is described in ISO 16000-33 (2017), 9) which concerns determination of PAEs in indoor air using GC-MS. In the ISO methods, 9) Florisil TM (Merck) is used as the adsorbent for the solvent extraction methods. In contrast, three other kinds of adsorbents-activated carbon, octadecyl silica (ODS), and styrene-divinylbenzene (SDB) copolymer-are recommended in Japanese standard protocol. 8) Florisil TM preparation, according to ISO 16000-33, is very time-consuming because it requires 6 h of heating at 800°C and 45 min of mixing after addition of water. On the other hand, preparation of each adsorbent according to the Japanese standard protocol is much easier and
Analytica Chimica Acta, 2012
A novel microextraction technique, air-assisted liquid-liquid microextraction (AALLME), which is a new version of dispersive liquid-liquid microextraction (DLLME) method has been developed for extraction and preconcentration of phthalate esters, dimethyl phthalate (DMP), diethyl phthalate (DEP), di-isobutyl phthalate (DIBP), din -butyl phthalate (DNBP), and di-2-ethylhexyl phthalate (DEHP), from aqueous samples prior to gas chromatography-flame ionization detection (GC-FID) analysis. In this method, much less volume of an organic solvent is used as extraction solvent in the absence of a disperser solvent. Fine organic droplets were formed by sucking and injecting of the mixture of aqueous sample solution and extraction solvent with a syringe for several times in a conical test tube. After extraction, phase separation was performed by centrifugation and the enriched analytes in the sedimented phase were determined by GC-FID. Under the optimum extraction conditions, the method showed low limits of detection and quantification between 0.12-1.15 and 0.85-4 ng mL −1 , respectively. Enrichment factors (EFs) and extraction recoveries (ERs) were in the ranges of 889-1022 and 89-102%, respectively. The relative standard deviations (RSDs) for the extraction of 100 ng mL −1 and 500 ng mL −1 of each phthalate ester were less than 4% for intra-day (n = 6) and inter-days (n = 4) precision. Finally some aqueous samples were successfully analyzed using the proposed method and three analytes, DIBP, DNBP and DEHP, were determined in them at ng mL −1 level.
The Effect of Temperature on the Migration of Phthalate Plasticizers from Plastic Sachet into Water
Phthalates are compounds used principally as plasticizers, to impact flexibility, workability and durability to polymers used to contain consumer products such as water etc. These phthalates are not chemically bound to polymers; hence they are easily released and migrate into the containing consumer product. The leaching may take place in harsh conditions such as under the sun among others. Hence the ―PA‖ sachet water was used as a case study. PA sachet water was subjected to different room temperatures; 25 o C, 45 o C, and 65 o C for 8 hours each day for 5 days. Liquid-liquid extraction of the phthalates from the different samples of water was carried out using dichloromethane. These samples were analyzed for benzyl butyl phthalate (BBP), di-butyl phthalate (DBP), di-2-ethylbutyl phthalate (DEHP), di (n-octyl) phthalates, DNOP, diisononyl phthalates (DINP using UV-VIS spectroscopy and GC-MS. The results showed that there was no leaching of phthalates into the water when the water was subjected to room temperature up to 65 o C.
2018
Phthalates are used as plasticizers in the manufacturing of plastics to increase their flexibility. Phthalates are endocrine disruptors and given their potential toxicity and widespread use, many countries have implemented strict regulations on their usage. A rapid gas chromatography time-of-flight mass spectrometry (GC-TOFMS) analytical method was developed for the determination and quantification of six regulated phthalates. Three extraction methods were investigated including two standard techniques; a dissolution method and a Soxhlet method (EN 14372:2004E). These two standard methods were compared to a simpler ultrasonic extraction method. The recoveries and accuracy of the measurements were assessed by analyzing a polypropylene (PP) certified reference material (matrix CRM) and spiked polyvinyl chloride (PVC) samples. The ultrasonic extraction method resulted in better recoveries (>80%) when compared to the dissolution method. The results obtained from extracting the CRM us...