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Holger M Koch - One of the best experts on this subject based on the ideXlab platform.
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The MAK‐Collection for Occupational Health and Safety - Phthalates, long‐chain (diisononyl Phthalate, di‐n‐decyl Phthalate, Diisodecyl Phthalate, diundecyl Phthalate and didodecyl Phthalate) [Air Monitoring Methods, 2014]
The MAK Collection for Occupational Health and Safety, 2016Co-Authors: J.‐u. Hahn, Holger M Koch, K H Pannwitz, R Hebisch, T H Brock, H. Assenmacher‐maiworm, A HartwigAbstract:This analytical method is a validated measurement procedure for the determination of long-chain Phthalates such as diisononyl Phthalate, di-n-decyl Phthalate, Diisodecyl Phthalate, diundecyl Phthalate and didodecyl Phthalate present in the workplace air in the gaseous and particulate state. Sampling is performed by drawing a defined volume of air through a cellulose acetate filter located in the sampling head with an adsorption tube filled with silica gel connected downstream using a suitable pump. The flow rate is set to 1 L/min with a recommended air sample volume of 60 or 120 litres after 1 or 2 hours. The collected Phthalates are desorbed with methanol and then analysed by means of liquid chromatography using a UV detector (HPLC-UV). Quantitative determination is based on calibration functions obtained by means of multiple-point calibrations using an internal standard. The limits of quantification (LOQs) for a Phthalate are between 0.003 and 0.26 mg/m3 for an air sample volume of 240 litres. The expanded uncertainty for these parameters is between 16 and 22%, depending on the Phthalate and concentration. Joint Publication of the Analytical Subcommittee of the Chemistry Board of Experts of the Expert Committee Raw Materials and Chemical Industry of the German Social Accident Insurance and the Working Group “Air Monitoring Methods” of the Permanent Senate Commission of the DFG for the Investigation of Health Hazards of Chemical Compounds in the Work Area. Keywords: long-chain Phthalates; diisononyl Phthalate; di-n-decyl Phthalate; Diisodecyl Phthalate; diundecyl Phthalate; didodecyl Phthalate; air analysis; workplace measurement; hazardous substances; workplace monitoring; measurement method; measuring procedure; cellulose acetate filter; silica gel tube; liquid chromatography; HPLC
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Phthalates long chain diisononyl Phthalate di n decyl Phthalate Diisodecyl Phthalate diundecyl Phthalate and didodecyl Phthalate air monitoring methods 2014
The MAK Collection for Occupational Health and Safety, 2016Co-Authors: J U Hahn, Holger M Koch, H Assenmachermaiworm, K H Pannwitz, R Hebisch, T H Brock, A HartwigAbstract:This analytical method is a validated measurement procedure for the determination of long-chain Phthalates such as diisononyl Phthalate, di-n-decyl Phthalate, Diisodecyl Phthalate, diundecyl Phthalate and didodecyl Phthalate present in the workplace air in the gaseous and particulate state. Sampling is performed by drawing a defined volume of air through a cellulose acetate filter located in the sampling head with an adsorption tube filled with silica gel connected downstream using a suitable pump. The flow rate is set to 1 L/min with a recommended air sample volume of 60 or 120 litres after 1 or 2 hours. The collected Phthalates are desorbed with methanol and then analysed by means of liquid chromatography using a UV detector (HPLC-UV). Quantitative determination is based on calibration functions obtained by means of multiple-point calibrations using an internal standard. The limits of quantification (LOQs) for a Phthalate are between 0.003 and 0.26 mg/m3 for an air sample volume of 240 litres. The expanded uncertainty for these parameters is between 16 and 22%, depending on the Phthalate and concentration. Joint Publication of the Analytical Subcommittee of the Chemistry Board of Experts of the Expert Committee Raw Materials and Chemical Industry of the German Social Accident Insurance and the Working Group “Air Monitoring Methods” of the Permanent Senate Commission of the DFG for the Investigation of Health Hazards of Chemical Compounds in the Work Area. Keywords: long-chain Phthalates; diisononyl Phthalate; di-n-decyl Phthalate; Diisodecyl Phthalate; diundecyl Phthalate; didodecyl Phthalate; air analysis; workplace measurement; hazardous substances; workplace monitoring; measurement method; measuring procedure; cellulose acetate filter; silica gel tube; liquid chromatography; HPLC
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Phthalate exposure during cold plastisol application a human biomonitoring study
Toxicology Letters, 2012Co-Authors: Holger M Koch, Andreas Haller, Tobias Weis, Heiko Udo Käfferlein, Joachim Stork, Thomas BruningAbstract:Abstract The Phthalates DEHP (Diethylhexyl Phthalate), DiNP (Diisononyl Phthalate) and DiDP (Diisodecyl Phthalate) are constituents of plastisols. We sought to obtain first data on occupational exposures to the above Phthalates by analyzing their metabolites in pre- and post-shift urine samples from 5 workers in a car manufacturing plant engaged in seam sealing with a DINP based plastisol. Pre-shift samples were collected after a work-free period of at least 2 days. As a comparison group we investigated 10 employees from the same plant. The comparison group had Phthalate exposures in the range of the general German population. All plastisol workers had post shift values of DiNP and DiDP metabolites that were approx. 20-times higher, and pre-shift values that were approx. 5–10 times higher than those of the general background exposure. Post-shift values of DiNP metabolites were (median [maximum]: OH-MiNP: 117 [442] μg/L; oxo-MiNP: 44.3 [175] μg/L; carboxy-MiNP: 57.8 [286] μg/L), pre shift values were (OH-MiNP: 26 [164] μg/L; oxo-MiNP 12.9 [68.6] μg/L; carboxy-MiNP: 32.3 [103] μg/L), compared to the comparison group (OH-MiNP: 6.2 [33] μg/L; oxo-MiNP: 2.8 [16] μg/L; carboxy-MiNP: 6.5 [31] μg/L). DiDP values were generally lower. Regarding DEHP we found no significant work related exposure. The dermal exposure route might play an important role for Phthalates in plastisols, with possible influences on distribution and elimination kinetics and therefore data interpretation.
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Phthalate exposure during cold plastisol application—a human biomonitoring study
Toxicology Letters, 2011Co-Authors: Holger M Koch, Andreas Haller, Heiko Udo Käfferlein, Joachim Stork, Tobias Weiß, Thomas BruningAbstract:Abstract The Phthalates DEHP (Diethylhexyl Phthalate), DiNP (Diisononyl Phthalate) and DiDP (Diisodecyl Phthalate) are constituents of plastisols. We sought to obtain first data on occupational exposures to the above Phthalates by analyzing their metabolites in pre- and post-shift urine samples from 5 workers in a car manufacturing plant engaged in seam sealing with a DINP based plastisol. Pre-shift samples were collected after a work-free period of at least 2 days. As a comparison group we investigated 10 employees from the same plant. The comparison group had Phthalate exposures in the range of the general German population. All plastisol workers had post shift values of DiNP and DiDP metabolites that were approx. 20-times higher, and pre-shift values that were approx. 5–10 times higher than those of the general background exposure. Post-shift values of DiNP metabolites were (median [maximum]: OH-MiNP: 117 [442] μg/L; oxo-MiNP: 44.3 [175] μg/L; carboxy-MiNP: 57.8 [286] μg/L), pre shift values were (OH-MiNP: 26 [164] μg/L; oxo-MiNP 12.9 [68.6] μg/L; carboxy-MiNP: 32.3 [103] μg/L), compared to the comparison group (OH-MiNP: 6.2 [33] μg/L; oxo-MiNP: 2.8 [16] μg/L; carboxy-MiNP: 6.5 [31] μg/L). DiDP values were generally lower. Regarding DEHP we found no significant work related exposure. The dermal exposure route might play an important role for Phthalates in plastisols, with possible influences on distribution and elimination kinetics and therefore data interpretation.
Bárbara Socas-rodríguez - One of the best experts on this subject based on the ideXlab platform.
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A green and simple procedure based on deep eutectic solvents for the extraction of Phthalates from beverages
Food Chemistry, 2019Co-Authors: Álvaro Santana-mayor, Bárbara Socas-rodríguez, Ruth Rodríguez-ramos, Miguel Ángel Rodríguez-delgadoAbstract:Abstract In this work, a green, inexpensive, simple and fast deep eutectic solvent (DES)-based dispersive liquid–liquid microextraction was evaluated, for the first time, for the extraction of Phthalates (i.e. benzylbutyl Phthalate, diisobutyl Phthalate, diisopentyl Phthalate, di-n-pentyl Phthalate, di-(2-ethylhexyl) Phthalate, di-n-octyl Phthalate, diisononyl Phthalate, Diisodecyl Phthalate) from different beverages. Separation and determination were achieved by high performance liquid chromatography-diode-array detection while confirmation was carried out by tandem mass spectrometry. The main factors affecting the extraction such as type and volume of DES and emulsifier, pH and ionic strength, were optimised. Choline chloride:phenol-based DES showed the best results. The methodology was validated for tea, apple-based beverage and pineapple juice. Recovery values ranged from 84 to 120% with relative standard deviation values lower than 11%. Limits of detection of the method were in the range 5.1–14.2 µg L−1 for tea, 5.3–17.8 µg L−1 for apple beverages and 5.9–15.6 µg L−1 for pineapple juices.
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Determination of phthalic acid esters in different baby food samples by gas chromatography tandem mass spectrometry
Analytical and Bioanalytical Chemistry, 2018Co-Authors: Bárbara Socas-rodríguez, Javier González-sálamo, Álvaro Santana-mayor, Antonio V. Herrera-herrera, Javier Hernández-borgesAbstract:In this work, a new method has been developed for the determination of 14 phthalic acid esters (i.e., benzylbutyl Phthalate (BBP), bis-2- n -butoxyethyl Phthalate (DBEP), dibutyl Phthalate (DBP), dicyclohexyl Phthalate (DCHP), bis-2-ethoxyethyl Phthalate (DEEP), diethyl Phthalate (DEP), Diisodecyl Phthalate (DIDP), diisononyl Phthalate (DINP), bis-isopentyl Phthalate (DIPP), bis (2-methoxyethyl) Phthalate (DMEP), dimethyl Phthalate (DMP), di- n -octyl Phthalate (DNOP), bis- n -pentyl Phthalate (DNPP), dipropyl Phthalate (DPP)) and one adipate (bis (2-ethylhexyl) adipate (DEHA)) in different baby foods. Separation was carried out by gas chromatography triple quadrupole tandem mass spectrometry while the previous extraction of the samples was carried out using the QuEChERS method. The methodology was validated for four baby food samples (two fruit compotes of different compositions and two meat and fish purees with vegetables) using dibutyl Phthalate-3,4,5,6-d_4 (DBP-d_4) as internal standard. Determination coefficients ( R ^2) of matrix-matched calibration curves were above 0.9922 in all cases while relative recovery values ranged between 70 and 120%, with relative standard deviation values below 19%. The limits of quantification of the method ranged between 0.03 and 1.11 μg/kg. Finally, the analysis of commercially available samples was carried out finding the presence of BBP, DEHA, DEP, DIDP, and DPP in some of the studied samples.
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Reduced graphene oxide-coated magnetic-nanoparticles as sorbent for the determination of Phthalates in environmental samples by micro-dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography tandem mass spectrometry
Journal of Chromatography A, 2018Co-Authors: Álvaro Santana-mayor, Bárbara Socas-rodríguez, María M. Afonso, José Antonio Palenzuela-lópez, Miguel Ángel Rodríguez-delgadoAbstract:Abstract In this work, the suitability of Fe 3 O 4 nanoparticles coated with reduced-graphene oxide as sorbent was evaluated for the extraction of a group of fourteen phthalic acid esters (i.e. benzylbutyl Phthalate (BBP), bis-2- n -butoxyethyl Phthalate (DBEP), dibutyl Phthalate (DBP), diisobutyl Phthalate (DIBP), dicyclohexyl Phthalate (DCHP), bis-2-ethoxyethyl Phthalate (DEEP), Diisodecyl Phthalate (DIDP), diisononyl Phthalate (DINP), bis-isopentyl Phthalate (DIPP), bis-(2-methoxyethyl) Phthalate (DMEP), dimethyl Phthalate (DMP), di- n -octyl Phthalate (DNOP), bis- n -pentyl Phthalate (DNPP), dipropyl Phthalate (DPP)) from environmental samples. Extraction was carried out using magnetic-micro dispersive solid-phase extraction while separation, identification and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The methodology was validated for three different types of water samples using dibutyl Phthalate-3,4,5,6-d 4 as internal standard for all of them. Recovery values ranged from 70 to 120% for the three matrices with relative standard deviation values lower than 20%. Limits of quantification of the method achieved were in the range 6–178 ng/L for all samples and analytes. The methodology was applied for the evaluation of real samples finding the presence of DMP, DPP, BBP, DIBP and DBP in some of the analysed matrices.
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Determination of phthalic acid esters in water samples using core-shell poly(dopamine) magnetic nanoparticles and gas chromatography tandem mass spectrometry
Journal of Chromatography A, 2017Co-Authors: Javier González-sálamo, Bárbara Socas-rodríguez, Javier Hernández-borges, Miguel Ángel Rodríguez-delgadoAbstract:In this work, the first application of core-shell poly(dopamine) magnetic nanoparticles as sorbent for the extraction of a group of eleven phthalic acid esters of interest (i.e. diethyl Phthalate (DEP), dipropyl Phthalate (DPP), dibutyl Phthalate (DBP), bis-isopentyl Phthalate (DIPP), bis-n-pentyl Phthalate (DNPP), benzylbutyl Phthalate (BBP), dicyclohexyl Phthalate (DCHP), di-(2-ethylhexyl) Phthalate (DEHP), di-n-octyl Phthalate (DNOP), diisononyl Phthalate (DINP) and Diisodecyl Phthalate (DIDP)) and one adipate (bis (2-ethylhexyl) adipate, DEHA) from different water samples (Milli-Q, mineral, tap, pond and waste water) is proposed. Analysis were carried out by gas chromatography triple quadrupole tandem mass spectrometry. Parameters that affect the extraction performance were optimized following a step by step approach, being the optimum conditions the extraction of water at pH 6, with 60 mg of sorbent and the elution with 6 mL of dichloromethane. The methodology was validated for the five selected water samples using DBP-d4 as internal standard. Determination coefficients of matrix-matched calibration curves were above 0.9904 in all cases while relative recovery values ranged between 71 and 120%, with relative standard deviation values below 19%. The limits of quantification of the method ranged between 9 and 20 ng/L. Matrix effects were found for most analytes and water samples. Real water samples were also analyzed, finding DEP and DBP at concentrations below 4.20 and 1.23 μg/L, respectively, in mineral, tap and waste water. DCHP, DEHP and BBP were also found in some of the samples at concentrations below the LOQs of the method.
Javier Hernández-borges - One of the best experts on this subject based on the ideXlab platform.
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Analysis of phthalic acid esters in sea water and sea sand using polymer-coated magnetic nanoparticles as extraction sorbent.
Journal of Chromatography A, 2019Co-Authors: Gabriel Jiménez-skrzypek, Javier González-sálamo, Diana Angélica Varela-martínez, Miguel Ángel González-curbelo, Javier Hernández-borgesAbstract:Abstract In this work, poly(dopamine)-coated magnetic nanoparticles (Fe3O4@pDA) have been used as sorbents for the magnetic dispersive solid-phase extraction (m-dSPE) of a group of 10 phthalic acid esters (dipropyl Phthalate, DPP, dibutyl Phthalate, DBP, dicyclohexyl Phthalate, DCHP, bis(2-ethylhexyl)Phthalate, DEHP, di-n-octyl Phthalate, DNOP, Diisodecyl Phthalate, DIDP, butylbenzyl Phthalate, BBP, diisononyl Phthalate, DINP, diisopentyl Phthalate, DIPP, di-n-pentyl Phthalate, DNPP) and one adipate (di(2-ethylhexyl) adipate, DEHA) from sea water and sea sand extracts employing DBP-d4 and DHP-d4 as internal standards. After m-dSPE, analysis was carried out by gas chromatography mass spectrometry. Mean recovery values (which were determined at three concentration levels) ranged between 70 and 120%, with relative standard deviation values ≤ 20%, for nearly all analytes in both matrices. Matrix-matched calibration curves revealed the presence of matrix effects for certain PAEs, specially for sea sand, though linearity was assayed with determination coefficients (R2) above 0.991 for all target analytes. The limits of quantification of the method were in the range 1.8–319 ng/L for sea water and 0.020–4.0 ng/g for sea sand. Several samples of each type collected at different sites of the coast of Tenerife were also analysed. Only DEHA, DNOP and DIPP were detected in some of the sea sand samples at concentrations ≤ 44 ng/g.
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Determination of phthalic acid esters in different baby food samples by gas chromatography tandem mass spectrometry
Analytical and Bioanalytical Chemistry, 2018Co-Authors: Bárbara Socas-rodríguez, Javier González-sálamo, Álvaro Santana-mayor, Antonio V. Herrera-herrera, Javier Hernández-borgesAbstract:In this work, a new method has been developed for the determination of 14 phthalic acid esters (i.e., benzylbutyl Phthalate (BBP), bis-2- n -butoxyethyl Phthalate (DBEP), dibutyl Phthalate (DBP), dicyclohexyl Phthalate (DCHP), bis-2-ethoxyethyl Phthalate (DEEP), diethyl Phthalate (DEP), Diisodecyl Phthalate (DIDP), diisononyl Phthalate (DINP), bis-isopentyl Phthalate (DIPP), bis (2-methoxyethyl) Phthalate (DMEP), dimethyl Phthalate (DMP), di- n -octyl Phthalate (DNOP), bis- n -pentyl Phthalate (DNPP), dipropyl Phthalate (DPP)) and one adipate (bis (2-ethylhexyl) adipate (DEHA)) in different baby foods. Separation was carried out by gas chromatography triple quadrupole tandem mass spectrometry while the previous extraction of the samples was carried out using the QuEChERS method. The methodology was validated for four baby food samples (two fruit compotes of different compositions and two meat and fish purees with vegetables) using dibutyl Phthalate-3,4,5,6-d_4 (DBP-d_4) as internal standard. Determination coefficients ( R ^2) of matrix-matched calibration curves were above 0.9922 in all cases while relative recovery values ranged between 70 and 120%, with relative standard deviation values below 19%. The limits of quantification of the method ranged between 0.03 and 1.11 μg/kg. Finally, the analysis of commercially available samples was carried out finding the presence of BBP, DEHA, DEP, DIDP, and DPP in some of the studied samples.
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Determination of phthalic acid esters in water samples using core-shell poly(dopamine) magnetic nanoparticles and gas chromatography tandem mass spectrometry
Journal of Chromatography A, 2017Co-Authors: Javier González-sálamo, Bárbara Socas-rodríguez, Javier Hernández-borges, Miguel Ángel Rodríguez-delgadoAbstract:In this work, the first application of core-shell poly(dopamine) magnetic nanoparticles as sorbent for the extraction of a group of eleven phthalic acid esters of interest (i.e. diethyl Phthalate (DEP), dipropyl Phthalate (DPP), dibutyl Phthalate (DBP), bis-isopentyl Phthalate (DIPP), bis-n-pentyl Phthalate (DNPP), benzylbutyl Phthalate (BBP), dicyclohexyl Phthalate (DCHP), di-(2-ethylhexyl) Phthalate (DEHP), di-n-octyl Phthalate (DNOP), diisononyl Phthalate (DINP) and Diisodecyl Phthalate (DIDP)) and one adipate (bis (2-ethylhexyl) adipate, DEHA) from different water samples (Milli-Q, mineral, tap, pond and waste water) is proposed. Analysis were carried out by gas chromatography triple quadrupole tandem mass spectrometry. Parameters that affect the extraction performance were optimized following a step by step approach, being the optimum conditions the extraction of water at pH 6, with 60 mg of sorbent and the elution with 6 mL of dichloromethane. The methodology was validated for the five selected water samples using DBP-d4 as internal standard. Determination coefficients of matrix-matched calibration curves were above 0.9904 in all cases while relative recovery values ranged between 71 and 120%, with relative standard deviation values below 19%. The limits of quantification of the method ranged between 9 and 20 ng/L. Matrix effects were found for most analytes and water samples. Real water samples were also analyzed, finding DEP and DBP at concentrations below 4.20 and 1.23 μg/L, respectively, in mineral, tap and waste water. DCHP, DEHP and BBP were also found in some of the samples at concentrations below the LOQs of the method.
Miguel Ángel Rodríguez-delgado - One of the best experts on this subject based on the ideXlab platform.
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A green and simple procedure based on deep eutectic solvents for the extraction of Phthalates from beverages
Food Chemistry, 2019Co-Authors: Álvaro Santana-mayor, Bárbara Socas-rodríguez, Ruth Rodríguez-ramos, Miguel Ángel Rodríguez-delgadoAbstract:Abstract In this work, a green, inexpensive, simple and fast deep eutectic solvent (DES)-based dispersive liquid–liquid microextraction was evaluated, for the first time, for the extraction of Phthalates (i.e. benzylbutyl Phthalate, diisobutyl Phthalate, diisopentyl Phthalate, di-n-pentyl Phthalate, di-(2-ethylhexyl) Phthalate, di-n-octyl Phthalate, diisononyl Phthalate, Diisodecyl Phthalate) from different beverages. Separation and determination were achieved by high performance liquid chromatography-diode-array detection while confirmation was carried out by tandem mass spectrometry. The main factors affecting the extraction such as type and volume of DES and emulsifier, pH and ionic strength, were optimised. Choline chloride:phenol-based DES showed the best results. The methodology was validated for tea, apple-based beverage and pineapple juice. Recovery values ranged from 84 to 120% with relative standard deviation values lower than 11%. Limits of detection of the method were in the range 5.1–14.2 µg L−1 for tea, 5.3–17.8 µg L−1 for apple beverages and 5.9–15.6 µg L−1 for pineapple juices.
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Reduced graphene oxide-coated magnetic-nanoparticles as sorbent for the determination of Phthalates in environmental samples by micro-dispersive solid-phase extraction followed by ultra-high-performance liquid chromatography tandem mass spectrometry
Journal of Chromatography A, 2018Co-Authors: Álvaro Santana-mayor, Bárbara Socas-rodríguez, María M. Afonso, José Antonio Palenzuela-lópez, Miguel Ángel Rodríguez-delgadoAbstract:Abstract In this work, the suitability of Fe 3 O 4 nanoparticles coated with reduced-graphene oxide as sorbent was evaluated for the extraction of a group of fourteen phthalic acid esters (i.e. benzylbutyl Phthalate (BBP), bis-2- n -butoxyethyl Phthalate (DBEP), dibutyl Phthalate (DBP), diisobutyl Phthalate (DIBP), dicyclohexyl Phthalate (DCHP), bis-2-ethoxyethyl Phthalate (DEEP), Diisodecyl Phthalate (DIDP), diisononyl Phthalate (DINP), bis-isopentyl Phthalate (DIPP), bis-(2-methoxyethyl) Phthalate (DMEP), dimethyl Phthalate (DMP), di- n -octyl Phthalate (DNOP), bis- n -pentyl Phthalate (DNPP), dipropyl Phthalate (DPP)) from environmental samples. Extraction was carried out using magnetic-micro dispersive solid-phase extraction while separation, identification and quantification of the target analytes were achieved by ultra-high-performance liquid chromatography coupled to triple quadrupole tandem mass spectrometry. The methodology was validated for three different types of water samples using dibutyl Phthalate-3,4,5,6-d 4 as internal standard for all of them. Recovery values ranged from 70 to 120% for the three matrices with relative standard deviation values lower than 20%. Limits of quantification of the method achieved were in the range 6–178 ng/L for all samples and analytes. The methodology was applied for the evaluation of real samples finding the presence of DMP, DPP, BBP, DIBP and DBP in some of the analysed matrices.
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Determination of phthalic acid esters in water samples using core-shell poly(dopamine) magnetic nanoparticles and gas chromatography tandem mass spectrometry
Journal of Chromatography A, 2017Co-Authors: Javier González-sálamo, Bárbara Socas-rodríguez, Javier Hernández-borges, Miguel Ángel Rodríguez-delgadoAbstract:In this work, the first application of core-shell poly(dopamine) magnetic nanoparticles as sorbent for the extraction of a group of eleven phthalic acid esters of interest (i.e. diethyl Phthalate (DEP), dipropyl Phthalate (DPP), dibutyl Phthalate (DBP), bis-isopentyl Phthalate (DIPP), bis-n-pentyl Phthalate (DNPP), benzylbutyl Phthalate (BBP), dicyclohexyl Phthalate (DCHP), di-(2-ethylhexyl) Phthalate (DEHP), di-n-octyl Phthalate (DNOP), diisononyl Phthalate (DINP) and Diisodecyl Phthalate (DIDP)) and one adipate (bis (2-ethylhexyl) adipate, DEHA) from different water samples (Milli-Q, mineral, tap, pond and waste water) is proposed. Analysis were carried out by gas chromatography triple quadrupole tandem mass spectrometry. Parameters that affect the extraction performance were optimized following a step by step approach, being the optimum conditions the extraction of water at pH 6, with 60 mg of sorbent and the elution with 6 mL of dichloromethane. The methodology was validated for the five selected water samples using DBP-d4 as internal standard. Determination coefficients of matrix-matched calibration curves were above 0.9904 in all cases while relative recovery values ranged between 71 and 120%, with relative standard deviation values below 19%. The limits of quantification of the method ranged between 9 and 20 ng/L. Matrix effects were found for most analytes and water samples. Real water samples were also analyzed, finding DEP and DBP at concentrations below 4.20 and 1.23 μg/L, respectively, in mineral, tap and waste water. DCHP, DEHP and BBP were also found in some of the samples at concentrations below the LOQs of the method.
J. H. Braybrook - One of the best experts on this subject based on the ideXlab platform.
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Gas chromatography-mass spectrometry determination of the migration of Phthalate plasticisers from polyvinyl chloride toys and childcare articles.
Journal of chromatography. A, 2003Co-Authors: Andy O. Earls, I. P. Axford, J. H. BraybrookAbstract:Two laboratory-based linear horizontal agitation methods for determining a range of Phthalate esters from soft polyvinyl chloride (PVC) toys are presented in compliance with EU legislation. Both of these methods were validated through interlaboratory trials using a PVC reference disc and four soft PVC toy/childcare articles intended or likely to be mouthed. Two of these commercial samples contained diisononyl Phthalate (DINP), one Diisodecyl Phthalate (DIDP) and one bis(2-ethylhexyl) Phthalate (DEHP). Acceptable repeatability (r, within-laboratory) and reproducibility (R, between-laboratory) data were demonstrated for both the analytical detection technique (GC-MS) (r = 9.8% and R = 8.1%) and agitation/extraction procedure (r=21.9% and R = 35.3% at 37 degrees C; r = 22.7% and R = 31.1% at 65 degrees C) for DINP. This was achieved through the participation of six laboratories. The remaining three Phthalates from the EU Scientific Committee for Toxicity, Ecotoxicity and the Environment (CSTEE) list--dibutyl Phthalate (DBP), benzyl butyl Phthalate (BBP) and di-n-octyl Phthalate (DnOP)--were not tested due to the unavailability of suitable materials.
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Gas chromatography-mass spectrometry determination of the migration of Phthalate plasticisers from polyvinyl chloride toys and childcare articles
Journal of Chromatography A, 2003Co-Authors: Andy O. Earls, I. P. Axford, J. H. BraybrookAbstract:Two laboratory-based linear horizontal agitation methods for determining a range of Phthalate esters from soft polyvinyl chloride (PVC) toys are presented in compliance with EU legislation. Both of these methods were validated through interlaboratory trials using a PVC reference disc and four soft PVC toy/childcare articles intended or likely to be mouthed. Two of these commercial samples contained diisononyl Phthalate (DINP), one Diisodecyl Phthalate (DIDP) and one bis(2-ethylhexyl) Phthalate (DEHP). Acceptable repeatability (r, within-laboratory) and reproducibility (R, between-laboratory) data were demonstrated for both the analytical detection technique (GC-MS) (r=9.8% and R=8.1%) and agitation/extraction procedure (r=21.9% and R=35.3% at 37°C; r=22.7% and R=31.1% at 65°C) for DINP. This was achieved through the participation of six laboratories. The remaining three Phthalates from the EU Scientific Committee for Toxicity, Ecotoxicity and the Environment (CSTEE) list - dibutyl Phthalate (DBP), benzyl butyl Phthalate (BBP) and di-n-octyl Phthalate (DnOP) - were not tested due to the unavailability of suitable materials. © 2002 Published by Elsevier Science B.V. All rights reserved.
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Gas chromatography-mass spectrometry determination of the migration of Phthalate plasticisers from polyvinyl chloride toys and childcare articles.
Journal of Chromatography A, 2003Co-Authors: Andy O. Earls, I. P. Axford, J. H. BraybrookAbstract:Abstract Two laboratory-based linear horizontal agitation methods for determining a range of Phthalate esters from soft polyvinyl chloride (PVC) toys are presented in compliance with EU legislation. Both of these methods were validated through interlaboratory trials using a PVC reference disc and four soft PVC toy/childcare articles intended or likely to be mouthed. Two of these commercial samples contained diisononyl Phthalate (DINP), one Diisodecyl Phthalate (DIDP) and one bis(2-ethylhexyl) Phthalate (DEHP). Acceptable repeatability (r, within-laboratory) and reproducibility (R, between-laboratory) data were demonstrated for both the analytical detection technique (GC–MS) (r=9.8% and R=8.1%) and agitation/extraction procedure (r=21.9% and R=35.3% at 37 °C; r=22.7% and R=31.1% at 65 °C) for DINP. This was achieved through the participation of six laboratories. The remaining three Phthalates from the EU Scientific Committee for Toxicity, Ecotoxicity and the Environment (CSTEE) list—dibutyl Phthalate (DBP), benzyl butyl Phthalate (BBP) and di-n-octyl Phthalate (DnOP)—were not tested due to the unavailability of suitable materials.