{"id":45301,"date":"2020-10-15T00:00:00","date_gmt":"2020-10-15T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/analyse-gc-ms-des-phtalates-comparaison-de-7-phases-stationnaires\/"},"modified":"2026-01-29T14:30:54","modified_gmt":"2026-01-29T14:30:54","slug":"analyse-gc-ms-des-phtalates-comparaison-de-7-phases-stationnaires","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/notes-dapplication\/gnan2380-fr\/analyse-gc-ms-des-phtalates-comparaison-de-7-phases-stationnaires","title":{"rendered":"Analyse GC-MS des phtalates : comparaison de 7 phases stationnaires"},"content":{"rendered":"\n

Abstract<\/h2>\n\n\n\n

Les phtalates sont omnipr\u00e9sents dans notre environnement et doivent \u00eatre contr\u00f4l\u00e9s en raison de leur impact n\u00e9gatif potentiel sur la sant\u00e9 humaine. Il est donc indispensable de pouvoir les s\u00e9parer et les d\u00e9tecter. La chromatographie en phase gazeuse est la technique de choix pour s\u00e9parer ces compos\u00e9s. Elle peut \u00eatre associ\u00e9e \u00e0 diff\u00e9rents modes de d\u00e9tection, notamment la capture d\u2019 \u00e9lectrons (ECD), l\u2019ionisation de flamme (FID) et la spectrom\u00e9trie de masse (SM). Dans cette \u00e9tude, le logiciel de mod\u00e9lisation chromatographique Pro EZ<\/em>GC a \u00e9t\u00e9 utilis\u00e9 pour identifier la meilleure phase stationnaire et d\u00e9terminer les conditions optimales pour l\u2019analyse GC-MS des phtalates. Sept phases stationnaires ont \u00e9t\u00e9 \u00e9tudi\u00e9es : Rtx-440, Rxi-XLB, Rxi-5ms, Rtx-50, Rxi-35Sil MS, Rtx-CLPesticides et Rtx-CLPesticides2. Les r\u00e9sultats obtenus ont \u00e9t\u00e9 compar\u00e9s. Dans tous les cas les 18 phtalates r\u00e9pertori\u00e9s dans les m\u00e9thodes EPA (Environmental Protection Agency) et\/ou europ\u00e9ennes ont \u00e9t\u00e9 analys\u00e9s en moins de 6 minutes. Par ailleurs, 37 phtalates ont \u00e9galement \u00e9t\u00e9 analys\u00e9s en moins de 40 minutes gr\u00e2ce \u00e0 une m\u00e9thode optimis\u00e9e. La meilleure r\u00e9solution de ce m\u00e9lange complexe de phtalates a \u00e9t\u00e9 obtenue avec les colonnes Rtx-440, phase exclusive Restek et Rxi-XLB.<\/p>\n\n\n\n

Introduction<\/h2>\n\n\n\n

Les phtalates sont couramment utilis\u00e9s comme plastifiants dans divers produits industriels. Certains d\u2019entre eux sont cependant consid\u00e9r\u00e9s comme des perturbateurs endocriniens [1] et sont li\u00e9s \u00e0 de nombreuses pathologies comme les malformations cong\u00e9nitales [2] ; l\u2019hypertension art\u00e9rielle chez les enfants [3] ; les cardiopathies hypertensives induites par la grossesse [4] ; les troubles respiratoires [5] et l’ob\u00e9sit\u00e9 [6]. L\u2019Union Europ\u00e9enne (UE) et l\u2019EPA ont restreint l\u2019utilisation des phtalates les plus nocifs (Tableau I).<\/p>\n\n\n\n

La GC-MS est couramment utilis\u00e9e pour l’analyse des phtalates car elle est simple, rapide et \u00e9conomique. La d\u00e9tection par spectrom\u00e9trie de masse permet de d\u00e9terminer la nature des phtalates. Il est essentiel de choisir une colonne chromatographique garantissant de bonnes s\u00e9parations car les similitudes structurelles entre les phtalates peuvent rendre difficiles l\u2019identification et la quantification MS. Par exemple, de nombreux phtalates partagent un m\u00eame ion de base (m\/z 149), ce qui complique l\u2019identification et la quantification des phtalates co\u00e9lu\u00e9s. La pr\u00e9sence dans les m\u00e9langes de phtalates de grade technique et d\u2019isom\u00e8res constituent une difficult\u00e9 suppl\u00e9mentaire.<\/p>\n\n\n\n

Un article publi\u00e9 r\u00e9cemment passait en revue les colonnes GC et LC les plus fr\u00e9quemment utilis\u00e9es pour l\u2019analyse des phtalates [7]. Selon ce document, la GC-MS produit une meilleure r\u00e9solution de ces compos\u00e9s par rapport \u00e0 la LC-MS. Les colonnes GC les plus couramment utilis\u00e9es sont dans l\u2019ordre : de type 5% ph\u00e9nyle siloxane, XLB, 35% ph\u00e9nyle siloxane, 17, 50% ph\u00e9nyle siloxane et 1 (100% m\u00e9thyle siloxane). Les s\u00e9parations obtenues avec chaque phase stationnaire peuvent \u00eatre optimis\u00e9es en ajustant les conditions analytiques. Dans la pratique, ces ajustements constituent un travail long et fastidieux. Le logiciel de mod\u00e9lisation Pro EZ<\/em>GC permet d\u2019 optimiser rapidement les conditions analytiques (par exemple, le choix du gaz vecteur, son d\u00e9bit, le programme de temp\u00e9rature, les dimensions de la colonne et de la pr\u00e9colonne) pour obtenir les meilleurs r\u00e9sultats dans le temps le plus court possible, avec chacune des phases stationnaires. Pour cette \u00e9tude, une biblioth\u00e8que de 37 phtalates (Tableau II) a \u00e9t\u00e9 cr\u00e9\u00e9e dans le programme Pro EZ<\/em>GC pour \u00eatre ensuite utilis\u00e9e avec les sept phases stationnaires : Rtx-440, Rxi-XLB, Rxi-5ms, Rtx-50, Rxi-35Sil MS, Rtx-CLPesticides et Rtx-CLPesticides2.<\/p>\n\n\n\n

\u00c9talons analytiques<\/h2>\n\n\n\n

La solution-\u00e9talon d\u2019esters de phtalate EPA 8061A (r\u00e9f. 33227) contenant 15 des analytes-cibles, chacun \u00e0 une concentration de 1 000 \u03bcg\/ml, a \u00e9t\u00e9 utilis\u00e9e comme \u00e9talon principal. Le benzoate de benzyle (r\u00e9f. 31847) \u00e9tait l\u2019\u00e9talon interne. Tous les autres \u00e9talons proviennent de la soci\u00e9t\u00e9 Chem Service.<\/p>\n\n\n\n

Appareillage<\/h2>\n\n\n\n

L\u2019analyse GC-MS a \u00e9t\u00e9 r\u00e9alis\u00e9e avec un Shimadzu QP2010 Plus. Chacune des sept colonnes Restek (dans leur configuration de 30 m \u00d7 0,25 mm \u00d7 0,25 \u03bcm – 0,20 \u03bcm pour la colonne Rtx-CLPesticides2) est tour \u00e0 tour install\u00e9e dans l\u2019appareil. Le logiciel Pro ZGC (sous Windows) a permis de d\u00e9terminer les conditions optimales pour chaque colonne. Les performances des colonnes ont ensuite \u00e9t\u00e9 compar\u00e9es en proc\u00e9dant \u00e0 l\u2019analyse r\u00e9elle des solutions pr\u00e9par\u00e9es, en appliquant pour chaque colonne les m\u00eames conditions analytiques qui avaient produit les meilleures s\u00e9parations. Cette comparaison permet de mieux comprendre les diff\u00e9rences de s\u00e9lectivit\u00e9 entre les colonnes. Les descriptions d\u00e9taill\u00e9es des colonnes et les conditions analytiques sont pr\u00e9sent\u00e9es respectivement dans le Tableau I et le Tableau III.<\/p>\n\n\n\n

Pr\u00e9paration des \u00e9chantillons<\/h2>\n\n\n\n

Les \u00e9talons ont \u00e9t\u00e9 dissous et dilu\u00e9s dans du chlorure de m\u00e9thyl\u00e8ne pour pr\u00e9parer des solutions \u00e0 50 \u03bcg\/ml (80 \u03bcg\/ml pour l’\u00e9talon interne de benzoate de benzyle). Pour ces pr\u00e9parations, toute vaisselle ou accessoires en plastique ont \u00e9t\u00e9 proscrits au profit de mat\u00e9riel en verre (flacons jaug\u00e9s, seringues, fioles, etc.).<\/p>\n\n\n\n

<\/a>R\u00e9sultats et discussion<\/h2>\n\n\n\n

Nous avons compar\u00e9 la performance de sept colonnes pour la s\u00e9paration de 37 phtalates. Le logiciel Pro EZ<\/em>GC a permis de pr\u00e9voir les temps de r\u00e9tention pour chaque phase stationnaire en utilisant les m\u00eames conditions analytiques. Ces conditions, d\u00e9crites dans le Tableau I, sont celles qui ont permis d\u2019obtenir les meilleurs r\u00e9sultats parmi l\u2019ensemble de conditions sp\u00e9cifiques optimis\u00e9es pour chaque colonne. Nous avons consid\u00e9r\u00e9 qu\u2019il y avait “co\u00e9lution” lorsque la r\u00e9solution entre deux compos\u00e9s \u00e9tait inf\u00e9rieure \u00e0 1,5. Le temps d\u2019analyse total \u00e9tait inf\u00e9rieur \u00e0 6 minutes. Pour confirmer les temps de r\u00e9tention pr\u00e9vus par le logiciel Pro EZ<\/em>GC, des analyses ont \u00e9t\u00e9 faites avec chaque phase stationnaire dans les m\u00eames conditions que celles “conseill\u00e9es” par le logiciel (Figure 1). \u00c9tant donn\u00e9 que la longueur r\u00e9elle des colonnes n\u2019\u00e9tait pas exactement de 30 m\u00e8tres, comme dans la simulation, les temps de r\u00e9tention absolus \u00e9taient l\u00e9g\u00e8rement diff\u00e9rents par rapport aux valeurs pr\u00e9vues. L’ordre d\u2019\u00e9lution et les co\u00e9lutions \u00e9taient conformes \u00e0 ce qu\u2019avait pr\u00e9vu le logiciel. Les colonnes Rtx-440, Rxi-XLB, Rtx-CLPesticides et Rxi-35Sil MS ont s\u00e9par\u00e9 \u00e0 la ligne de base les 37 phtalates r\u00e9pertori\u00e9s. Les deux isom\u00e8res de phtalate de bis[4-methyle-2-pentyle] n\u2019ont \u00e9t\u00e9 r\u00e9solus sur aucune des sept phases. L’ordre d\u2019\u00e9lution \u00e9tait comparable sur les colonnes Rtx-440, Rxi-XLB, Rtx-CLPesticides et Rxi-5ms.<\/p>\n\n\n\n

Nous avons observ\u00e9 des diff\u00e9rences dans l\u2019ordre d\u2019\u00e9lution avec les phases Rxi-35Sil MS et Rtx-50. L\u2019ordre d\u2019\u00e9lution a notamment chang\u00e9 avec la colonne Rxi-35Sil MS pour ces quatre paires de compos\u00e9s : les isom\u00e8res de phtalate de bis(2-methoxy\u00e9thyle) et bis(4-m\u00e9thyle-2-pentyle) (pics 6 et 7\/8), de bis(2-\u00e9thoxy\u00e9thyle) et di-n-pentyle (pics 9 et 10), de benzyle butyle et d\u2019hexyle-2-\u00e9thylhexyle (pics 12 et 13) et de bis(2-butoxy\u00e9thyle) et bis(2-\u00e9thylhexyle) (pics 14 et 15).<\/p>\n\n\n\n

Les colonnes Rtx-440 et Rxi-XLB pr\u00e9sentaient globalement les meilleures s\u00e9parations dans ces conditions. Les pics qui ont co\u00e9lu\u00e9 avec les autres colonnes \u00e9taient bien r\u00e9solus avec les colonnes Rtx-440 et Rxi-XLB. Les paires non r\u00e9solues avec les autres phases sont les phtalates de bis(2-\u00e9thylhexyle) et de dicyclohexyle (pics 15 et 16) avec la colonne Rxi-5ms ; les phtalates de bis(2-\u00e9thylhexyle) et de benzyle butyle (pics 15 et 12) avec la colonne Rtx-50 ; et les phtalates de bis(2-m\u00e9thoxy\u00e9thyle) et de bis[4-m\u00e9thyle-2-pentyle] (pics 6 et 7,8) ainsi que le phtalate de bis(2-ethoxy\u00e9thyle) et de di-n-pentyle (pics 9 et 10) sur la colonne Rtx-CLPesticides2. Dans les m\u00e9langes d\u2019isom\u00e8res de grade technique, il est possible d\u2019identifier des groupes d\u2019isom\u00e8res, tels que le phtalate de diisononyle et le phtalate de diisod\u00e9cyle (pics 18 et 19). Il est cependant impossible de r\u00e9soudre compl\u00e8tement chaque isom\u00e8re au sein de ces groupes. Heureusement, leurs ions sp\u00e9cifiques permettent leur identification et quantification, comme le m\/z 293 pour le phtalate de diisononyle et le m\/z 307 pour le phtalate de diisodecyle (Figure 1<\/strong>).<\/p>\n\n\n\n

Tableau I :<\/strong> Temps de r\u00e9tention pr\u00e9vus par le logiciel Pro EZ<\/em>GC avec 7 colonnes Restek<\/p>\n\n\n\n

Colonne : 30 m x 0,25 mm x 0,25 \u03bcm (0,20 \u03bcm pour la colonne Rtx-CLPesticides2)
Vitesse lin\u00e9aire constante : 66,7 cm\/sec
Four : 200 \u00b0C (isotherme de 0,5 min) \u00e0 330 \u00b0C (320 \u00b0C pour la colonne Rtx-50) \u00e0 30 \u00b0C\/min (isotherme de 1 min)<\/p>\n\n\n

\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n\n
ak #<\/strong><\/th>\nName<\/strong><\/th>\nListed<\/strong><\/th>\nRetention Time (min)<\/strong><\/th>\nCAS #<\/strong><\/th>\nPurity<\/strong><\/th>\n<\/tr>\n
Rtx-440
(cat. 12923)<\/strong><\/th>\n		Rxi-XLB
(cat. 13723)<\/strong><\/th>\n		Rtx-
CLPesticides
(cat. 11123)<\/strong><\/th>\n		Rxi-35Sil MS (cat. 13823)<\/strong><\/th>\nRtx-50
(cat. 10523)<\/strong><\/th>\n		Rxi-5ms
(cat. 13423)<\/strong><\/th>\n		Rtx-
CLPesticides2
(cat. 11323)<\/strong><\/th>\n<\/tr>\n
1<\/td>\nDimethyl phthalate*<\/td>\nEPA 8061A, EPA Priority<\/td>\n1.28<\/td>\n1.16<\/td>\n1.14<\/td>\n1.29<\/td>\n1.46<\/td>\n1.10<\/td>\n1.23<\/td>\n131-11-3<\/td>\nNeat<\/td>\n<\/tr>\n
2<\/td>\nDiethyl phthalate*<\/td>\nEPA 8061A, EPA Priority, EU<\/td>\n1.54<\/td>\n1.39<\/td>\n1.33<\/td>\n1.55<\/td>\n1.73<\/td>\n1.30<\/td>\n1.47<\/td>\n84-66-2<\/td>\nNeat<\/td>\n<\/tr>\n
3<\/td>\nBenzyl benzoate<\/td>\nInternal Standard<\/td>\n2.11<\/td>\n1.87<\/td>\n1.56<\/td>\n2.17<\/td>\n2.31<\/td>\n1.70<\/td>\n1.88<\/td>\n120-51-4<\/td>\nNeat<\/td>\n<\/tr>\n
4<\/td>\nDiisobutyl phthalate*<\/td>\nEPA 8061A<\/td>\n2.25<\/td>\n2.04<\/td>\n1.88<\/td>\n2.21<\/td>\n2.34<\/td>\n1.91<\/td>\n2.10<\/td>\n84-69-5<\/td>\nNeat<\/td>\n<\/tr>\n
5<\/td>\nDi-n<\/em>-butyl phthalate*<\/td>\nEPA 8061A, EPA Priority<\/td>\n2.58<\/td>\n2.33<\/td>\n2.10<\/td>\n2.53<\/td>\n2.69<\/td>\n2.17<\/td>\n2.38<\/td>\n84-74-2<\/td>\nNeat<\/td>\n<\/tr>\n
6<\/td>\nBis(2-methoxyethyl) phthalate*<\/td>\nEPA 8061A<\/td>\n2.74<\/td>\n2.48<\/td>\n2.26<\/td>\n2.86<\/td>\n3.10<\/td>\n2.27<\/td>\n2.63<\/td>\n117-82-8<\/td>\nNeat<\/td>\n<\/tr>\n
7<\/td>\nBis(4-methyl-2-pentyl) phthalate isomer 1*<\/td>\nEPA 8061A<\/td>\n2.85<\/td>\n2.62<\/td>\n2.37<\/td>\n2.71<\/td>\n2.83<\/td>\n2.50<\/td>\n2.64<\/td>\n84-63-9<\/td>\nNeat<\/td>\n<\/tr>\n
8<\/td>\nBis(4-methyl-2-pentyl) phthalate isomer 2*<\/td>\nEPA 8061A<\/td>\n2.86<\/td>\n2.63<\/td>\n2.37<\/td>\n2.72<\/td>\n2.84<\/td>\n2.51<\/td>\n2.65<\/td>\n84-63-9<\/td>\nNeat<\/td>\n<\/tr>\n
9<\/td>\nBis(2-ethoxyethyl) phthalate*<\/td>\nEPA 8061A<\/td>\n3.08<\/td>\n2.80<\/td>\n2.51<\/td>\n3.13<\/td>\n3.33<\/td>\n2.59<\/td>\n2.90<\/td>\n605-54-9<\/td>\nNeat<\/td>\n<\/tr>\n
10<\/td>\nDi-n<\/em>-pentyl phthalate*<\/td>\nEPA 8061A<\/td>\n3.16<\/td>\n2.91<\/td>\n2.58<\/td>\n3.08<\/td>\n3.21<\/td>\n2.71<\/td>\n2.89<\/td>\n131-18-0<\/td>\nNeat<\/td>\n<\/tr>\n
11<\/td>\nDi-n<\/em>-hexyl phthalate*<\/td>\nEPA 8061A<\/td>\n3.73<\/td>\n3.46<\/td>\n3.07<\/td>\n3.61<\/td>\n3.69<\/td>\n3.25<\/td>\n3.42<\/td>\n84-75-3<\/td>\nNeat<\/td>\n<\/tr>\n
12<\/td>\nButyl benzyl phthalate*<\/td>\nEPA 8061A, EPA Priority, EU<\/td>\n3.85<\/td>\n3.56<\/td>\n3.12<\/td>\n3.93<\/td>\n4.13<\/td>\n3.30<\/td>\n3.63<\/td>\n85-68-7<\/td>\nNeat<\/td>\n<\/tr>\n
13<\/td>\nHexyl 2-ethylhexyl phthalate<\/td>\nEPA 8061A<\/td>\n3.98<\/td>\n3.72<\/td>\n3.29<\/td>\n3.83<\/td>\n3.92<\/td>\n3.52<\/td>\n3.66<\/td>\n75673-16-4<\/td>\nTechnical<\/td>\n<\/tr>\n
14<\/td>\nBis(2-butoxyethyl) phthalate*<\/td>\nEPA 8061A<\/td>\n4.12<\/td>\n3.82<\/td>\n3.39<\/td>\n4.08<\/td>\n4.21<\/td>\n3.60<\/td>\n3.85<\/td>\n117-83-9<\/td>\nNeat<\/td>\n<\/tr>\n
15<\/td>\nBis(2-ethylhexyl) phthalate*<\/td>\nEPA 8061A<\/td>\n4.21<\/td>\n3.95<\/td>\n3.52<\/td>\n4.05<\/td>\n4.12<\/td>\n3.82<\/td>\n3.91<\/td>\n117-81-7<\/td>\nNeat<\/td>\n<\/tr>\n
16<\/td>\nDicyclohexyl phthalate*<\/td>\nEPA 8061A, EPA Priority, EU<\/td>\n4.33<\/td>\n4.04<\/td>\n3.55<\/td>\n4.42<\/td>\n4.58<\/td>\n3.78<\/td>\n4.08<\/td>\n84-61-7<\/td>\nNeat<\/td>\n<\/tr>\n
17<\/td>\nDi-n<\/em>-octyl phthalate*<\/td>\nEPA 8061A, EPA Priority, EU<\/td>\n4.76<\/td>\n4.50<\/td>\n3.97<\/td>\n4.59<\/td>\n4.62<\/td>\n4.24<\/td>\n4.39<\/td>\n117-84-0<\/td>\nNeat<\/td>\n<\/tr>\n
18<\/td>\nDiisononyl phthalate<\/td>\nEU<\/td>\n5.10<\/td>\n4.84<\/td>\n4.23<\/td>\n4.84<\/td>\n4.84<\/td>\n4.50<\/td>\n4.64<\/td>\n68515-48-0<\/td>\nIsomer mix<\/td>\n<\/tr>\n
19<\/td>\nDiisodecyl phthalate<\/td>\nEU<\/td>\n5.20<\/td>\n4.95**<\/td>\n4.42<\/td>\n5.01<\/td>\n5.18<\/td>\n4.71<\/td>\n4.90<\/td>\n26761-40-0<\/td>\nIsomer mix<\/td>\n<\/tr>\n
20<\/td>\nDinonyl phthalate*<\/td>\nEPA 8061A<\/td>\n5.24<\/td>\n4.95**<\/td>\n4.39<\/td>\n5.04<\/td>\n5.10<\/td>\n4.72<\/td>\n4.83<\/td>\n84-76-4<\/td>\nNeat<\/td>\n<\/tr>\n<\/tbody>\n<\/table>\n<\/figure>\n\n\n

Remarque : les zones gris\u00e9es indiquent les co\u00e9lutions (Rs<1,5).
*Ces compos\u00e9s figurent dans le m\u00e9lange d\u2019esters de phtalate de la M\u00e9thode 8061A EPA Restek (r\u00e9f. 33227).
**Les pics 19 et 20 sont non-isobariques et peuvent \u00eatre s\u00e9par\u00e9s en mode SIM.<\/p>\n\n\n\n


Nous avons observ\u00e9 des diff\u00e9rences dans l\u2019ordre d\u2019\u00e9lution avec les phases Rxi-35Sil MS et Rtx-50. L\u2019ordre d\u2019\u00e9lution a notamment chang\u00e9 avec la colonne Rxi-35Sil MS pour ces quatre paires de compos\u00e9s : les isom\u00e8res de phtalate de bis(2-methoxy\u00e9thyle) et bis(4-m\u00e9thyle-2-pentyle) (pics 6 et 7\/8), de bis(2-\u00e9thoxy\u00e9thyle) et di-n-pentyle (pics 9 et 10), de benzyle butyle et d\u2019hexyle-2-\u00e9thylhexyle (pics 12 et 13) et de bis(2-butoxy\u00e9thyle) et bis(2-\u00e9thylhexyle) (pics 14 et 15).<\/p>\n\n\n\n

Les colonnes Rtx-440 et Rxi-XLB pr\u00e9sentaient globalement les meilleures s\u00e9parations dans ces conditions. Les pics qui ont co\u00e9lu\u00e9 avec les autres colonnes \u00e9taient bien r\u00e9solus avec les colonnes Rtx-440 et Rxi-XLB. Les paires non r\u00e9solues avec les autres phases sont les phtalates de bis(2-\u00e9thylhexyle) et de dicyclohexyle (pics 15 et 16) avec la colonne Rxi-5ms ; les phtalates de bis(2-\u00e9thylhexyle) et de benzyle butyle (pics 15 et 12) avec la colonne Rtx-50 ; et les phtalates de bis(2-m\u00e9thoxy\u00e9thyle) et de bis[4-m\u00e9thyle-2-pentyle] (pics 6 et 7,8) ainsi que le phtalate de bis(2-ethoxy\u00e9thyle) et de di-n-pentyle (pics 9 et 10) sur la colonne Rtx-CLPesticides2. Dans les m\u00e9langes d\u2019isom\u00e8res de grade technique, il est possible d\u2019identifier des groupes d\u2019isom\u00e8res, tels que le phtalate de diisononyle et le phtalate de diisod\u00e9cyle (pics 18 et 19). Il est cependant impossible de r\u00e9soudre compl\u00e8tement chaque isom\u00e8re au sein de ces groupes. Heureusement, leurs ions sp\u00e9cifiques permettent leur identification et quantification, comme le m\/z 293 pour le phtalate de diisononyle et le m\/z 307 pour le phtalate de diisodecyle (Figure 1<\/strong>).<\/p>\n\n\n\n

Une comparaison plus compl\u00e8te des sept phases stationnaires a \u00e9galement \u00e9t\u00e9 r\u00e9alis\u00e9e pour la s\u00e9paration de 37 phtalates (40 pics en tout, dont trois isom\u00e8res) en utilisant les temps de r\u00e9tention pr\u00e9vus par le programme Pro EZ<\/em>GC (Tableau II). Les conditions analytiques reprises dans le Tableau III ont permis la s\u00e9paration de 34 des 40 pics avec les colonnes Rtx-440 et Rxi-XLB en moins de 40 minutes, les deux phases pr\u00e9sentant des diff\u00e9rences d\u2019ordre d\u2019\u00e9lution. Le chromatogramme obtenu avec la colonne Rtx-440 est pr\u00e9sent\u00e9 en Figure 2<\/strong>. Pour certaines paires qui n\u2019\u00e9taient pas r\u00e9solues \u00e0 la ligne de base, la r\u00e9solution reste suffisante pour une analyse qualitative. Il n\u2019a pas \u00e9t\u00e9 possible d\u2019\u00e9tablir des conditions analytiques qui soient optimales pour toutes les phases. Le programme qui produit les meilleurs r\u00e9sultats en termes de dur\u00e9e de l\u2019analyse et de nombre de pics r\u00e9solus a \u00e9t\u00e9 retenu pour r\u00e9aliser cette comparaison. Ces conditions peuvent \u00eatre optimis\u00e9es avec le logiciel Pro EZ<\/em>GC si d\u2019autres compos\u00e9s doivent \u00eatre s\u00e9par\u00e9s. Consid\u00e9rant les dur\u00e9es d\u2019analyse et les s\u00e9parations obtenues, les colonnes Rtx-440 et Rxi-XLB apparaissent comme les meilleurs choix pour l\u2019analyse des phtalates.<\/p>\n\n\n\n

Tableau II : <\/strong>Temps de r\u00e9tention pr\u00e9vus par le logiciel Pro EZ<\/em>GC avec 7 colonnes Restek<\/p>\n\n\n\n

Colonne : 30 m x 0,25 mm x 0,25 \u03bcm (0,20 \u03bcm pour la colonne Rtx-CLPesticides2)
Vitesse lin\u00e9aire constante : 48 cm\/sec
Four : 150 \u00b0C (isotherme de 0,8 min) \u00e0 200 \u00b0C \u00e0 5 \u00b0C\/min \u00e0 275 \u00b0C \u00e0 3 \u00b0C\/min (isotherme de 2 min)<\/p>\n\n\n\n

\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n\r\n
Peak #<\/strong><\/th>\r\nName<\/strong><\/th>\r\nListed<\/strong><\/th>\r\nRetention Time (min)<\/strong><\/th>\r\nCAS #<\/strong><\/th>\r\nPurity<\/strong><\/th>\r\n<\/tr>\r\n
Rtx-440
(cat. 12923)<\/strong><\/th>\r\n		Rxi-XLB
(cat. 13723)<\/strong><\/th>\r\n		Rxi-5ms (cat. 13423)<\/strong><\/th>\r\nRtx-50 (cat. 10523)<\/strong><\/th>\r\nRxi-35Sil MS (cat. 13823)<\/strong><\/th>\r\nRtx-
CLPesticides
(cat. 11123)<\/strong><\/th>\r\n		Rtx-
CLPesticides2
(cat. 11323)<\/strong><\/th>\r\n<\/tr>\r\n<\/thead>\r\n
1<\/td>\r\nDimethyl phthalate*<\/td>\r\nEPA 8061A, EPA Priority<\/td>\r\n4.606<\/td>\r\n3.924<\/td>\r\n3.294<\/td>\r\n5.912<\/td>\r\n4.902<\/td>\r\n3.75<\/td>\r\n4.334<\/td>\r\n131-11-3<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
2<\/td>\r\nDimethyl isophthalate<\/td>\r\n—<\/td>\r\n5.491<\/td>\r\n4.690<\/td>\r\n3.85<\/td>\r\n6.35<\/td>\r\n5.498<\/td>\r\n4.174<\/td>\r\n4.793<\/td>\r\n1459-93-4<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
3<\/td>\r\nDiethyl phthalate*<\/td>\r\nEPA 8061A, EPA Priority, EU<\/td>\r\n6.537<\/td>\r\n5.642<\/td>\r\n4.762<\/td>\r\n7.809<\/td>\r\n6.785<\/td>\r\n5.24<\/td>\r\n6.106<\/td>\r\n84-66-2<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
4<\/td>\r\nBenzyl benzoate<\/td>\r\nInternal Standard<\/td>\r\n9.931<\/td>\r\n8.667<\/td>\r\nN\/A<\/td>\r\n11.099<\/td>\r\nN\/A<\/td>\r\n6.725<\/td>\r\n8.583<\/td>\r\n120-51-4<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
5<\/td>\r\nDiisobutyl phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n11.185<\/td>\r\n10.029<\/td>\r\n8.817<\/td>\r\n11.817<\/td>\r\n11.008<\/td>\r\n9.101<\/td>\r\n10.333<\/td>\r\n84-69-5<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
6<\/td>\r\nDi-n<\/em>-butyl phthalate*<\/td>\r\nEPA 8061A, EPA Priority<\/td>\r\n13.152<\/td>\r\n11.850<\/td>\r\n10.405<\/td>\r\n14.031<\/td>\r\n13.094<\/td>\r\n10.481<\/td>\r\n12.029<\/td>\r\n84-74-2<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
7<\/td>\r\nBis(2-methoxyethyl) phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n14.343<\/td>\r\n12.784<\/td>\r\n11.045<\/td>\r\n17.095<\/td>\r\n15.424<\/td>\r\n11.54<\/td>\r\n13.725<\/td>\r\n117-82-8<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
8<\/td>\r\nBis(4-methyl-2-pentyl) phthalate isomer 1*<\/td>\r\nEPA 8061A<\/td>\r\n15.192<\/td>\r\n13.754<\/td>\r\n12.47<\/td>\r\n15.184<\/td>\r\n14.454<\/td>\r\n12.166<\/td>\r\n13.825<\/td>\r\n84-63-9<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
9<\/td>\r\nBis(4-methyl-2-pentyl) phthalate isomer-2*<\/td>\r\nEPA 8061A<\/td>\r\n15.350<\/td>\r\n13.828<\/td>\r\n12.55<\/td>\r\n15.277<\/td>\r\n14.542<\/td>\r\n12.233<\/td>\r\n13.906<\/td>\r\n84-63-9<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
10<\/td>\r\nBis(2-ethoxyethyl) phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n16.910<\/td>\r\n15.132<\/td>\r\n13.199<\/td>\r\n19.063<\/td>\r\n17.59<\/td>\r\n13.186<\/td>\r\n15.875<\/td>\r\n605-54-9<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
11<\/td>\r\nDi-n<\/em>-pentyl phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n17.454<\/td>\r\n15.880<\/td>\r\n13.856<\/td>\r\n17.974<\/td>\r\n17.128<\/td>\r\n13.588<\/td>\r\n15.768<\/td>\r\n131-18-0<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
12<\/td>\r\nButyl cyclohexyl phthalate<\/td>\r\n—<\/td>\r\n19.452<\/td>\r\n17.689<\/td>\r\n15.478<\/td>\r\n21.19<\/td>\r\n19.843<\/td>\r\n14.979<\/td>\r\n17.96<\/td>\r\n84-64-0<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
13<\/td>\r\nButyl 2-ethylhexyl phthalate<\/td>\r\n—<\/td>\r\n19.823<\/td>\r\n18.172<\/td>\r\n16.174<\/td>\r\n20.062<\/td>\r\n19.238<\/td>\r\n15.566<\/td>\r\n17.958<\/td>\r\n85-69-8<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
14<\/td>\r\nDi-n<\/em>-hexyl phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n22.138<\/td>\r\n20.279<\/td>\r\n17.984<\/td>\r\n22.152<\/td>\r\n21.469<\/td>\r\n17.215<\/td>\r\n19.829<\/td>\r\n84-75-3<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
15<\/td>\r\nButyl octyl phthalate<\/td>\r\n—<\/td>\r\n22.338<\/td>\r\n20.557<\/td>\r\n18.136<\/td>\r\n22.37<\/td>\r\n21.668<\/td>\r\n17.344<\/td>\r\n20.009<\/td>\r\n84-78-6<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
16<\/td>\r\nButyl benzyl phthalate*<\/td>\r\nEPA 8061A, EPA Priority, EU<\/td>\r\n22.799<\/td>\r\n20.783<\/td>\r\n18.029<\/td>\r\n25.365<\/td>\r\n23.782<\/td>\r\n17.384<\/td>\r\n21.128<\/td>\r\n85-68-7<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
17<\/td>\r\nHexyl 2-ethylhexyl phthalate<\/td>\r\nEPA 8061A<\/td>\r\n24.404<\/td>\r\n22.668<\/td>\r\n20.266<\/td>\r\n24.110<\/td>\r\n23.500<\/td>\r\n19.126<\/td>\r\n22.049<\/td>\r\n75673-16-4<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
18<\/td>\r\nButyl isodecyl phthalate<\/td>\r\n—<\/td>\r\n24.632<\/td>\r\n22.793<\/td>\r\n20.392<\/td>\r\n24.220<\/td>\r\n23.685<\/td>\r\n19.424<\/td>\r\n22.22<\/td>\r\n42343-36-2<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
19<\/td>\r\nBis(2-ethylhexyl)hexahydro phthalate<\/td>\r\n—<\/td>\r\n25.066<\/td>\r\n23.389<\/td>\r\n21.254<\/td>\r\n23.089<\/td>\r\n23.063<\/td>\r\n19.142<\/td>\r\n21.961<\/td>\r\n84-71-9<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
20<\/td>\r\nBis(2-n<\/em>-butoxyethyl) phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n25.601<\/td>\r\n23.563<\/td>\r\n20.930<\/td>\r\n26.746<\/td>\r\n25.647<\/td>\r\n19.849<\/td>\r\n23.533<\/td>\r\n117-83-9<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
21<\/td>\r\nDicyclohexyl phthalate*<\/td>\r\nEPA 8061A, EPA Priority, EU<\/td>\r\n26.651<\/td>\r\n24.495<\/td>\r\n21.771<\/td>\r\n28.989<\/td>\r\n27.671<\/td>\r\n20.530<\/td>\r\n24.792<\/td>\r\n84-61-7<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
22<\/td>\r\nBis(2-ethylhexyl) phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n26.692<\/td>\r\n24.845<\/td>\r\n22.585<\/td>\r\n25.903<\/td>\r\n25.458<\/td>\r\n21.135<\/td>\r\n24.048<\/td>\r\n117-81-7<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
23<\/td>\r\nButyl-n<\/em>-decyl phthalate<\/td>\r\n—<\/td>\r\n27.362<\/td>\r\n25.268<\/td>\r\n22.657<\/td>\r\n26.888<\/td>\r\n26.410<\/td>\r\n21.404<\/td>\r\n24.471<\/td>\r\n89-19-0<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
24<\/td>\r\nDiphenyl phthalate<\/td>\r\n—<\/td>\r\n27.987<\/td>\r\n25.712<\/td>\r\n22.372<\/td>\r\n32.277<\/td>\r\n30.170<\/td>\r\n21.614<\/td>\r\n26.473<\/td>\r\n84-62-8<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
25<\/td>\r\nBis(4-methylcyclohexyl) phthalate isomer 1<\/td>\r\n—<\/td>\r\n28.003<\/td>\r\n25.922<\/td>\r\n23.016<\/td>\r\n29.547<\/td>\r\n28.476<\/td>\r\n21.677<\/td>\r\n25.923<\/td>\r\n59-43-8<\/td>\r\nIsomer mix<\/td>\r\n<\/tr>\r\n
26<\/td>\r\nBis(4-methylcyclohexyl) phthalate isomer 2<\/td>\r\n—<\/td>\r\n29.002<\/td>\r\n26.993<\/td>\r\n23.816<\/td>\r\n30.345<\/td>\r\n29.400<\/td>\r\n22.604<\/td>\r\n26.739<\/td>\r\n59-43-8<\/td>\r\nIsomer mix<\/td>\r\n<\/tr>\r\n
27<\/td>\r\nHexyl isodecyl phthalate<\/td>\r\n—<\/td>\r\n29.176<\/td>\r\n27.271<\/td>\r\n24.523<\/td>\r\n28.189<\/td>\r\n27.965<\/td>\r\n23.224<\/td>\r\n26.336<\/td>\r\n61702-81-6<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
28<\/td>\r\nBenzyl 2-ethylhexyl phthalate<\/td>\r\n—<\/td>\r\n29.791<\/td>\r\n27.781<\/td>\r\n24.747<\/td>\r\n31.498<\/td>\r\n30.216<\/td>\r\n23.219<\/td>\r\n27.594<\/td>\r\n27215-22-1<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
29<\/td>\r\nBis(4-methylcyclohexyl) phthalate isomer-3<\/td>\r\n—<\/td>\r\n29.964<\/td>\r\n28.034<\/td>\r\n24.617<\/td>\r\n31.189<\/td>\r\n30.285<\/td>\r\n23.498<\/td>\r\n27.559<\/td>\r\n59-43-8<\/td>\r\nIsomer mix<\/td>\r\n<\/tr>\r\n
30<\/td>\r\nBis(2-ethylhexyl) isophthalate<\/td>\r\n—<\/td>\r\n30.132<\/td>\r\n28.037<\/td>\r\n25.684<\/td>\r\n28.133<\/td>\r\n28.243<\/td>\r\n23.907<\/td>\r\n26.648<\/td>\r\n137-89-3<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
31<\/td>\r\nBis(2-(ethoxyethoxy)ethyl) phthalate<\/td>\r\n—<\/td>\r\n30.233<\/td>\r\n28.434<\/td>\r\n24.879<\/td>\r\n32.942<\/td>\r\n31.252<\/td>\r\n23.995<\/td>\r\n28.681<\/td>\r\n117-85-1<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
32<\/td>\r\nDi-n<\/em>-octyl phthalate*<\/td>\r\nEPA 8061A, EPA Priority, EU<\/td>\r\n31.562<\/td>\r\n29.626<\/td>\r\n26.796<\/td>\r\n30.475<\/td>\r\n30.328<\/td>\r\n24.915<\/td>\r\n28.455<\/td>\r\n117-84-0<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
33<\/td>\r\nn<\/em>-Hexyl decyl phthalate<\/td>\r\n—<\/td>\r\n31.680<\/td>\r\n29.748<\/td>\r\n26.878<\/td>\r\n30.788<\/td>\r\n30.450<\/td>\r\n24.994<\/td>\r\n28.566<\/td>\r\n25724-58-7<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n
34<\/td>\r\nDiphenyl isophthalate<\/td>\r\n—<\/td>\r\n32.362<\/td>\r\n29.850<\/td>\r\nN\/A<\/td>\r\n34.707<\/td>\r\n32.396<\/td>\r\n25.114<\/td>\r\n29.437<\/td>\r\n744-45-6<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
35<\/td>\r\nDibenzyl phthalate<\/td>\r\n—<\/td>\r\n33.234<\/td>\r\n30.725<\/td>\r\n27.141<\/td>\r\n37.396<\/td>\r\n35.372<\/td>\r\n25.501<\/td>\r\n31.359<\/td>\r\n523-31-9<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
36<\/td>\r\nDiisononyl phthalate<\/td>\r\nEU<\/td>\r\n33.684<\/td>\r\n31.802<\/td>\r\n28.779<\/td>\r\n32.500<\/td>\r\n32.708<\/td>\r\n27.391<\/td>\r\n30.811<\/td>\r\n68515-48-0<\/td>\r\nIsomer mix<\/td>\r\n<\/tr>\r\n
37<\/td>\r\nDi-n<\/em>-octyl isophthalate<\/td>\r\n—<\/td>\r\n34.483<\/td>\r\n32.463<\/td>\r\n29.168<\/td>\r\n32.035<\/td>\r\nN\/A<\/td>\r\n27.223<\/td>\r\n30.388<\/td>\r\n4654-18-6<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
38<\/td>\r\nDiisodecyl phthalate<\/td>\r\nEU<\/td>\r\n35.775<\/td>\r\n33.792<\/td>\r\n30.876<\/td>\r\n35.041<\/td>\r\nN\/A<\/td>\r\n29.11<\/td>\r\n32.169<\/td>\r\n26761-40-0<\/td>\r\nIsomer mix<\/td>\r\n<\/tr>\r\n
39<\/td>\r\nDinonyl phthalate*<\/td>\r\nEPA 8061A<\/td>\r\n36.159<\/td>\r\n34.103<\/td>\r\n30.994<\/td>\r\n34.609<\/td>\r\n34.705<\/td>\r\n28.867<\/td>\r\n32.604<\/td>\r\n84-76-4<\/td>\r\nNeat<\/td>\r\n<\/tr>\r\n
40<\/td>\r\nn<\/em>-Octyl-n<\/em>-decyl phthalate<\/td>\r\n—<\/td>\r\n36.182<\/td>\r\n34.170<\/td>\r\n30.961<\/td>\r\n34.664<\/td>\r\n34.7<\/td>\r\n28.861<\/td>\r\n32.628<\/td>\r\n119-07-3<\/td>\r\nTechnical<\/td>\r\n<\/tr>\r\n<\/tbody>\r\n<\/table>\r\n<\/figure>\n\n\n\n

Remarque : les zones gris\u00e9es indiquent les co\u00e9lutions (Rs<1,5).
*Ces compos\u00e9s se trouvent dans le m\u00e9lange d\u2019esters des phtalates 8061A de la m\u00e9thode EPA Restek (r\u00e9f. 33227).<\/p>\n\n\n\n

Tableau III :<\/strong> Conditions analytiques GC-MS<\/p>\n\n\n\n

Parameters<\/strong><\/th>Values for EPA EU List<\/strong><\/th>Values for Extended List<\/strong><\/th><\/tr><\/thead>
Inlet temperature (\u00b0C)<\/td>280<\/td>280<\/td><\/tr>
Injection volume (\u00b5L)<\/td>1.0<\/td>1.0<\/td><\/tr>
Liner<\/td>Restek Premium 3.5 mm Precision liner w\/ wool (cat.# 23320.1)<\/td>Restek Premium 3.5 mm Precision liner w\/ wool (cat.# 23320.1)<\/td><\/tr>
Oven temperature program<\/td>200 \u00b0C (hold 0.5 min) to 330 \u00b0C* at 30 \u00b0C\/min
(hold 1 min)<\/td>		150 \u00b0C (hold 0.8 min) to 200 \u00b0C at 5 \u00b0C\/min to 275 \u00b0C at 3 \u00b0C\/min
(hold 2 min)<\/td><\/tr>
Carrier gas: He control mode<\/td>Constant linear velocity: 66.7 cm\/sec @ 200 \u00b0C
(3 mL\/min**)<\/td>		Constant linear velocity: 48 cm\/sec @ 150 \u00b0C
(1.6 mL\/min)<\/td><\/tr>
Split ratio<\/td>20:1<\/td>20:1<\/td><\/tr>
Detector<\/td>MS<\/td>MS<\/td><\/tr>
Mode:<\/td>Full Scan (59\u2013400)<\/td>Full Scan (59\u2013400)<\/td><\/tr>
Transfer line temp.:<\/td>300 \u00b0C<\/td>300 \u00b0C<\/td><\/tr>
Scan event time<\/td>0.1 sec<\/td>0.1 sec<\/td><\/tr>
Analyzer type:<\/td>Quadrupole<\/td>Quadrupole<\/td><\/tr>
Source temp.:<\/td>280 \u00b0C<\/td>280 \u00b0C<\/td><\/tr>
Solvent delay time:<\/td>0.9 min<\/td>2.5 min<\/td><\/tr>
Tune type:  <\/td>PFTBA<\/td>PFTBA<\/td><\/tr>
Ionization mode:<\/td>EI<\/td>EI<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

**320 \u00b0C pour la colonne Rtx-50
**3 ml\/min peut \u00eatre trop \u00e9lev\u00e9 pour certains appareils. Consultez le manuel d\u2019utilisation de l\u2019appareil.<\/p>\n\n\n\n

M\u00eame si la GC-MS est la technique la plus couramment utilis\u00e9e, l\u2019analyse des phtalates peut \u00e9galement \u00eatre r\u00e9alis\u00e9e par GC-ECD. La m\u00e9thode EPA 8061A d\u00e9crit l\u2019identification et la quantification des phtalates dans des matrices aqueuses et solides avec deux colonnes mont\u00e9es en parall\u00e8le et deux d\u00e9tecteurs \u00e0 capture d\u2019\u00e9lectrons [8]. Les colonnes Rtx-440 et Rxi-35Sil MS r\u00e9pondent parfaitement aux exigences de cette m\u00e9thode. Le logiciel Pro\u00a0EZ<\/em>GC a permis d\u2019\u00e9tablir des conditions op\u00e9ratoires pour une analyse rapide avec la colonne Rtx-440. La colonne Rxi-35Sil MS s\u2019est av\u00e9r\u00e9e \u00eatre une excellente colonne de confirmation \u00e9tant donn\u00e9 les diff\u00e9rences dans l\u2019ordre d\u2019\u00e9lution observ\u00e9es. Les conditions analytiques en GC-ECD peuvent facilement \u00eatre adapt\u00e9es \u00e0 partir des m\u00e9thodes GC-MS d\u00e9crites dans le Tableau III en utilisant le translateur de m\u00e9thode en ligne gratuit Pro\u00a0EZ<\/em>GC Restek. <\/p>\n\n\n\n

Conclusion<\/h2>\n\n\n\n

Les performances des 7 colonnes GC les plus couramment utilis\u00e9es pour l\u2019analyse des phtalates ont \u00e9t\u00e9 compar\u00e9es en utilisant le programmePro EZ<\/em>GC, qui a grandement facilit\u00e9 l\u2019optimisation des conditions d\u2019analyse. La s\u00e9lectivit\u00e9 et l\u2019efficacit\u00e9 des colonnes Rtx-440 et Rxi-XLB ont garanti des temps d\u2019analyse courts pour l\u2019ensemble des phtalates \u00e9tudi\u00e9s. Consid\u00e9rant la bonne r\u00e9solution globale, les temp\u00e9ratures maximales autoris\u00e9es par leur excellente stabilit\u00e9 thermique (340 \u00b0C pour la colonne Rtx-440 et 360 \u00b0C pour la colonne Rxi-XLB [Tableau IV]), et leur tr\u00e8s faible “bleeding”, les colonnes Rtx-440 et Rxi-XLB s\u2019imposent pour l\u2019analyse GC-MS des phtalates. Les colonnes Rtx-440 et Rxi-35Sil MS utilis\u00e9es en parall\u00e8le sont recommand\u00e9es dans le cas d\u2019analyse par GC-ECD.<\/p>\n\n\n\n

Table IV :<\/strong> Temp\u00e9ratures maximales<\/p>\n\n\n\n

 <\/th>Rtx-440
(r\u00e9f. 12923)<\/strong><\/th>		Rxi-XLB
(r\u00e9f. 13723)<\/strong><\/th>		Rxi-5ms
(r\u00e9f. 13423)<\/strong><\/th>		Rtx-50
(r\u00e9f. 10523)<\/strong><\/th>		Rxi-35Sil MS
(r\u00e9f. 13823)<\/strong><\/th>		Rtx-CLPesticides
(r\u00e9f. 11123)<\/strong><\/th>		Rtx-CLPesticides2
(r\u00e9f. 11323)<\/strong><\/th><\/tr><\/thead>
Maximum Temperature (\u00b0C)<\/td>340<\/td>360<\/td>350<\/td>320<\/td>360<\/td>340<\/td>340<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Remerciements<\/h2>\n\n\n\n

Les auteurs remercient la soci\u00e9t\u00e9 Shimadzu Corporation pour son aide.<\/p>\n\n\n\n

R\u00e9f\u00e9rences<\/h2>\n\n\n\n
    \n
  1. H. Choi, J. Kim, Y. Im, S. Lee, Y. Kim, The association between some endocrine disruptors and hypospadias in biological samples. J. Environ. Sci. Health, Part A: Toxic\/Hazard. Subst. Environ. Eng. 47 (13) (2012) 2173\u20132179. http:\/\/www.ncbi.nlm.nih.gov\/pubmed\/22871016<\/strong><\/a><\/li>\n\n\n\n
  2. N. Nassar, P. Abeywardana, A. Barker, C. Bower, Parental occupational exposure to potential endocrine disrupting chemicals and risk of hypospadias in infants. Occup. Environ. Med. 67 (9) (2010) 585\u2013589. http:\/\/www.ncbi.nlm.nih.gov\/pubmed\/19939854<\/strong><\/a><\/li>\n\n\n\n
  3. L. Trasande, S. Sathyanarayana, A.J. Spanier, H. Trachtman, T.M. Attina, E.M. Urbina, Urinary phthalates are associated with higher blood pressure in childhood. J. Pediatr. 163 (3) (2013) 747\u2013753e1. http:\/\/www.ncbi.nlm.nih.gov\/pmc\/articles\/PMC4074773\/<\/strong><\/a><\/li>\n\n\n\n
  4. E.F. Werner, J.M. Braun, K. Yolton, J.C. Khoury, B.P. Lanphear, The association between maternal urinary phthalate concentrations and blood pressure in pregnancy: The HOME Study. Environ. Health 14 (2015) 75. http:\/\/www.ehjournal.net\/content\/14\/1\/75<\/strong><\/a><\/li>\n\n\n\n
  5. J.J. Jaakkola, T.L. Knight, The role of exposure to phthalates from polyvinyl chloride products in the development of asthma and allergies: A systematic review and meta-analysis. Environ. Health Perspect. 116 (7) (2008) 845\u2013853. http:\/\/www.ncbi.nlm.nih.gov\/pmc\/articles\/PMC2453150\/<\/strong><\/a><\/li>\n\n\n\n
  6. E.E. Hatch, J.W. Nelson, R.W. Stahlhut, T.F. Webster, Association of endocrine disruptors and obesity: Perspectives from epidemiological studies. Int. J. Androl. 33 (2) (2010) 324\u2013332. http:\/\/www.ncbi.nlm.nih.gov\/pubmed\/20113374<\/strong><\/a><\/li>\n\n\n\n
  7. S. Net, A. Delmont, R. Sempere, A. Paluselli, B. Ouddane, Reliable quantification of phthalates in environmental matrices (air, water, sludge, sediment and soil): A review. Sci. Total Environ. 515-516 (2015) 162\u2013180. http:\/\/www.ncbi.nlm.nih.gov\/pubmed\/25723871<\/strong><\/a><\/li>\n\n\n\n
  8. U.S. Environmental Protection Agency, Method 8061A, Phthalate Esters by Gas Chromatography with Electron Capture Detection (GC\/ECD), Rev. 1, December 1996. https:\/\/www.epa.gov\/sites\/production\/files\/2015-12\/documents\/8061a.pdf<\/strong><\/a><\/li>\n\n\n\n
  9. D. Li, Phthalate determination by dual column set in eight minutes, ChromaBLOGraphy, Restek Corporation, 2015.<\/li>\n<\/ol>\n\n\n
    Figure 1:<\/strong>\u00a0EPA- and EU-listed phthalates and internal standard (benzyl benzoate) are shown under full scan mode and selected ion scan mode (m\/z 293 and m\/z 307) on seven different GC stationary phases (see Table III for conditions).<\/div>
    \n\n

    Rtx-440<\/strong><\/p>\n\n\n

    \"EPA<\/div>

    GC_EV1408<\/p>

    Peaks<\/h4>\n
    <\/th>Peaks<\/th><\/tr><\/thead>\n
    1.<\/td>Dimethyl phthalate<\/a><\/td><\/tr>\n
    2.<\/td>Diethyl phthalate<\/a><\/td><\/tr>\n
    3.<\/td>Benzyl benzoate<\/a><\/td><\/tr>\n
    4.<\/td>Diisobutyl phthalate<\/a><\/td><\/tr>\n
    5.<\/td>Di-n-butyl phthalate<\/a><\/td><\/tr>\n
    6.<\/td>Bis(2-methoxyethyl) phthalate<\/a><\/td><\/tr>\n
    7.<\/td>Bis[4-methyl-2-pentyl] phthalate isomer 1<\/td><\/tr>\n
    8.<\/td>Bis[4-methyl-2-pentyl] phthalate isomer 2<\/a><\/td><\/tr>\n
    9.<\/td>Bis(2-ethoxyethyl) phthalate<\/a><\/td><\/tr>\n
    10.<\/td>Di-n-pentyl phthalate<\/a><\/td><\/tr>\n<\/tbody><\/table>\n\n
    <\/th>Peaks<\/th><\/tr><\/thead>
    11.<\/td>Di-n-hexyl phthalate<\/a><\/td><\/tr>\n
    12.<\/td>Butyl benzyl phthalate<\/a><\/td><\/tr>\n
    13.<\/td>Hexyl-2-ethylhexyl phthalate<\/a><\/td><\/tr>\n
    14.<\/td>Bis(2-butoxyethyl) phthalate<\/a><\/td><\/tr>\n
    15.<\/td>Bis(2-ethylhexyl) phthalate<\/a><\/td><\/tr>\n
    16.<\/td>Dicyclohexyl phthalate<\/a><\/td><\/tr>\n
    17.<\/td>Di-n-octyl phthalate<\/a><\/td><\/tr>\n
    18.<\/td>Diisononyl phthalate<\/a><\/td><\/tr>\n
    19.<\/td>Diisodecyl phthalate<\/a><\/td><\/tr>\n
    20.<\/td>Dinonyl phthalate<\/a><\/td><\/tr>\n<\/tbody><\/table><\/div>
    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n\n\n

    Rxi-XLB<\/strong><\/p>\n\n\n

    \"EPA<\/div>

    GC_EV1409<\/p>

    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n\n\n

    Rtx-CLPesticides<\/strong><\/p>\n\n\n

    \"EPA<\/div>

    GC_EV1414<\/p>

    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n\n\n

    Rxi-35Sil MS<\/strong><\/p>\n\n\n

    \"EPA<\/div>

    GC_EV1413<\/p>

    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n\n\n

    Rtx-50<\/strong><\/p>\n\n\n

    \"EPA<\/div>

    GC_EV1415<\/p>

    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n\n\n

    Rxi-5ms<\/strong><\/p>\n\n\n

    \"EPA<\/div>

    GC_EV1412<\/p>

    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n\n\n

    Rtx-CLPesticides2<\/strong><\/p>\n\n\n

    \"EPA<\/div>

    GC_EV1416<\/p>

    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n
    Figure 2:<\/strong>\u00a0Target compounds on the extended phthalate list (50 \u00b5g\/mL) are separated under full scan mode on an Rtx-440 column (see Table III for conditions).<\/div>
    \n
    \"Phthalates<\/div>

    GC_EV1407<\/p>

    Peaks<\/h4>\n
    <\/th>Peaks<\/th><\/tr><\/thead>\n
    1.<\/td>Dimethyl phthalate<\/a><\/td><\/tr>\n
    2.<\/td>Dimethyl isophthalate<\/a><\/td><\/tr>\n
    3.<\/td>Diethyl phthalate<\/a><\/td><\/tr>\n
    4.<\/td>Benzyl benzoate<\/a><\/td><\/tr>\n
    5.<\/td>Diisobutyl phthalate<\/a><\/td><\/tr>\n
    6.<\/td>Di-n-butyl phthalate<\/a><\/td><\/tr>\n
    7.<\/td>Bis(2-methoxyethyl) phthalate<\/a><\/td><\/tr>\n
    8.<\/td>Bis[4-methyl-2-pentyl] phthalate isomer 1<\/a><\/td><\/tr>\n
    9.<\/td>Bis[4-methyl-2-pentyl] phthalate isomer 2<\/a><\/td><\/tr>\n
    10.<\/td>Bis(2-ethoxyethyl) phthalate<\/a><\/td><\/tr>\n
    11.<\/td>Di-n-pentyl phthalate<\/a><\/td><\/tr>\n
    12.<\/td>Butyl cyclohexyl phthalate<\/a><\/td><\/tr>\n
    13.<\/td>Butyl 2-ethylhexyl phthalate<\/a><\/td><\/tr>\n<\/tbody><\/table>\n\n
    <\/th>Peaks<\/th><\/tr><\/thead>
    14.<\/td>Di-n-hexyl phthalate<\/a><\/td><\/tr>\n
    15.<\/td>Butyl octyl phthalate<\/a><\/td><\/tr>\n
    16.<\/td>Butyl benzyl phthalate<\/a><\/td><\/tr>\n
    17.<\/td>Hexyl-2-ethylhexyl phthalate<\/a><\/td><\/tr>\n
    18.<\/td>Butyl isodecyl phthalate<\/a><\/td><\/tr>\n
    19.<\/td>Bis(2-ethylhexyl)hexahydro phthalate<\/a><\/td><\/tr>\n
    20.<\/td>Bis(2-n-butoxyethyl) phthalate<\/a><\/td><\/tr>\n
    21.<\/td>Dicyclohexyl phthalate<\/a><\/td><\/tr>\n
    22.<\/td>Bis(2-ethylhexyl) phthalate<\/a><\/td><\/tr>\n
    23.<\/td>Butyl-n-decyl phthalate<\/a><\/td><\/tr>\n
    24.<\/td>Diphenyl phthalate<\/a><\/td><\/tr>\n
    25.<\/td>Bis(4-methylcyclohexyl) phthalate isomer 1<\/a><\/td><\/tr>\n
    26.<\/td>Bis(4-methylcyclohexyl) phthalate isomer 2<\/a><\/td><\/tr>\n<\/tbody><\/table>\n\n
    <\/th>Peaks<\/th><\/tr><\/thead>
    27.<\/td>Hexyl isodecyl phthalate<\/a><\/td><\/tr>\n
    28.<\/td>Benzyl 2-ethylhexyl phthalate<\/a><\/td><\/tr>\n
    29.<\/td>Bis(4-methylcyclohexyl) phthalate isomer 3<\/a><\/td><\/tr>\n
    30.<\/td>Bis(2-ethylhexyl) isophthalate<\/a><\/td><\/tr>\n
    31.<\/td>Bis(2-(ethoxyethoxy)ethyl) phthalate<\/a><\/td><\/tr>\n
    32.<\/td>Di-n-octyl phthalate<\/a><\/td><\/tr>\n
    33.<\/td>n-Hexyl decyl phthalate<\/a><\/td><\/tr>\n
    34.<\/td>Diphenyl isophthalate<\/a><\/td><\/tr>\n
    35.<\/td>Dibenzyl phthalate<\/a><\/td><\/tr>\n
    36.<\/td>Diisononyl phthalate<\/a><\/td><\/tr>\n
    37.<\/td>Di-n-octyl isophthalate<\/a><\/td><\/tr>\n
    38.<\/td>Diisodecyl phthalate<\/a><\/td><\/tr>\n
    39.<\/td>Dinonyl phthalate<\/a><\/td><\/tr>\n
    40.<\/td>n-Octyl n-decyl phthalate<\/a><\/td><\/tr>\n<\/tbody><\/table><\/div>
    <\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n\n
    <\/div>\n\n\n
    \n

    Products Mentioned<\/h3>\n
    \n
    \n
    \n
    \n Catalog No. 33227 <\/a> <\/div>\n
    \n
    Solution \u00e9talon d\u2019esters de phtalate EPA 8061A, 1000\u00a0\u00b5g\/ml, hexane:ac\u00e9tone (80:20), ampoule de 1\u00a0ml<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n
    \n
    \n Catalog No. 31847 <\/a> <\/div>\n
    \n
    Benzoate de benzyle (\u00e9talon interne), 5000\u00a0\u00b5g\/ml, hexane, ampoule de 1\u00a0ml<\/div>\n <\/div>\n
    \n Voir le produit<\/a>\n <\/div>\n <\/div>\n <\/div>\n <\/div>\n \n\n\n
    <\/div>\n","protected":false},"excerpt":{"rendered":"

    Cette note d’application compare les sept colonnes les plus couramment utilis\u00e9es pour l’analyse des phtalates. Les colonnes Rtx-440 et Rxi-XLB sont les choix privil\u00e9gi\u00e9s pour l’analyse GC-MS des phtalates en raison de leurs temps d’analyse rapides et de leur bonne r\u00e9solution pour les 18 phtalates r\u00e9glement\u00e9s et une liste \u00e9tendue de 40 compos\u00e9s. Pour les travaux de GC-ECD, deux colonnes (Rtx-440 et Rxi-35Sil MS) sont recommand\u00e9es.<\/p>\n","protected":false},"author":21,"featured_media":7081,"comment_status":"closed","ping_status":"open","sticky":false,"template":"","format":"standard","meta":{"_acf_changed":false,"_kad_blocks_custom_css":"","_kad_blocks_head_custom_js":"","_kad_blocks_body_custom_js":"","_kad_blocks_footer_custom_js":"","_kadence_starter_templates_imported_post":false,"_kad_post_transparent":"","_kad_post_title":"","_kad_post_layout":"","_kad_post_sidebar_id":"","_kad_post_content_style":"","_kad_post_vertical_padding":"","_kad_post_feature":"","_kad_post_feature_position":"","_kad_post_header":false,"_kad_post_footer":false,"footnotes":""},"categories":[782],"tags":[],"industries-application":[2208,2214],"post-badge":[],"resource-type":[],"product-library":[2456,2444],"resource-technique":[2316,2320],"ppma_author":[587,513,441],"class_list":["post-45301","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-notes-dapplication","industries-application-environnement","industries-application-industrie-agroalimentaire","product-library-colonnes-gc","product-library-produits-pour-la-chromatographie-en-phase-gazeuse","resource-technique-chromatographie-en-phase-gazeuse-gc","resource-technique-spectrometrie-de-masse-ms"],"acf":[],"taxonomy_info":{"category":[{"value":782,"label":"Notes 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d\u2019application","category_nicename":"notes-dapplication","category_parent":0}],"tag_info":false,"authors":[{"term_id":587,"user_id":0,"is_guest":1,"slug":"dan-li","display_name":"Dan Li","avatar_url":"https:\/\/secure.gravatar.com\/avatar\/?s=96&d=mm&r=g","0":null,"1":"","2":"","3":"","4":"","5":"","6":"","7":"","8":""},{"term_id":513,"user_id":0,"is_guest":1,"slug":"becca-stevens","display_name":"Rebecca Stevens","avatar_url":"https:\/\/secure.gravatar.com\/avatar\/?s=96&d=mm&r=g","0":null,"1":"","2":"","3":"","4":"","5":"","6":"","7":"","8":""},{"term_id":441,"user_id":21,"is_guest":0,"slug":"chris-english","display_name":"Chris 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