{"id":45307,"date":"2021-01-13T00:00:00","date_gmt":"2021-01-13T00:00:00","guid":{"rendered":"https:\/\/discover.restek.com\/uncategorized\/une-nouvelle-approche-pour-lanalyse-des-pfas-a-chaines-ultracourtes-dans-les-echantillons-deaux\/"},"modified":"2026-01-28T21:54:18","modified_gmt":"2026-01-28T21:54:18","slug":"une-nouvelle-approche-pour-lanalyse-des-pfas-a-chaines-ultracourtes-dans-les-echantillons-deaux","status":"publish","type":"post","link":"https:\/\/discover.restek.com\/fr\/notes-dapplication\/evan3220-fr\/une-nouvelle-approche-pour-lanalyse-des-pfas-a-chaines-ultracourtes-dans-les-echantillons-deaux","title":{"rendered":"Une nouvelle approche pour l\u2019analyse des PFAS \u00e0 cha\u00eenes ultracourtes dans les \u00e9chantillons d\u2019eaux"},"content":{"rendered":"\n

R\u00e9sum\u00e9<\/h2>\n\n\n\n

Le renforcement de la surveillance dans les eaux potables et non potables d\u2019un nombre plus important de PFAS oblige \u00e0 une m\u00e9thodologie plus efficace. Ici, nous avons d\u00e9velopp\u00e9 une approche unique permettant l\u2019analyse simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourtes (C2, C3), \u00e0 cha\u00eenes moyennes (C4 \u2013 C8), \u00e0 cha\u00eenes longues (> C8) et alternatifs, \u00e9liminant le besoin de m\u00e9thodes s\u00e9par\u00e9es. Les r\u00e9sultats des exp\u00e9riences sont pr\u00e9sent\u00e9s.<\/p>\n\n\n\n

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

Les substances per- et polyfluoroalkyl\u00e9es (PFAS) \u00e0 cha\u00eenes ultracourtes (C2 et C3) sont des petites mol\u00e9cules tr\u00e8s polaires qui contribuent \u00e0 plus de 40% du total des PFAS d\u00e9tect\u00e9s dans les eux environnementales (ex : eaux pluviales, eux fluviales, eaux souterraines) [1, 2, 3].
Les PFAS \u00e0 cha\u00eenes ultracourtes comprennent l\u2019acide trifluoroac\u00e9tique (TFA), l\u2019acide perfluoropropano\u00efque (PFPrA), le sulfonate de perfluoro\u00e9thane (PFEtS) et le sulfonate de perfluoropropane (PFPrS), le TFA \u00e9tant le plus pr\u00e9sent (abondant) et le plus difficile \u00e0 analyser par chromatographie. Les m\u00e9thodes actuelles de surveillance des PFAS ne traitent pas de ces nouveaux compos\u00e9s d\u2019int\u00e9r\u00eat \u00e0 cha\u00eenes ultracourtes en raison de leur r\u00e9tention insuffisante sur des colonnes de phase inverse. D\u2019autre part, les m\u00e9thodes analytiques par chromatographie d\u2019\u00e9change d\u2019anions ont souvent trop de r\u00e9tention et montrent de faibles performances chromatographiques pour les PFAS \u00e0 cha\u00eenes ultracourtes. Et le d\u00e9fi devient encore plus grand lorsque l\u2019on souhaite analyser simultan\u00e9ment les PFAS \u00e0 cha\u00eenes ultracourtes, \u00e0 cha\u00eenes longues et alternatifs sur une seule m\u00e9thode.<\/p>\n\n\n\n

Pour d\u00e9passer ces limites, nous avons utilis\u00e9 une nouvelle colonne hybride HILIC\/\u00c9change Ionique (Raptor Polar X) pour d\u00e9velopper une m\u00e9thode LC-MS\/MS simple et rapide pour l\u2019analyse des PFAS \u00e0 cha\u00eenes C2 \u00e0 C8 et des PFAS alternatifs. Gr\u00e2ce \u00e0 ses m\u00e9canismes multimodes de r\u00e9tention, la colonne permet l\u2019analyse simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourtes et \u00e0 cha\u00eenes longues, sur une seule et m\u00eame m\u00e9thode isocratique. Cette m\u00e9thode d\u2019injection directe a \u00e9t\u00e9 \u00e9valu\u00e9e par des analyses de pr\u00e9cision et de justesse d\u2019\u00e9chantillons d\u2019eaux dop\u00e9es (eau du robinet, eau fluviale, eau souterraine et eau provenant d\u2019ouvrages de travaux publics (effluents des eaux us\u00e9es). Comme d\u00e9montr\u00e9 ici, la m\u00e9thode fournit une configuration et des conditions favorables \u00e0 une haute cadence d\u2019analyse pour les laboratoires d\u2019analyses environnementales int\u00e9ress\u00e9s par l\u2019ajout des PFAS \u00e0 cha\u00eenes ultracourtes \u00e0 leur analyse actuelle des PFAS.<\/p>\n\n\n\n

Exp\u00e9rience<\/h2>\n\n\n\n

M\u00e9thode chromatographique :<\/h3>\n\n\n\n

Les conditions chromatographiques \u00e9taient les suivantes. Les transitions et le standard interne utilis\u00e9s pour chaque analyte sont indiqu\u00e9s
dans le Tableau I.<\/p>\n\n\n\n

Column:<\/td>Raptor Polar X (2.7 \u00b5m, 50 mm x 2.1 mm ID [cat.# 9311A52])<\/td><\/tr>
Column temp.:<\/td>40 \u00b0C<\/td><\/tr>
Injection volume:<\/td>10 \u00b5L<\/td><\/tr>
Mobile phase A:<\/td>Water, 10 mM ammonium formate, 0.05% formic acid<\/td><\/tr>
Mobile phase B:<\/td>Acetonitrile:methanol (60:40), 0.05% formic acid<\/td><\/tr>
 <\/td>Time (min)<\/td>%B<\/td><\/tr>
 <\/td>0.00<\/td>85<\/td><\/tr>
 <\/td>8.00<\/td>85<\/td><\/tr>
Flow rate:<\/td>0.5 mL\/min<\/td><\/tr>
Ion mode:<\/td>Negative ESI<\/td><\/tr>
Mode:<\/td>MRM<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Tableau I :<\/strong> Transitions MS des analytes pour l\u2019analyse simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourtes, \u00e0 cha\u00eenes longues, et alternatifs, dans les \u00e9chantillons d\u2019eaux.<\/p>\n\n\n\n

Analyte<\/strong><\/th>Ion Parent (Pr\u00e9curseur)<\/strong><\/th>Ion Fils (Produit)<\/strong><\/th>SI pour la Quantification<\/strong><\/th><\/tr><\/thead>
TFA<\/td>113.03<\/td>69.01<\/td>13<\/sup>C2<\/sub>-PFHxA<\/td><\/tr>
PFPrA<\/td>163.03<\/td>119.01<\/td>13<\/sup>C2<\/sub>-PFHxA<\/td><\/tr>
PFBA<\/td>212.97<\/td>168.97<\/td>13<\/sup>C2<\/sub>-PFHxA<\/td><\/tr>
PFHxA<\/td>312.97<\/td>268.90<\/td>13<\/sup>C2<\/sub>-PFHxA<\/td><\/tr>
PFOA<\/td>412.90<\/td>368.91<\/td>13<\/sup>C2<\/sub>-PFOA<\/td><\/tr>
HFPO-DA<\/td>284.97<\/td>168.92<\/td>13<\/sup>C2<\/sub>-PFOA<\/td><\/tr>
ADONA<\/td>376.90<\/td>250.93<\/td>13<\/sup>C2<\/sub>-PFOA<\/td><\/tr>
PFEtS<\/td>198.98<\/td>79.92<\/td>13<\/sup>C3<\/sub>-PFBS<\/td><\/tr>
PFPrS<\/td>248.97<\/td>79.98<\/td>13<\/sup>C3<\/sub>-PFBS<\/td><\/tr>
PFBS<\/td>298.97<\/td>79.97<\/td>13<\/sup>C3<\/sub>-PFBS<\/td><\/tr>
PFHxS<\/td>398.90<\/td>79.97<\/td>13<\/sup>C3<\/sub>-PFBS<\/td><\/tr>
PFOS<\/td>498.84<\/td>79.97<\/td>13<\/sup>C4<\/sub>-PFOS<\/td><\/tr>
9Cl-PF3ONS<\/td>530.78<\/td>350.85<\/td>13<\/sup>C4<\/sub>-PFOS<\/td><\/tr>
11Cl-PF3OUdS<\/td>630.78<\/td>450.80<\/td>13<\/sup>C4<\/sub>-PFOS<\/td><\/tr>
13<\/sup>C2<\/sub>-PFHxA<\/td>314.97<\/td>269.93<\/td>–<\/td><\/tr>
13<\/sup>C2<\/sub>-PFOA<\/td>414.90<\/td>369.87<\/td>–<\/td><\/tr>
13<\/sup>C3<\/sub>-PFBS<\/td>301.90<\/td>79.97<\/td>–<\/td><\/tr>
13<\/sup>C4<\/sub>-PFOS<\/td>502.84<\/td>79.97<\/td>–<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

Pr\u00e9paration des \u00e9chantillons<\/h3>\n\n\n\n

Dans un flacon en polypropyl\u00e8ne (utilis\u00e9 pour diminuer la contamination), 250 \u03bcL de chaque \u00e9chantillon d\u2019eau ont \u00e9t\u00e9 m\u00e9lang\u00e9s avec 250 \u03bcL de m\u00e9thanol et 5 \u03bcL d\u2019une solution de standards internes (10 ng\/mL de 13C2-PFHxA, 13C2-PFOA, 13C3-PFBS, 13C4-PFOS dans le m\u00e9thanol). Le flacon a \u00e9t\u00e9 ferm\u00e9 avec un bouchon en poly\u00e9thyl\u00e8ne cap (une fois de plus, pour r\u00e9duire la contamination) pour injection et analyse.<\/p>\n\n\n\n

Les standards utilis\u00e9s pour la calibration ont \u00e9t\u00e9 pr\u00e9par\u00e9s en utilisant de l\u2019eau d\u00e9sionis\u00e9e (g\u00e9n\u00e9r\u00e9e par un syst\u00e8me Thermo Scientific Barnstead E-Pure) et la dopant avec les 14 analytes sur une gamme de 10 \u00e0 800 ng\/L. Les solutions standards ont ensuite \u00e9t\u00e9 dilu\u00e9es 1:1 dans du m\u00e9thanol en suivant la proc\u00e9dure de pr\u00e9paration d\u2019\u00e9chantillon ci-dessus.<\/p>\n\n\n\n

Un \u00e9chantillon d\u2019eau du robinet provenant des installations Restek et trois \u00e9chantillons d\u2019eaux (eau fluviale de Chicago, eau souterraine et eau d\u2019effluents) fournis par l\u2019Agence Am\u00e9ricaine de Protection de l\u2019Environnement (U.S. EPA) ont \u00e9t\u00e9 dop\u00e9s \u00e0 40 et 160 ppt. Les blancs et les \u00e9chantillons d\u2019eau dop\u00e9s ont \u00e9t\u00e9 dilu\u00e9s 1:1 dans du m\u00e9thanol (comme d\u00e9crit ci-dessus) avant analyse chromatographique et quantification gr\u00e2ce aux standards. Pour l\u2019analyse du TFA dans l\u2019eau souterraine, l\u2019\u00e9chantillon a \u00e9t\u00e9 dilu\u00e9 cinq fois avec de l\u2019eau d\u00e9sionis\u00e9e avant d\u2019\u00eatre dop\u00e9 \u00e0 40 et 160 ppt, en raison de sa concentration \u00e9lev\u00e9e en TFA.<\/p>\n\n\n\n

<\/div>\n\n\n\n

R\u00e9sultats & Discussion<\/h2>\n\n\n\n

Performances Chromatographiques<\/h3>\n\n\n\n

Une m\u00e9thode isocratique a \u00e9t\u00e9 d\u00e9velopp\u00e9e permettant une analyse simple, rapide, et surtout simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourtes, \u00e0 cha\u00eenes longues et alternatifs, dans les \u00e9chantillons d\u2019eaux. Tous les analytes sont \u00e9lu\u00e9s en 4 minutes, avec une r\u00e9tention \u00e9quilibr\u00e9e et de bonnes formes de pics (Figure 1). Aucune interf\u00e9rence provenant des matrices n\u2019a \u00e9t\u00e9 observ\u00e9e dans aucun des \u00e9chantillons d\u2019eau en utilisant un cycle de 8 minutes. Comme cela sera discut\u00e9 ci-dessous, le palier d\u2019environ 4 minutes apr\u00e8s le dernier compos\u00e9 \u00e9lu\u00e9 s\u2019est av\u00e9r\u00e9 n\u00e9cessaire pour \u00e9viter d\u2019\u00e9ventuelles interf\u00e9rences provenant des matrices.<\/p>\n\n\n

Figure 1 :<\/strong>\u00a0Chromatogramme d\u2019un standard \u00e0 400 ng\/l.<\/div>
\n
\"Ultrashort-<\/div>

LC_EV0569<\/p>

Peaks<\/h4>\n
<\/th>Peaks<\/th>tR<\/sub> (min)<\/th>Conc.
(ng\/L)<\/th>		Precursor Ion<\/th>Product Ion<\/th><\/tr><\/thead>\n
1.<\/td>11-Chloroeicosafluoro-3-oxanonane-1-sulfonate (11CL-PF3OUdS)<\/td>1.25<\/td>400<\/td>630.78<\/td>450.80<\/td><\/tr>\n
2.<\/td>9-Chlorohexadecafluoro-3-oxanonane-1-sulfonate (9Cl-PF3ONS)<\/td>1.34<\/td>400<\/td>530.78<\/td>350.85<\/td><\/tr>\n
3.<\/td>Perfluorooctanesulfonic acid (PFOS)<\/a><\/td>1.38<\/td>400<\/td>498.84<\/td>79.97<\/td><\/tr>\n
4.<\/td>Perfluorohexanesulfonic acid (PFHxS)<\/a><\/td>1.49<\/td>400<\/td>398.90<\/td>79.97<\/td><\/tr>\n
5.<\/td>Perfluorobutanesulfonic acid (PFBS)<\/a><\/td>1.64<\/td>400<\/td>298.97<\/td>79.97<\/td><\/tr>\n
6.<\/td>Perfluoropropanesulfonic acid (PFPrS)<\/td>1.73<\/td>400<\/td>248.97<\/td>79.98<\/td><\/tr>\n
7.<\/td>Perfluoroethanesulfonic acid (PFEtS)<\/td>1.86<\/td>400<\/td>198.98<\/td>79.92<\/td><\/tr>\n<\/tbody><\/table>\n\n
<\/th>Peaks<\/th>tR<\/sub> (min)<\/th>Conc.
(ng\/L)<\/th>		Precursor Ion<\/th>Product Ion<\/th><\/tr><\/thead>
8.<\/td>Hexafluoropropylene oxide dimer acid (HFPO-DA)<\/a><\/td>2.06<\/td>400<\/td>284.97<\/td>168.92<\/td><\/tr>\n
9.<\/td>Perfluorooctanoic acid (PFOA)<\/a><\/td>2.11<\/td>400<\/td>412.90<\/td>368.91<\/td><\/tr>\n
10.<\/td>Ammonium 4,8-dioxa-3H-perfluorononanoate (ADONA)<\/a><\/td>2.15<\/td>400<\/td>376.90<\/td>250.93<\/td><\/tr>\n
11.<\/td>Perfluorohexanoic acid (PFHxA)<\/a><\/td>2.36<\/td>400<\/td>312.97<\/td>268.90<\/td><\/tr>\n
12.<\/td>Perfluorobutanoic acid (PFBA)<\/a><\/td>2.76<\/td>400<\/td>212.97<\/td>168.97<\/td><\/tr>\n
13.<\/td>Perfluoropropionic acid (PFPrA)<\/td>3.06<\/td>400<\/td>163.03<\/td>119.01<\/td><\/tr>\n
14.<\/td>Trifluoroacetic acid (TFA)<\/a><\/td>3.77<\/td>400<\/td>113.03<\/td>69.01<\/td><\/tr>\n<\/tbody><\/table><\/div>

Conditions<\/h4>
Column<\/th>Raptor Polar X (cat.# 9311A52<\/a>)<\/td><\/tr>
Dimensions:<\/th>50 mm x 2.1 mm ID<\/td><\/tr>
Particle Size:<\/th>2.7 \u00b5m<\/td><\/tr>
<\/td>
Temp.:<\/th>40 \u00b0C<\/td><\/tr>
Standard\/Sample<\/th><\/td><\/tr>
Diluent:<\/th>50:50 Water:methanol<\/td><\/tr>
Conc.:<\/th>400 ng\/L<\/td><\/tr><\/td><\/tr>
Inj. Vol.:<\/th>10 \u00b5L <\/td><\/tr>
Mobile Phase<\/th><\/td><\/tr>
A:<\/th>Water, 10 mM ammonium formate, 0.05% formic acid <\/td><\/tr>
B:<\/th>60:40 Acetonitrile:methanol, 0.05% formic acid <\/td><\/tr>
<\/td>
Time (min)<\/th>Flow (mL\/min)<\/th>%A<\/th>%B<\/th><\/tr><\/thead>
0.00<\/td>0.5<\/td>15<\/td>85<\/td><\/tr>
8.00<\/td>0.5<\/td>15<\/td>85<\/td><\/tr><\/tbody><\/table><\/td><\/tr><\/table>
Detector<\/th>MS\/MS<\/td><\/tr>
Ion Mode:<\/th>ESI- <\/td><\/tr>
Mode:<\/th>MRM <\/td><\/tr>
Instrument<\/th>UHPLC<\/td><\/tr><\/table><\/div><\/div><\/div>
<\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n\n
<\/div>\n\n\n\n

Lin\u00e9arit\u00e9<\/h3>\n\n\n\n

La gamme d\u2019\u00e9talonnage est de 20 \u00e0 800 ppt pour le TFA et de 10 \u00e0 800 ppt pour les autres analytes. Quatre standards internes ont \u00e9t\u00e9 \u00e9valu\u00e9s pour d\u00e9terminer la courbe d\u2019\u00e9talonnage la plus appropri\u00e9e pour les diff\u00e9rents analytes. Tous les composes ont montr\u00e9 une lin\u00e9arit\u00e9 acceptable avec des valeurs de r2 >0.996 et des \u00e9carts <20% (en utilisant une r\u00e9gression quadratique pond\u00e9r\u00e9 1\/x).<\/p>\n\n\n\n

Justesse et Pr\u00e9cision<\/h3>\n\n\n\n

Dans nos exp\u00e9riences initiales, une interf\u00e9rence matricielle a \u00e9t\u00e9 observ\u00e9e ai niveau du signal du TFA, lorsque les \u00e9chantillons d\u2019eaux \u00e9taient analys\u00e9s en utilisant un cycle isocratique de 5 minutes.<\/p>\n\n\n\n

Diff\u00e9rents temps d\u2019analyse ont \u00e9t\u00e9 test\u00e9s et il a \u00e9t\u00e9 d\u00e9termin\u00e9 qu\u2019un cycle de 8 minutes \u00e9tait n\u00e9cessaire pour \u00e9viter ces interf\u00e9rences provenant des matrices. La dur\u00e9e du palier isocratique peut devoir \u00eatre modifi\u00e9e en fonction de l\u2019instrumentation utilis\u00e9e et\/ou des \u00e9chantillons \u00e0 analyser.<\/p>\n\n\n\n

Les blancs ont montr\u00e9 divers niveaux de TFA et des PFAS en C3, C4, C6, et C8, sans ADONA, HFPO-DA, 9Cl-PF3ONS et 11Cl-PF3OUdS d\u00e9tectables (Tableau II). Un exemple d\u2019un chromatogramme pour l\u2019analyse simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourte, \u00e0 cha\u00eenes longues et alternatifs, dans un \u00e9chantillon blanc d\u2019eau d\u2019effluents, est montr\u00e9 en Figure 2.<\/p>\n\n\n\n

Tableau II :<\/strong> Analytes d\u00e9tectables dans les \u00e9chantillons blancs<\/p>\n\n\n\n

 <\/th> <\/th>Detected Concentration (ng\/L)<\/strong><\/th><\/tr><\/thead>
Samples<\/strong><\/td>TFA<\/strong><\/td>PFPrA<\/strong><\/td>PFBA<\/strong><\/td>PFHxA<\/strong><\/td>PFOA<\/strong><\/td>HFPO-DA<\/strong><\/td>ADONA<\/strong><\/td>PFEtS<\/strong><\/td>PFPrS<\/strong><\/td>PFBS<\/strong><\/td>PFHxS<\/strong><\/td>PFOS<\/strong><\/td>9Cl-PF3ONS<\/strong><\/td>11Cl-PF3OUdS<\/strong><\/td><\/tr>
Tap Water<\/td>164.2<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td><\/tr>
River Water<\/td>193.3<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td><\/tr>
Groundwater<\/td>1425<\/td>ND<\/td>ND<\/td>ND<\/td>5.4<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>6.7<\/td>3.9<\/td>ND<\/td>ND<\/td>ND<\/td><\/tr>
POTW Water<\/td>352.8<\/td>9.6<\/td>15.3<\/td>93.5<\/td>20.4<\/td>ND<\/td>ND<\/td>ND<\/td>ND<\/td>6.8<\/td>6.7<\/td>9.6<\/td>ND<\/td>ND<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

ND: non-detectable<\/p>\n\n\n

Figure 2:<\/strong>\u00a0Detectable PFAS in blank POTW water.<\/div>
\n
\"Detectable<\/div>

LC_EV0572<\/p>

Peaks<\/h4>\n
<\/th>Peaks<\/th>tR<\/sub> (min)<\/th>Precursor Ion<\/th>Product Ion<\/th><\/tr><\/thead>\n
1.<\/td>Perfluorooctanesulfonic acid (PFOS)<\/a><\/td>1.35<\/td>498.84<\/td>79.97<\/td><\/tr>\n
2.<\/td>Perfluorohexanesulfonic acid (PFHxS)<\/a><\/td>1.45<\/td>398.90<\/td>79.97<\/td><\/tr>\n
3.<\/td>Perfluorobutanesulfonic acid (PFBS)<\/a><\/td>1.58<\/td>298.97<\/td>79.97<\/td><\/tr>\n
4.<\/td>Perfluorooctanoic acid (PFOA)<\/a><\/td>2.05<\/td>412.90<\/td>368.91<\/td><\/tr>\n
5.<\/td>Perfluorohexanoic acid (PFHxA)<\/a><\/td>2.34<\/td>312.97<\/td>268.90<\/td><\/tr>\n
6.<\/td>Perfluorobutanoic acid (PFBA)<\/a><\/td>2.76<\/td>212.97<\/td>168.97<\/td><\/tr>\n
7.<\/td>Perfluoropropionic acid (PFPrA)<\/td>3.06<\/td>163.03<\/td>119.01<\/td><\/tr>\n
8.<\/td>Trifluoroacetic acid (TFA)<\/a><\/td>3.78<\/td>113.03<\/td>69.01<\/td><\/tr>\n<\/tbody><\/table><\/div>

Conditions<\/h4>
Column<\/th>Raptor Polar X (cat.# 9311A52<\/a>)<\/td><\/tr>
Dimensions:<\/th>50 mm x 2.1 mm ID<\/td><\/tr>
Particle Size:<\/th>2.7 \u00b5m<\/td><\/tr>
<\/td>
Temp.:<\/th>40 \u00b0C<\/td><\/tr>
Standard\/Sample<\/th><\/td><\/tr>
Diluent:<\/th>Methanol<\/td><\/tr>
Conc.:<\/th> Endogenous levels<\/td><\/tr><\/td><\/tr>
Inj. Vol.:<\/th>10 \u00b5L <\/td><\/tr>
Mobile Phase<\/th><\/td><\/tr>
A:<\/th>Water, 10 mM ammonium formate, 0.05% formic acid <\/td><\/tr>
B:<\/th> Acetonitrile:methanol (60:40), 0.05% formic acid <\/td><\/tr>
<\/td>
Time (min)<\/th>Flow (mL\/min)<\/th>%A<\/th>%B<\/th><\/tr><\/thead>
0.00<\/td>0.5<\/td>15<\/td>85<\/td><\/tr>
8.00<\/td>0.5<\/td>15<\/td>85<\/td><\/tr><\/tbody><\/table><\/td><\/tr><\/table>
Detector<\/th>MS\/MS<\/td><\/tr>
Ion Mode:<\/th>ESI- <\/td><\/tr>
Mode:<\/th>MRM <\/td><\/tr>
Instrument<\/th>UHPLC<\/td><\/tr>
Sample Preparation<\/th>In a polypropylene vial, 250 \u03bcL of blank POTW water was mixed with 250 \u03bcL of methanol and 5 \u03bcL of internal standard solution (10 ng\/mL of 13<\/sup>C2<\/sub>-PFHxA, 13<\/sup>C2<\/sub>-PFOA, 13<\/sup>C3<\/sub>-PFBS, and 13<\/sup>C4<\/sub>-PFOS in methanol). The vial was capped with a polyethylene cap for injection analysis.<\/td><\/tr><\/table><\/div><\/div><\/div>
<\/path><\/g><\/path><\/g><\/svg>Download PDF<\/a><\/div><\/div><\/div>\n<\/div><\/div><\/div>\n\n\n
<\/div>\n\n\n\n

Pour d\u00e9terminer la justesse (pourcentage de rendement), les quantit\u00e9s mesur\u00e9es dans les \u00e9chantillons dopes ont \u00e9t\u00e9 ajust\u00e9s pour tenir compte de la concentration dans les blancs. Les \u00e9chantillons d\u2019eaux ont \u00e9t\u00e9 dop\u00e9s \u00e0 faible et forte concentration, en double, pour chaque s\u00e9rie analytique. Trois s\u00e9ries analytiques ont \u00e9t\u00e9 mesur\u00e9es sur des jours diff\u00e9rents. Le tableau III montre les r\u00e9sultats de justesse et pr\u00e9cision calcul\u00e9s \u00e0 partir des trois s\u00e9ries de donn\u00e9es. La justesse de la m\u00e9thode dans les \u00e9chantillons d\u2019eaux a \u00e9t\u00e9 d\u00e9montr\u00e9e par des valeurs de rendement se situant \u00e0 moins de 30% de la concentration nominale pour les niveaux dop\u00e9s et de limite de quantification. L\u2019\u00e9cart-type relative \u00e9tait <20%, montrant une pr\u00e9cision de m\u00e9thode acceptable pour l\u2019analyse simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourtes, \u00e0 cha\u00eenes longues et alternatifs, dans les \u00e9chantillons d\u2019eaux.<\/p>\n\n\n\n

Tableau III :<\/strong> Pr\u00e9cision et Justesse de la M\u00e9thode<\/p>\n\n\n\n

 <\/td>%Pr\u00e9cision Moyen (%RSD)<\/strong><\/td><\/tr>
Matrices<\/strong><\/td>Eau du robinet<\/strong><\/td>Eau fluviale<\/strong><\/td>Eau souterraine**<\/strong><\/td>Eau d\u2019effluents (POTW)<\/strong><\/td>Eau d\u00e9ionis\u00e9e<\/strong><\/td><\/tr>
Conc. (ng\/L)<\/strong><\/td>40<\/strong><\/td>160<\/strong><\/td>40<\/strong><\/td>160<\/strong><\/td>40<\/strong><\/td>160<\/strong><\/td>40<\/strong><\/td>160<\/strong><\/td>10*
(LLOQ)<\/strong><\/td><\/tr>
TFA<\/strong><\/td>106 (16.9)<\/td>97.9 (7.10)<\/td>97.4 (10.8)<\/td>97.6 (6.12)<\/td>97.5 (14.5)<\/td>103 (8.87)<\/td>102 (17.1)<\/td>96.4 (7.33)<\/td>107
(3.55)<\/td><\/tr>
PFPrA<\/strong><\/td>95.1 (4.08)<\/td>105 (3.48)<\/td>94.5 (6.85)<\/td>104 (2.36)<\/td>103 (9.37)<\/td>105 (8.34)<\/td>91.8 (4.90)<\/td>104 (7.09)<\/td>109
(1.61)<\/td><\/tr>
PFBA<\/strong><\/td>106 (6.80)<\/td>117 (3.18)<\/td>105
(7.40)<\/td>		114 (4.91)<\/td>111 (2.48)<\/td>120 (3.27)<\/td>106 (6.58)<\/td>114 (4.85)<\/td>104
(4.91)<\/td><\/tr>
PFHxA<\/strong><\/td>93.3 (7.41)<\/td>111 (2.61)<\/td>91.8 (11.34)<\/td>103 (4.55)<\/td>102 (6.62)<\/td>109 (7.11)<\/td>103 (8.37)<\/td>108 (3.13)<\/td>115
(1.64)<\/td><\/tr>
PFOA<\/strong><\/td>100 (4.24)<\/td>107 (3.14)<\/td>103
(6.71)<\/td>		105 (2.64)<\/td>92.6 (3.85)<\/td>107 (3.09)<\/td>102 (4.57)<\/td>109 (3.64)<\/td>106
(3.28)<\/td><\/tr>
HFPO-DA<\/strong><\/td>95.7 (11.9)<\/td>108 (9.05)<\/td>86.6 (8.97)<\/td>104 (5.45)<\/td>94.1 (18.6)<\/td>105 (9.35)<\/td>95.2 (8.49)<\/td>106 (9.23)<\/td>102
(16.8)<\/td><\/tr>
ADONA<\/strong><\/td>106 (3.75)<\/td>116 (2.38)<\/td>100
(6.86)<\/td>		110 (4.59)<\/td>104 (4.91)<\/td>113 (5.23)<\/td>111 (5.26)<\/td>115 (2.65)<\/td>105
(4.76)<\/td><\/tr>
PFEtS<\/strong><\/td>94.8 (9.68)<\/td>110 (5.39)<\/td>89.4 (7.43)<\/td>102 (9.76)<\/td>96.5 (4.09)<\/td>108 (6.11)<\/td>104 (8.18)<\/td>109 (5.23)<\/td>99.8
(9.85)<\/td><\/tr>
PFPrS<\/strong><\/td>104 (4.97)<\/td>115 (4.19)<\/td>95.0 (3.87)<\/td>107 (4.26)<\/td>106 (10.6)<\/td>114 (3.36)<\/td>111 (4.88)<\/td>114 (2.96)<\/td>108
(3.28)<\/td><\/tr>
PFBS<\/strong><\/td>97.4 (10.1)<\/td>113 (3.97)<\/td>93.6 (5.24)<\/td>104 (4.19)<\/td>97.8 (4.47)<\/td>107 (4.23)<\/td>94.1 (10.7)<\/td>108 (4.48)<\/td>100
(11.0)<\/td><\/tr>
PFHxS<\/strong><\/td>99.4 (15.7)<\/td>114 (3.56)<\/td>94.3 (9.79)<\/td>104 (5.28)<\/td>95.2 (5.63)<\/td>112 (3.20)<\/td>104 (8.19)<\/td>111 (4.07)<\/td>107
(11.7)<\/td><\/tr>
PFOS<\/strong><\/td>104 (7.54)<\/td>107 (7.69)<\/td>103
(8.43)<\/td>		105 (7.23)<\/td>97.3 (14.9)<\/td>110 (4.84)<\/td>109 (7.47)<\/td>108 (7.53)<\/td>102
(4.20)<\/td><\/tr>
9Cl-PF3ONS<\/strong><\/td>98.7 (3.52)<\/td>105 (8.35)<\/td>91.8 (7.66)<\/td>103 (5.68)<\/td>94.7 (9.83)<\/td>105 (8.90)<\/td>105 (6.76)<\/td>107 (8.27)<\/td>107
(4.31)<\/td><\/tr>
11Cl-PF3OUdS<\/strong><\/td>106 (10.1)<\/td>113 (3.54)<\/td>95.0 (3.52)<\/td>113 (8.15)<\/td>107 (6.61)<\/td>112 (4.54)<\/td>119 (4.25)<\/td>120 (9.10)<\/td>98.2
(11.3)<\/td><\/tr><\/tbody><\/table><\/figure>\n\n\n\n

*LLOQ de 20 ng\/L pour le TFA<\/p>\n\n\n\n

**L\u2019eau souterraine a \u00e9t\u00e9 dilu\u00e9e 5 fois uniquement pour le TFA<\/p>\n\n\n\n

<\/div>\n\n\n\n

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

Une m\u00e9thode isocratique simple a \u00e9t\u00e9 d\u00e9velopp\u00e9e pour l\u2019analyse simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourtes, \u00e0 cha\u00eenes longues et alternatifs, dans les \u00e9chantillons d\u2019eaux. Gr\u00e2ce aux diff\u00e9rents m\u00e9canismes d\u2019interaction et de r\u00e9tention entre ces analytes et la colonne Raptor Polar X (2.7 \u03bcm) de 2.1 x 50 mm, la m\u00e9thode analytique s\u2019est d\u00e9montr\u00e9e \u00eatre rapide, robuste et sensible avec une pr\u00e9cision et une justesse acceptables. Cette m\u00e9thode est parfaite pour les laboratoires d\u2019analyse souhaitant d\u00e9velopper leurs dosages actuels de PFAS dans les eaux potables et non potables en y incluant les compos\u00e9s en C2 et C3.<\/p>\n\n\n\n

<\/div>\n\n\n\n

R\u00e9f\u00e9rences<\/h2>\n\n\n\n
    \n
  1. S. Taniyasu, K. Kannan, L.W.Y. Yeung, K.Y. Kwok, P.K.S Lam, N. Yamashita, Analysis of trifluoroacetic acid and other short-chain perfluorinated acids (C2-C4) in precipitation by liquid chromatography-tandem mass spectrometry: comparison to patterns of long-chain perfluorinated acids (C5-C18), Anal. Chim. Acta. 619 (2008) 221-230. https:\/\/pubmed.ncbi.nlm.nih.gov\/18558116\/<\/a><\/li>\n\n\n\n
  2. J. Janda, K. Nodler, H-J. Brauch, C. Zwiener, F.T. Lange, Robust trace analysis of polar (C2-C8) perfluorinated carboxylic acids by liquid chromatography-tandem mass spectrometry: method development and application to surface water, groundwater, and drinking water, Environ. Sci. Pollut.R. 26 (2018) 7326-7336. https:\/\/pubmed.ncbi.nlm.nih.gov\/29557039\/<\/a><\/li>\n\n\n\n
  3. K.Y. Kwok, S. Taniyasu, L.W.Y. Yeung, M.B. Murphy, P.K.S. Lam, Y. Horii, K. Kannan, G. Petrick, R.K. Sinha, N. Yamashita, Flux of perfluorinated chemicals through wet deposition in Japan, the United States, and other countries, Environ. Sci. Technol. 44 (2010) 7043-7049. https:\/\/pubmed.ncbi.nlm.nih.gov\/20795671\/<\/a><\/li>\n<\/ol>\n\n\n\n
    <\/div>\n\n\n
    \n

    Products Mentioned<\/h3>\n
    \n
    \n
    \n
    \n Catalog No. 9311A52 <\/a> <\/div>\n
    \n
    Colonne LC Raptor Polar X, 2.7\u00b5m, 50×2.1mm<\/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":"

    L’approche unique \u00e9tablie ici permet l\u2019analyse simultan\u00e9e des PFAS \u00e0 cha\u00eenes ultracourtes (C2, C3), \u00e0 cha\u00eenes moyennes (C4 \u2013 C8), \u00e0 cha\u00eenes longues (> C8) et alternatifs dans les eaux potables et non potables. Cette m\u00e9thode d\u2019injection directe a \u00e9t\u00e9 \u00e9valu\u00e9e par des analyses de pr\u00e9cision et de justesse d\u2019\u00e9chantillons d\u2019eaux dop\u00e9es.<\/p>\n","protected":false},"author":46,"featured_media":6535,"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":[2212,2210,2208,2758],"post-badge":[],"resource-type":[],"product-library":[2463,2446,2471,2445],"resource-technique":[2318,2362],"ppma_author":[578],"class_list":["post-45307","post","type-post","status-publish","format-standard","has-post-thumbnail","hentry","category-notes-dapplication","industries-application-analyse-de-pfas","industries-application-eau-potable-eaux-usees","industries-application-environnement","industries-application-semivolatiles","product-library-colonnes-lc","product-library-etalons-de-reference","product-library-etalons-en-solution","product-library-produits-pour-la-chromatographie-en-phase-liquide","resource-technique-chromatographie-en-phase-liquide","resource-technique-ms-ms-fr"],"acf":[],"taxonomy_info":{"category":[{"value":782,"label":"Notes 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