Trends of Perfluorinated Alkyl Substances in Herring Gull Eggs from Two Coastal. Colonies in Northern Norway:
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1 SUPPORTING INFORMATION Trends of Perfluorinated Alkyl Substances in Herring Gull Eggs from Two Coastal Colonies in Northern Norway: Jonathan Verreault, Urs Berger,#, *, Geir W. Gabrielsen Norwegian Polar Institute, Tromsø, NO-996, Norway Department of Applied Environmental Science, Stockholm University, Stockholm, SE , Sweden # Norwegian Institute for Air Research, Tromsø, NO-996, Norway * Corresponding author phone: ; fax: ; address: urs.berger@itm.su.se (U. Berger). 1
2 TABLE S1. Analytical standard compounds used in this study and selected instrumental parameters for quantification of each compound. Compound Abbreviation Obtained as Supplier Perfluorobutane sulfonate PFBS Potassium salt Donation from Dyneon Belgium N.V. Cone voltage [V] Q-ToF-HRMS Triple quadrupole MS-MS Quantification mass [m/z] Perfluorohexane sulfonate PFHxS Potassium salt Interchim a Perfluorooctane sulfonate PFOS Potassium salt Fluka b Perfluorodecane sulfonate PFDcS Ammonium salt % (weight) in - butoxyethanol in water (7%) Sigma-Aldrich c : Fluorotelomer sulfonate 6: FTS Sulfonic acid Interchim a Perfluorooctane sulfonamide PFOSA - ABCR d Perfluoro-n-octane 18 O-sulfonate 18 O -PFOS Ammonium salt Donation from the M Company Cone voltage [V] MRM precursor product mass [m/z] Perfluorohexanoate PFHxA Carboxylic acid Fluka b Perfluoroheptanoate PFHpA Carboxylic acid Sigma-Aldrich c Perfluorooctanoate PFOA Carboxylic acid Sigma-Aldrich c Perfluorononanoate PFNA Carboxylic acid Sigma-Aldrich c Perfluorodecanoate PFDcA Carboxylic acid Fluka b Perfluoroundecanoate PFUnA Carboxylic acid Sigma-Aldrich c Perfluorododecanoate PFDoA Carboxylic acid Sigma-Aldrich c e Perfluorotridecanoate PFTriA e Perfluorotetradecanoate PFTeA Carboxylic acid Sigma-Aldrich c e Perfluoropentadecanoate PFPeA e ,,,- 1 C-Perfluoro-n-octanoate f 1 C-PFOA Carboxylic acid Wellington g H-Perfluoroheptanoate h 7H-PFHpA Carboxylic acid ABCR d a Interchim, Montluçon Cedex, France. b Fluka, Buchs, Switzerland. c Sigma-Aldrich, Stockholm, Sweden. d ABCR, Karlsruhe, Germany. 6 e PFTriA and PFPeA were not commercially available at the time of the study. Quantification was done on the basis of extrapolated response factors from PFDoA and 7 PFTeA. Later verification with the commercially available PFTriA (Wellington g ) showed that the interpolation was valid. 8 f used as internal (surrogate) standard (IS). 9 g Wellington, Guelph, ON, Canada. 10 h used as recovery internal (volume) standard (RIS). Collision energy [ev]
3 6 TABLE S. Method limits of quantification (MLOQs, pg/g ww), mean (± 1 standard error) a concentrations (pg/g ww) of individual perfluorinated alkyl substances and sums (Σ) of closely-related compounds in herring gull eggs collected between 198 and 00 from two colonies in Northern Norway MLOQs 6: FTS 161 <161 <161 <161 <161 <161 <161 PFOSA < 88 ± 8 6 ± 6 ± 1 ± 0 ± Perfluorosulfonates PFBS 9 <9 <9 <9 <9 <9 <9 PFHxS 1 ± 9 1 ± 9 0 ± 1 80 ± 7 1,070 ± ± 7 PFOS 1 1,00 ±,70,100 ±,00 9,00 ±,90 1,700 ±,110 7,000 ±,900,00 ±,0 PFDcS 1 8 ± 9 6 ± 8 8 ± 11 9 ± ± 8 10 ± ΣPFS 1,700 ±,760,00 ±,060 9,900 ±,0,600 ±,110 8,00 ±,010,00 ±,80 Perfluorocarboxylates PFHxA 1 <1 <1 <1 <1 <1 <1 PFHpA 167 <167 <167 <167 <167 <167 <167 PFOA 91 1 ± 167 ± 1 < ± 7 16 ± 7 6 ± 119 PFNA 6 18 ± 18 8 ± 9 0 ± 7 90 ± 8 1,00 ± 9 1,110 ± 80 PFDcA 9 1 ± 8 ± ± ± 7 1,00 ± ± 10 PFUnA 0 1,00 ± 1,0 ± 0,80 ± 1 1,60 ± 08,160 ± 6,60 ± 6 PFDoA 6 8 ± 60 ± 60 ± ± ± ± 119 PFTriA 768 ± 1 1,10 ± 00,0 ± 6,810 ± 77,0 ± 7 1,970 ± 69 PFTeA 18 <18 1 < ± 09 ± ± 8 77 ± 66 PFPeA 88 <88 1 < ± 6 0 ± ± < Σ10PFCA,710 ±,90 ± 7 7,90 ± 9 8,10 ± 9 10,00 ± 1,0 8,0 ± 99 Calculation of mean concentrations that included samples below the MLOQs was done by assigning randomly-generated numbers from a normal distribution between zero and the compound-specific MLOQs. However, concentration means for each of the colonies and sampling years were generated only if 60% or more of the egg samples had quantifiable concentrations of the given compound. If this criterion was not respected, a range concentration (<MLOQ max) was reported. a
4 FIGURE S1. Map of Northern Europe showing the two sampling colonies, and, of herring gull eggs in Northern Norway. Map adapted from Arctic Research Mapping Application ( 00 km Faroe Is. Finland Russia Norway Sweden Denmark
5 FIGURE S. Extracted high resolution mass chromatograms of PFOSA and PFSs from HPLC-Q-ToF full scan HRMS (A) and MRM chromatograms of PFCAs from HPLC/MS-MS analysis (B) of a sample from (00). See Experimental Section for details. For the PFSs, branched isomers eluting before the main linear isomer are visible (A). A PFOSA Da 89.1 B PFPeA 76 -> e PFTeA 71 -> 669.0e PFDcS Da 6.8 PFTriA 66 -> e Relative Abundance PFOS Da 1.7e Relative Abundance PFDoA PFUnA 61 -> 69.6e 6 -> e PFDcA 1 -> 69.78e PFHxS Da 990 PFNA 6 -> e PFOA 1 -> Retention Time [min] Retention Time [min]
6 FIGURE S. Mean (+ 1 standard error) percentage composition of eight individual perfluorocarboxylates (PFCAs) with chain lengths between 8 and 1 carbons to the sum PFCA (Σ 8 PFCA) concentrations in herring gull eggs from in 198, 199 and 00. % of Σ8PFCA PFOA PFNA PFDcA PFUnA PFDoA PFTriA PFTeA PFPeA
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