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Supplemental Information for a Suspect Screening Analysis for Contaminants Of Electronic Supplementary Material (ESI) for Analytical Methods. This journal is © The Royal Society of Chemistry 2020 Supplemental Information for A Suspect Screening Analysis for Contaminants of Emerging Concern in Municipal Wastewater and Surface Water Using Liquid-Liquid Extraction and Stir Bar Sorptive Extraction. Additional Materials and Methods Information: All the analytical standards, including surrogates, calibration mix, internal standards and hexachlorobenzene (cat # 32231) were purchased from Restek Corp. (Bellefonte, PA, USA). The surrogate standards include the Acid Surrogate Standard Mix (cat # 31003), Base Neutral Surrogate Standard Mix (cat # 31082) and QuEChERS Internal Standard Mix for GC-MS Analysis (cat # 33267). These were chosen because they represent environmentally relevant compound classes and provide a range of acidic and basic compounds. SV Internal Standard Mix (cat # 31206), a solution of 6 deuterated polycyclic aromatic hydrocarbons, was used because of its compliance with the US EPA Method 8270D for analysis of semi-volatile organic pollutants by GC-MS. 8270 Megamix (cat# 31850) was utilized as an additional calibration and target mix of 76 common environmental pollutants. Any sample analytes found in 8270 Megamix could then be quantified and it could also serve for single point semi-quantification purposes. Analytical grade dichloromethane, methanol and acetonitrile were purchased from Avantor (Center Valley, PA, USA), ChemPure Brand Chemicals (Ann Arbor, MI, USA) and Avantor respectively. The sodium sulfate and sodium chloride were supplied by Avantor and VWR (West Chester, PA, USA). The ultrapure water was delivered by the lab system Millipore Milli-Q Academic Ultrapure Water System (Billerica, MA, USA). Effects of Salt on PAH Recovery (Relative Response) 1.60 1.40 1.20 1.00 0.80 0.60 Response 0.40 0.20 Relative 0.00 (3.26) (3.72) (3.90) (3.90) (5.50) (6.18) (6.18) (6.18) (6.65) Acenaphthene Acenaphthylene p-Terphenyl-d14 Benzo(a)pyrene Dibenz(a,h)anthracene ... Indeno(1,2,3-cd)pyrene...Benzo(ghi)perylene 1-Methyl-Naphthalene2-Methyl-Naphthalene Benzo(b)fluorantheneBenzo(k)fluoranthene No salt 30% Salt 20% Salt Figure S1: Graph showing the relative response of PAHs as a function of the NaCl concentration during extraction. The logKow values are in parenthesis next to the analyte name. 70000 60000 2-Fluorophenol 50000 40000 30000 20000 10000 1st Time (s) 464 464 464 464 464 464 464 2nd Time (s) 1.4 1.45 1.5 1.55 1.6 1.65 1.7 112 WW mix_cis-100rep1n_2d_8-20-28:1 112 WW mix_cis-80rep1_2d_8-20-28:1 112 WW mix_cis-50rep1_2d_8-20-28:1 112 WW mix_cis-20rep1_2d_8-20-28:1 140000 1,3-Dichlorobenzene 120000 100000 80000 60000 40000 20000 1st Time (s) 626 626 626 626 626 626 626 626 626 626 2nd Time (s) 1.4 1.45 1.5 1.55 1.6 1.65 1.7 1.75 1.8 1.85 146 WW mix_cis-100rep1n_2d_8-20-28:1 146 WW mix_cis-80rep1_2d_8-20-28:1 146 WW mix_cis-50rep1_2d_8-20-28:1 146 WW mix_cis-20rep1_2d_8-20-28:1 500000 2-Fluorobiphenyl 400000 300000 200000 100000 1st Time (s) 1022 1022 1022 1022 1022 1022 1022 2nd Time (s) 1.3 1.4 1.5 1.6 1.7 1.8 1.9 172 WW mix_cis-100rep1n_2d_8-20-28:1 172 WW mix_cis-80rep1_2d_8-20-28:1 Figure S2: Extracted172 WW mix Ion_cis- 5Chromatograms0rep1_2d_8-20-28:1 showing17 the2 W WCIS mix _trappingcis-20rep1_ 2temperatured_8-20-28:1 effects on peak area. Orange represents -100 °C, green is -80 °C, blue is -50 °C, and pink is -20 °C. Table S.1. Percent Recoveries of sample method blanks LLE Spring SBSE Spring LLE WW Creek SBSE WW Creek Method Method Method Method Blank Blank Blank Blank Compound %R %R %R %R 2-Fluorophenol 53 29 ND ND Acid Surrogate Phenol-d6 20 ND ND ND Standard Mix (3/90 SOW) 2-Chlorophenol-d-4 66 56 ND ND 2,4,6-Tribromophenol 28 88 ND ND Base Neutral 1,2- Dichlorobenzene-d4 62 145 82 109 Surrogate 2-Fluorobiphenyl 53 66 81 95 Standard Mix Nitrobenzene-d5 63 94 47 ND (3/90 SOW) p-Terphenyl-d14 80 113 73 100 PCB 18 = 1,1’-Biphenyl, 2,2’,5-trichloro- 80 99 100 127 PCB 28 =1,1’-Biphenyl, QuEChERS 2,4,4’-trichloro- 80 109 85 114 Internal Standard Mix PCB 52 =1,1’-Biphenyl, for GC-MS 2,2’,5,5’-tetrachloro- 87 93 97 121 Analysis Triphenylmethane 93 95 88 123 Triphenylphosphate 88 68 NLR NLR Tris-(1,3-dichloro isopropyl)phosphate 92 70 NLR NLR LLE samples (n=2), SBSE (n=1). ND, non-detected. NLR, non-linear response. US EPA Comptox Chemistry Dashboard lists searched: EPA|ENDOCRINE: Endocrine Disruptor Screening Program (EDSP) Universe of Chemicals WATER|NORMAN: French Monitoring List DRUGS|NORMAN: Pharmaceutical List with EU, Swiss, US Consumption Data WATER|NORMAN: Wastewater Suspect List based on Swedish Product Data PESTICIDES|EPA: Pesticide Chemical Search Database Table S.2. Discovery compounds from the wastewater and spring creek samples. Compound Similarity Reverse Type 2-Butanol 816 957 PCP-flavorant, fragrance Dimenhydrinate 939 939 Drug-antiemetic Lidocaine 904 904 Drug-anesthetic Diphenyl sulfone 936 936 Manufacturing-colorant Doxepin 952 952 Drug-antidepressant 2-(methylthio)-benzothiazole 955 958 Consumer product Crotamiton 933 933 Drug-antiparasitic Amitriptyline 971 971 Drug-antidepressant Venlafaxine 943 947 Drug-antidepressant 3,4-Dichloro-benzenamine 953 955 Herbicide precursor Tramadol 866 866 Drug-analgesic Citalopram 915 915 Drug-antidepressant Bupropion 899 904 Drug-antidepressant Methadone 917 917 Drug-opioid Maltol 952 955 PCP-flavorant Musk ketone 932 941 PCP- fragrance Propofol 927 929 Drug-anesthetic Triclosan 878 896 PCP-Antibacterial Oxybenzone 896 896 PCP-sunscreen Levomenthol 957 957 Drug-anesthetic Thymol 742 771 PCP-Antibacterial Benzophenone 952 952 PCP-sunscreen Eucalyptol 933 933 PCP-fragrance Butylated Hydroxytoluene 889 890 PCP- body wash, makeup Benzothiazole 926 945 PCP-fragrance Cedrol 861 862 PCP- emollient Caffeine 952 952 PCP-eye cream, stimulant Homosalate 917 922 PCP-sunscreen Benadryl 911 928 Drug-antihistamine Carbamazepine 805 860 Drug-anticonvulsant Ibuprofen 791 856 Drug-analgesic Atrazine 845 846 Pesticide PCP, personal care product. Consumer product is the label on the EPA Comptox Database when the descriptor is not clear about the use. Similarity-number from the NIST search algorithm that defines how well the peak matches the library match using all masses, between 0-999. Reverse- number from NIST search algorithm defines how well the peak matches the library using masses in the database, between 0-999. 1 1 Leco Corporation, ChromaTOF® Software Instruction Manual, 2012..
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