UHPLC Orbitrap Application Note LCMS14003 Orbitrap CEC CEC 61 CEC 312 CEC SPE UHPLCThermo Scientifi c Orbitrap Thermo Scientifi c TraceFinder WWTP S1 PS 5 ºC S2 TWAS 5 ºC 1 WWTP 1 2 WWTP 2 1 2 S1 1 S2 2 S3 2 S4 S6 1 S5 10 4 2 ºC UHPLC-Orbitrap HPLC Fisher Scientifi c Thermo Scientifi c Barnstead Nanopure Laboratory Services NBranch LaSB E3454 1 Waters OASIS HLB SPE 6 cc 500 mg AnMBR PS TWAS AD V=540 L 35 ºC V=540 L 35 ºC S5 1 WWTPS1 2 5
2 PS FeCl 2 FeCl 2 S1 S3 S4 S6 2 4 WWTP Sigma-Aldrich D 13 C CDN Isotopes Cambridge Isotope Laboratories 5 HRG-3400RS WPS-3000 TCC-3400 Thermo Scientifi c Dionex UltiMate 3000 UHPLC 5 µl Thermo Scientifi c Betasil Agilent XDB C-18 2.1x100 mm Orbitrap 1 HPLC UHPLC H-ESI Orbitrap Thermo Scientifi c Exactive Plus Exactive Plus MSCAL5 MSCAL6 ESI 99 % 35 L/min 2,500 V 3,200 V 140,000 m/z 200 FWHM 1.6x10 6 C-trap Injection Time 50 msec 1.5/sec TraceFinder 61 CEC 312 CEC TraceFinder M H M NH 4 M Na M-H mass extraction window 5 ppm XIC XIC50,000 25 50 pg/ml ppt M 5 ppmm+1 10 % Fit threshold 90 % 312 CEC 1 65 10 % Microsoft Excel 1 MDL 61 21 10 1L Waters HLB SPE ph 7 TraceFinder 3 UHPLC-Orbitrap MS UHPLC-Orbitrap 250 µl 100 µl H 2 0
1#1 WWTP #2 3WWTP : ng/l MDL S1 #1 S1 #2 S1 #3 S2 #1 S3 #2 S3 #3 S4 #3 S5 #1 S6 #2 S6 #3 100 <MDL <MDL 578.5 111.5 1952.5 4026.5 <MDL <MDL 105.0 <MDL 50 <MDL <MDL <MDL <MDL 143.5 579.5 288.5 <MDL <MDL <MDL 10 147.5 3419.5 3417.5 107.5 <MDL 165.0 <MDL 3419.5 110.0 72.5 20 <MDL <MDL <MDL 49.0 53.0 109.0 23.0 <MDL <MDL <MDL 20 147.5 75.5 525.0 34.5 4426.5 <MDL 35.0 <MDL 288.0 105.5 200 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 2 332.5 <MDL <MDL 107.0 24.0 235.5 115.0 <MDL 262.0 183.5 100 918.0 289.0 289.5 316.0 304.5 319.5 315.0 298.5 606.5 536.0 DEET 150 <MDL <MDL <MDL <MDL <MDL 338.5 <MDL <MDL <MDL <MDL 100 <MDL <MDL <MDL 166.5 <MDL 148.5 <MDL <MDL <MDL <MDL 5 1781.5 <MDL <MDL 7.5 8.0 11.0 9.5 <MDL 976.5 636.5 10 38.0 <MDL <MDL 114.0 <MDL 118.5 54.5 <MDL 32.5 35.5 20 <MDL <MDL <MDL 81.0 <MDL 125.5 49.0 <MDL <MDL <MDL 20 29.0 <MDL <MDL <MDL <MDL 957.5 <MDL <MDL 108.5 <MDL A 200 4458.0 617.5 1252.5 522.0 1211.0 1675.5 213.0 249.0 3621.5 3383.5 50 1619.0 449.5 <MDL <MDL 678.0 1531.0 1337.0 <MDL 1441.0 345.5 200 <MDL 472.5 <MDL 1006.0 216.5 <MDL <MDL <MDL <MDL <MDL 10 <MDL 121.5 193.0 281.0 174.0 125.0 77.5 127.0 260.0 227.0 50 158.5 346.0 <MDL 170.0 237.0 166.5 170.0 196.0 159.5 159.5 50 <MDL 734.0 429.0 366.5 1176.5 532.0 247.5 411.0 <MDL <MDL 120 3068.5 <MDL <MDL 2422.0 <MDL <MDL <MDL 343.5 777.5 912.0 3 MDL M M 1M/ M 1 XIC 4 3-4A 3,5--4-4B Splenda 4C 5 M 0.2454 ppmxic 4
4 5 2 WWTP 10 312 CEC 10 %48 A 2 100% 100% N,N- 100% N- 100% O- 100% 100% 100% 100% 100% 100% 100% n- 100% 100% 100% 100% -10,11-100% 10,11-- 100% OH- 100% 100% 3-90% 90% 90% Di-OH- 90% 90% 80% 80% 3-4-- 70% 70% 60% 60% 2-2--5-50% 4- -2-50% 50% 80% OH- 80% 2-2,4-- 80% 5- -2-2-- 80% 5- -2-4- -2-- 80% 5- -2-4-- 80% 70% 70% 70% 70% 60% 60% 60% 60% 60%
UHPLC-Orbitrap Orbitrap TraceFinder 3 5 2.1x100 mm UHPLC 140,000 Orbitrap Application Note LCMS14003 M M 1 M/ M 1 SANCO 2 UHPLC 1. The Determination of Emerging Organic Pollutants in Environmental Matrices by Liquid Chromatography- Tandem Mass Spectrometry LC-MS/MS, Ontario Ministry of the Environment method E3454. laboratoryservicesbranch@ontario.ca 2. Method validation and quality control procedures for pesticide residues analysis in food and feed, Document N SANCO/12495/2011. ASMS2013 2014 Thermo Fisher Scientifi c Inc. E1405 TEL 0120-753-670 FAX 0120-753 -671 221-0022 3-9 E-mail: Analyze.jp@thermofisher.com www.thermoscientific.jp