LCMS14003:UHPLC-Orbitrap質量分析計による環境汚染物質のターゲット分析、ノンターゲット分析
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1 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 S1 1 S2 2 S3 2 S4 S6 1 S ºC UHPLC-Orbitrap HPLC Fisher Scientifi c Thermo Scientifi c Barnstead Nanopure Laboratory Services NBranch LaSB E 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 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 x100 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, pg/ml ppt M 5 ppmm+1 10 % Fit threshold 90 % 312 CEC % Microsoft Excel 1 MDL L Waters HLB SPE ph 7 TraceFinder 3 UHPLC-Orbitrap MS UHPLC-Orbitrap 250 µl 100 µl H 2 0
3 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 <MDL <MDL <MDL 50 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 35.0 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL DEET 150 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 100 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 81.0 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL A <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL 10 <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL <MDL MDL M M 1M/ M 1 XIC 4 3-4A 3,5--4-4B Splenda 4C 5 M ppmxic 4
4 4 5 2 WWTP 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, % OH- 100% 100% 3-90% 90% 90% Di-OH- 90% 90% 80% 80% % 70% 60% 60% % % 50% 80% OH- 80% 2-2,4-- 80% % % % 70% 70% 70% 70% 60% 60% 60% 60% 60%
5 UHPLC-Orbitrap Orbitrap TraceFinder x100 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. ASMS Thermo Fisher Scientifi c Inc. E1405 TEL FAX Analyze.jp@thermofisher.com
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2,2-2,2 -Iminodiethanol Diethanol amine CAS 111-42-2 C 4 H 11 NO 2 105.1356-105.0790-28 C 1) 1.0881 g/cm 3 1)
平成26年度 化学物質分析法開発報告書
2,2-2,2 -Iminodiethanol Diethanol amine CAS 111-42-2 C 4 H 11 NO 2 105.1356-105.0790-28 C 1) 1.0881 g/cm 3 1)
ソリッドコアUHPLCカラムとUHPLCシステム、質量分析計を利用した違法薬物の高速スクリーニング分析
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Isobutyl alcohol IUPAC 2-methylpropan-1-ol 2--1-2-Methyl-1-Propanol, Isobutanol CH 3 H 3 C OH CAS 78-83-1 C 4 H 10 O log P ow ( C) ( C) (kpa) (g/l) 74.12 74.14 1) -108 2) 108 2) 1.2 2) 87 2) 0.8 2) (74.1214)
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3--2-3-Iodo-2-propynyl butylcarbamate (IPBC) Carbamic acid, butyl-, 3-iodo-2-propynyl ester Iodocarb CAS 55406-53-6 C 8 H 12 NO 2 I C (g/cm 3 ) (mmhg) log P ow 281.09 (280.9910) 64 68 1.51 1.57 (20 C)
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N,N- N,N-Dimethylacetamide Acethyldimethylamine CAS 127-19-5 C 4 H 9 NO 87.12 ~ 87.14 87.68413 163-165 C 1) - 18.59 C 2) 1 mg/l 25 C 3) 3.3 hpa 2 C 4) log P ow -.77 2).9429 2/4 C 1) 3.1 4) 1.31E - 8 atm-m
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N N 1,, N 2 N N N N N 1,, N 2 N N N N N 1,, N 2 N N N 8 1 6 3 5 7 4 9 2 1 12 13 8 15 6 3 10 4 9 16 5 14 7 2 11 7 11 23 5 19 3 20 9 12 21 14 22 1 18 10 16 8 15 24 2 25 4 17 6 13 8 1 6 3 5 7 4 9 2 1 12 13
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26 3 31 BDF BDF BDF FAME BDF BDF BDF BDF BDF BDF BDF BDF BDF FAME BDF BDF 80.0 97.0% BDF 120 330 0.8% 2.2% 1. 1 1-1 1 1-2 1 2. 2 2-1 2 2-2 5 2-3 6 3. BDF 7 3-1 7 3-2 7 3-3 14 3-4 JOY 21 3-5 32 3-6 39 3-7
Agilent BioHPLC HPLC/UHPLC /
Agilent BioHPLC HPLC/UHPLC / HPLC/UHPLC ( Å Å ) BioHPLC MPa.. µm UHPLC Poroshell ( ) Agilent AdvanceBio RP-mAb : AdvanceBio RP-mAb Poroshell mab Agilent AdvanceBio :.7 µm C AdvanceBio Agilent Poroshell
14 4 12 10 8 6 3 2 4 2 1 0 0 100200300400500600 100200300400500600700 0 0 100200300400500600 100200300400500600700 (ppm) (ppm) 7 4 6 5 4 3 3 2 2 1 1 0 0 100200300400500600 100200300400500600700 0 0 100200300400500600
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b 0 1PPm 10PPm 100PPm 1000PPm 10000PPm 0.0001% 0.001% 0.01% 0.1% 1% 10% 1PPm 10PPm 100PPm 1000PPm 10000PPm 0.0001% 0.001% 0.01% 0.1% 1% 10% 1PPm 10PPm 100PPm 1000PPm 10000PPm 0.0001% 0.001% 0.01%
2 7 ( ) µ LC/MS/MS によるフェノール類分析 日本ウォーターズ株式会社 2015 Waters Corporation 1 対象化合物 Cl HO HO HO フェノール 2- クロロフェノール (2-CPh) Cl 4-クロロフェノール (4-CPh) HO Cl HO Cl HO Cl Cl 2,4
LC/MS/MS による類分析 日本ウォーターズ株式会社 15 Waters Corporation 1 対象化合物 - クロロ (-CPh) 4-クロロ (4-CPh),4- ジクロロ (,4-DPh),6- ジクロロ (,6-DPh),4,6- トリクロロ (,4,6-TPh) 15 Waters Corporation 1 サンプル調製 ( 検量線 標準液 ) 5 標準溶液添加 (,,4,,,5uL)
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HILIC ILIC BEH BEH 009 9 0 5 009 ihon Waters K.K. HILIC HILIC HILIC MS Sub-µm 009 ihon Waters K.K. HILIC? HILIC - Hydrophilic Interaction Chromatography 990 * HILIC (> 80%) *Alpert A. J. J.Chromatogr.
ラボ用汎用機器キャンペーン2019.Spring_cc17.indd
2019.4.1 Mon. 2019.9.20 Fri. Savant SpeedVac 25% OFF NEW DNA RNA Thermo Scientific TM Savant TM SpeedVac TM DNA130 HPLC / LC-MS Thermo Scientific TM Savant TM SpeedVac TM SPD1030 DNA130 / SPD1030 No. W
31, 21% 24, 17% 8, 5% 23, 16% 24, 16% 91, 62% 19, 13% 39, 27% 33, 23% 73 48 57 51 31 1 9 13.0% 7.4% 5.3% 12.5% 17.1% 13.2% 17.9% 4.5% 36.4% 56.5% 40.7% 36.8% 50.0% 67.1% 56.3% 65.8% 75.0% 26.0% 37.0%
37 27.0% 26 19.0% 74 54.0% 9 6.4% 13 9.2% 28 19.9% 26 18.4% 37 26.2%. 24 17.0% 99 69 75 59 39 1 6 4.5% 1.4% 7.7% 2.9% 25.0% 17.9% 20.8% 50.0% 41.7% 47.0% 51.4% 54.3% 61.5% 57.1% 55.6% 42.4% 50.0% 58.3%
3 DI 29 7 1 5 6 575 11 751, 13 1,1,25 6 1,251,5 2 1,51,75 1,752, 1 2,2,25 2,252,5 2,53, 3,3,5 3,5 5 1 15 2 25 3 5 6 575 12 751, 21 1,1,25 27 1,251,5 9 1,51,75 1,752, 1 2,2,25 2 2,252,5 2,53, 2 3,3,5
% 32.3 DI DI
2011 7 9 28.1 41.4 30.5 35.8 31.9% 32.3 DI 18.2 2.4 8.1 3.5 DI 9.4 32.2 0.0 25.9 2008 1 3 2 3 34.8 65.2 46.753.8 1 2 8.82.9 43.1 10 3 DI 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 21 22 23 24 25
2 DI 28 7 1 37 28 4 18 27 11 21 5 2 26 4 5 1 15 2 25 3 35 4 17 7 5 48 76 31 47 17 2 92 12 2 2 4 6 8 1 12 1 2 4 1 12 13 18 19 3 42 57 57 1 2 3 4 5 6 1 1 1 3 4 4 5 5 5.5 1 1.5 2 2.5 3 3.5 4 4.5 5
3, ,104 t mg/l 30 mg/l BOD mg 14 C 8, /kg 11 8, 1 11 OH = cm 3 / sec 11 OH /cm ppm
3, 3-1 200019 4800 CAS 91941 1138 3, 3-4, 4 - -3, 3 - H 2 N Cl Cl NH 2 C 12 H 10 C l2 N 2 253.13 1 95 1. 2 3, 4 132-133 402 5 >200 5 700kg/m 3 5 8.73 = 1 5.610-8 kpa 4.210-7 mmhg20 4 6 log Pow3.51 3.57
UPC 2 Baiba Cabovska, Michael D. Jones, and Andrew Aubin Waters Corporation, Milford, MA, USA UPC 2 ACQUITY UPC 2TM ACQUITY SQD Empower 3 UPC GC
UPC 2 Baiba Cabovska, Michael D. Jones, and Andrew Aubin Waters Corporation, Milford, MA, USA UPC 2 ACQUITY UPC 2TM ACQUITY SQD Empower 3 UPC 2 1-3 GC LC GC UltraPerformance Convergence Chromatography
Kanken5-0310fin.indd
4 Y o s h i o Tatsuzawa 20072004 1 2 1 2 3 4 5 6 7 8 9 10 2007 566,790 494,169 327,041 200,749 183,073 74,561 2007 2004100 270,440 93.9 263,316 106.7 174,523 90.8 160,246 104.5 129,796 98.6 128,357 99.2
