外因性内分泌攪乱化学物質調査暫定マニュアル(水質、底質、水生生物)

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1 (PCB) 1 ng/l (µg/kg, wet) (µg/kg) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) MS GC/MS-SIM 1M KOH GC/MS-SIM Wellington Laboratories BP-WD Wellington Laboratories BP-MS KC-300 KC-400 KC-500, KC mg/L 400mg/L I-1

2 Wellington Laboratories BP-WD PCB PCB Congener IUPAC No. 2- Chlorobiphenyl 1 4-Chlorobiphenyl 3 2,6-Dichlorobiphenyl 10 4,4'-Dichlorobiphenyl 15 2,2',6-Trichlorobiphenyl 19 3,4,4'- Trichlorobiphenyl 37 2,2',6,6'-Tetrachlorobiphenyl 54 3,3',4,4'- Tetrachlorobiphenyl 77 2,2',4,6,6'-Pentachlorobiphenyl 104 3,3',4,4',5- Pentachlorobiphenyl 126 2,2',4,4',6,6'-Hexachlorobiphenyl 155 3,3',4,4',5,5'- Hexachlorobiphenyl 169 2,2',3,4',5,6,6'-Heptachlorobiphenyl 188 2,2',3,4,4',5,5'- Heptachlorobiphenyl 189 2,2',3,3',4,4',5,5'-Octachlorobiphenyl 202 2,3,3',4,4',5,5',6-Octachlorobipheny 205 2,2',3,3',4,4',5,5',6-Nonachlorobiphenyl 206 2,2',3,3',4,5,5',6,6'- Nonachlorobiphenyl 208 2,2',3,3',4,4',5,5',6,6'-Decachlorobiphenyl 209 Wellington Laboratories BP-MS PCB PCB Congener IUPAC No. Monochlorobiphenyl 1, 3 Dichlorobiphenyl 4, 8, 10, 15 Trichlorobiphenyl 18, 19, 22, 28, 33, 37 Tetrachlorobiphenyl 44, 49, 52, 54, 70, 74,77, 81 Pentachlorobiphenyl 87, 95, 99, 101, 104, 105, 110, 114, 118, 119, 123, 126 Hexachlorobiphenyl 128, 138, 149, 151, 153, 155, 156, 157, 158, 167, 168, 169 Heptachlorobiphenyl 170, 171, 177, 178, 180, 183, 187, 188, 189, 191 Octachlorobiphenyl 194, 199, 201, 202, 205 Nonachlorobiphenyl 206, 208 Decachlorobiphenyl 209 Wellington Laboratories MBP-CG I-2

3 Wellington Laboratories MBP-CG 13 C PCB PCB Congener IUPAC No. 4-Chloro[13C12]biphenyl 3 4,4'- Dichloro[13C12]biphenyl 15 2,4',5- Trichloro[13C12]biphenyl 31 2,2',5,5'- Tetrachloro[13C12]biphenyl 52 2,3',4,4',5- Pentachloro[13C12]biphenyl 118 2,2',4,4',5,5'- Hexachloro[13C12]biphenyl 153 2,2',3,4,4',5,5'- Heptachloro[13C12]biphenyl 180 2,2',3,3',4,4',5,5'- Octachloro[13C12]biphenyl 194 2,2',3,3',4,4',5,5',6- Nonachloro[13C12]biphenyl 206 2,2',3,3',4,4',5,5',6,6'- Decachloro[13C12]biphenyl 209 d m ODS Sep-Pak Plus Silica Cartridge (690 mg) ( aters ) 10ml % 1M KOH 1M 5% C g 300ml 5ml I-3

4 30cm 10mm 5g 2cm 40ml GC/MS MS MS 1L 2L 10ml 30g 10ng 100ng 100ml 10 50ml 200ml 200ml 30 1ml 20g 200ml 10ng 100ng 1M KOH 50ml 80 50ml (GF/A) 20ml 30ml I-4

5 300ml 50ml 10 20ml 300ml 50ml 300ml 50ml 300ml 50ml 200ml 200ml 30 3ml 10ml 10ml 1ml 100ng 50ml 30 3ml 1ml 100ng 10mg I-5

6 100ml 100 g/ml 20 HT m 5% DB-5MS Ultra2 SGE cm/secHe 70 I-6

7 4-Chloro[13C12]biphenyl 4,4'- Dichloro[13C12]biphenyl 2,4',5- Trichloro[13C12]biphenyl 2,2',5,5'- Tetrachloro[13C12]biphenyl 2,3',4,4',5- Pentachloro[13C12]biphenyl 2,2',4,4',5,5'- Hexachloro[13C12]biphenyl 2,2',3,4,4',5,5'- Heptachloro[13C12]biphenyl 2,2',3,3',4,4',5,5'- Octachloro[13C12]biphenyl 2,2',3,3',4,4',5,5',6- Nonachloro[13C12]biphenyl 2,2',3,3',4,4',5,5',6,6'- Decachloro[13C12]biphenyl d % 70 (1.9min)--8 /min--300 (15min) I-7

8 4-Chloro[13C12]biphenyl 4,4'- Dichloro[13C12]biphenyl 2,4',5- Trichloro[13C12]biphenyl 2,2',5,5'- Tetrachloro[13C12]biphenyl 2,3',4,4',5- Pentachloro[13C12]biphenyl 2,2',4,4',5,5'- Hexachloro[13C12]biphenyl 2,2',3,4,4',5,5'- Heptachloro[13C12]biphenyl 2,2',3,3',4,4',5,5'- Octachloro[13C12]biphenyl 2,2',3,3',4,4',5,5',6- Nonachloro[13C12]biphenyl 2,2',3,3',4,4',5,5',6,6'- Decachloro[13C12]biphenyl d GC/MS GC/MS I-8

9 p,p'-ddt 1mg/L 1 L GC/MS DDT DDD DDE 20% DDT 20% cm SIM (RF) RF RF 15% RF 15% RF 15% RF RF=(As Cis)/(Ais Cs) As Ais Cis (ng) Cs (ng) KC-300 KC-600 (Cs ng) (ng) = (ng) mg/L KC-300 KC BZ#1 BZ#1 (ng) = 100ng = ng GC/MS SIM RF 8 RF RF 15% GC/MS RF I-9

10 PCB PCB window (5% phenyl methyl siloxane) PCB IUPAC #1, #3, #10, #15, #19, #37, #54, #77, #104, #126, #155, #169, #188, #189, #202, #205, #206, #208, #209 GC 5% phenyl methyl siloxane 4 4 2,2,6,6 - (IUPAC : #54) PCB 3,3,4,4 - (IUPAC : #77) GC PCB PCB 5 20% PCB SGE HT8 PCB PCB PCB (M-70) 5 20% PCB PCB PCB RF PCB Wellington Laboratories BP-MS BP-MS RF KC-300 KC-600 PCB PCB KC-300 KC-600 I-10

11 RF (ng) (ng)=(as Cis)/(Ais RF) As Ais Cis (ng) 10 50% 120% 80% 120% (CRM) (x) (s) (DL) DL = x s I-11

12 (s) (DL) DL = s MS PCB ODS 1M KOH 50ml 1M KOH 100ml I-12

13 HPLC µbondapak NH 2, 9mm i.d. 30cm, Waters (LC-NH 2 ) PCB 5% g MS HPLC PCB GC PCB KC300 KC600 M+70 PCB 5 10 JIS Z PCB CRM NIST SRM 1939 Wellington Laboratories CARP-1 20g WindowsPCB19 100ng -d 10 I-13

14 20g 100ng IUPAC PCB , ,2', ,4' ,2',6,6' ,2',4,6,6' ,4,4' ,2',4,4',6,6' ,3',4,4' ,2',3,4',5,6,6' ,3',4,4', ,2',3,3',5,5',6, ,3',4,4',5,5' ,3,3',4,4',5,5' ,2',3,3',4,5,5',6,6' ,3,3',4,4',5,5', ,2,',3,3',4,4',5,5, ,2',3,3',4,4',5,5,6,6' g 100ng IUPAC PCB , ,2', ,4' ,2',6,6' ,2',4,6,6' ,4,4' ,2',4,4',6,6' ,3',4,4' ,2',3,4',5,6,6' ,3',4,4', ,2',3,3',5,5',6, ,3',4,4',5,5' ,3,3',4,4',5,5' ,2',3,3',4,5,5',6,6' ,3,3',4,4',5,5', ,2,',3,3',4,4',5,5, ,2',3,3',4,4',5,5,6,6' I-14

15 1997 4,4' JIS Z WHO 1994 Analytical Chemistry of PCBs, M. D. Erickson, Butterworth Publishers, Polychlorinated biphenyls in the environment, V. Lang, J. Chromatogr., 595, 1-43, Mass Spectrometric Determination of Polychlorinated Biphenyls as Isomer Groups, J. E. Gebhart, T. L. Hayes, A. L. Alford-Stevens and W. L. Budde, Anal. Chem., 57, , Determination of Byproduct Polychlorobiphenyls in Commercial Products and Waters by High-Resolution Gas Chromatography/Electron Impact Mass Spectrometry, M. D. Erickson, J. S. Stanley, J. K. Turman, J. E. Going, D. P. Redford and D. T. Heggem, Environ. Sci. Technol, 22, 71-76, Comparison of methods for the gas-chromatographic determination of PCB congeners and chlorinated pesticides in marine reference materials, M. M. Schantz, R. M. Parris, J. Kurz, K. Ballschmiter and S. A. Wise, Fresenius J. Anal. Chem., 346, , I-15

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外因性内分泌攪乱化学物質調査暫定マニュアル(水質、底質、水生生物)

外因性内分泌攪乱化学物質調査暫定マニュアル(水質、底質、水生生物) (PCB) 1 ng/l (µg/kg, wet) (µg/kg) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001) 1 (0.001) 10 (0.01) 1 (0.001)

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