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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- ちかこ きちや
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1 p,p -DDT p,p -DDE p,p -DDD trans- cis- trans- cis- (PBB) (BaP) 25ng/L 5µg/kg GC/MS-SIM GC/MS-SIM GC/MS-SIM GC/MS-SIM (2-, 3-, 4- ) (4,4'- ) p,p'-ddt- 13 C 12 HCB- 13 C 6 BaP-d 12 -d10 -d 10 p- -d II-1
2 m ODS 96% II / % C g 300ml 5ml (Atlas Powder Co. )100g 2L 1L 30 1L % 25g 75g 30 Sep-Pak Plus Silica Cartridge (690 mg) (Waters ) 10ml 60 80
3 30ml (KD) 30cm 15mm 10g 2cm 100ml 30cm 10mm 5g 2cm 40ml 30cm 10mm 2.5% 10g 30% 2cm 30% GC/MS 1L 2L 30g 10ng 100ng 50ml 10 KD 5ml 1ml 20g 100ml 10ng 100ng 50ml rpm 10 5 II-3
4 500ml 1 50ml 5 KD 5ml BaP 40g 20ng 200ng 40ml 80ml 3000rpm ml 200ml KD 50ml 50ml 25ml 25ml 100ml 50ml 50ml 5ml 5 500ml 1L 50ml 300ml 100ml KD 5ml 25ml 50ml 10ml 50ml KD 5ml 2% II-4
5 ml KD 100ng 1000ng 1ml (Fr 1) 4 100ml(Fr 2) ml(Fr 3) 5ml Fr g 10g 10mm 300mm KD ml 100ng 1000ng 1ml (Fr 1) 4 100ml(Fr 2) ml(Fr 3) 5ml KD ml 100ng 1000ng 1ml 5ml KD ml 1ml 10mg 100mg/L p,p'-ddt- 13 C 12 HCB- 13 C 6 BaP-d 12 -d 10 -d 10 p- -d 14 II-5
6 20 GC/MS 30m 0.25mmi.d m 0.25mmi.d. 40cm cm % 50 (1 ) L m 0.25mmi.d m 15m 50 (1 ) L eV EI SIM 1 2 II-6
7 (PTRI, Programmed Temperature Retention Index) PTRI No CAS RN * p,p -DDT p,p -DDE p,p -DDD trans cis trans cis (HCB) * PTRI n- 5% II-7
8 No p,p'-ddt- 13 C HCB- 13 C d d d p- -d GC/MS GC/MS p,p'-ddt (DFTPP) 1mg/L 1 L GC/MS DDT DDD DDE 20% DDT 20% cm MS DFTPP 3 DFTPP SIM II-8
9 (RF) (RF) RF RF 15% RF 15% RF 15% RF RF=(As Cis)/(Ais Cs) As Ais Cis (ng) Cs (ng) 1 GC/MS SIM RF p,p'-ddt- 13 C 12 DDD DDE 20% 20% 8 RF RF 15% GC/MS RF 5 20% II-9
10 RF RF (ng) (ng)=(as Cis)/(Ais RF) As Ais Cis (ng) 10 80% 120% 80% 120% NIST EU BCR CRM (CRM) CRM II-10
11 (x) (s) (DL) DL = x s (s) (DL) DL = s (5ml) 2 g 5ml 20ml GC/MS p,p'-dde p,p'-ddt p,p'-dde 4% 100ml p,p'-ddt 15% 150ml BaP ODS II-11
12 15 30 GC/MS 30% Fr.3 Fr.3 5% 10ml 5% (5g) : 10ml Hexane 5% Acetone-Hexane 30% Acetone-Hexane Fr.1-1 Fr.1-2 Fr.1-3 Total Fr.2-1 Fr.2-2 Fr.2-3 Total Fr.3-1 Fr.3-2 Fr.3-3 Total BaP α-hch β-hch γ-hch δ-hch (Fr 1) II-12
13 15 150ml 209 RF %RSD 15% DDT HCB 13 C BaP 80% 120% 5 10 JIS Z CRM ( NIST SRM 1588) (EU BCR CRM 187, CRM 188) (EU BCR CRM 430) CRM 20g II-13
14 Compound µ µ Hexachlorobenzene * alpha-hch beta-hch gamma-hch delta-hch Heptachlor Aldrin Heptachlor epoxide Oxychlordene trans-chlordane cis-chlordane Endosulfan I trans-nonachlor ,4'-DDE Dieldrin Endrin ,4'-DDD * cis-nonachlor Endosulfan sulfate ,4'-DDT * Endrin ketone Methoxychlor Benzo(a)pyrene * Standard Methods 19th ed. American Public Health Association, EPA Method 8270B, US EPA, Official Methods of Analysis of The Association of Official Analytical Chemists 15th ed. Vol. 1, Association of Official Analytical Chemists, Inc., II-14
15 4,4' JIS Z J.R. Chapman, Wiley 1995 WHO II-15
16 -16
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)
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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8-18-29 3 291415 297 1-11-4 3/31/ 3/31/ 29 8 22 29 1 17 24 8-1 29 [1] PCB [2] HCB [3] [4] [5] DDT [6-1] p,p'-ddt [6-2] p,p'-dde pg/l ( ) nd 2,4 (46/47) 2.9 18 (47/47) 84 12 pg/g-dry ( ) nd 61, (61/62)
要調査項目等調査マニュアル
PBDEs TriBDE DeBDE 1 TriBDE 8 TeBDE 6 PeBDE 8 HxBDE 7 HpBDE 5 OcBDE 3 NoBDE 2 DeBDE 40 GC/MS 1 1 1 ng/l µg/kg, dry µg/kg TriBDE 0.1 0.01 0.01 TeBDE 0.1 0.01 0.01 PeBDE 0.1 0.01 0.01 HxBDE 0.1 0.01 0.01
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(a) (a) 1010 LC/MS JIS K 04501010 JIS K 04502010 JIS K 04503010 JIS K 04504010 (2) ( JIS K 04505010 JIS K 04506010 JIS K 0128 No 1 PCBPCB 2 αhchβhchγhchδhchp,p DDTp,p DDEp,p DDD I IItranscis transcis HCB
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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平成26年度 化学物質分析法開発報告書
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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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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)
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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)
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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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☆H23 13－農薬一斉分析（大垣）.doc
13 56 2011 Examination of Determination of Residual Pesticides in Agricultural Products Yuki OHGAKI, Katsuhiro HAYASHI, Hiroyuki KAWAI, and Kyoko SHIMURA GC/MS 92 LC/MS/MS 60 150 n- 5 GC/MS 92 79 70% LC/MS/MS
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