平成26年度化学物質分析法開発報告書

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1 2,2-2,2 -Iminodiethanol Diethanol amine CAS C 4 H 11 NO C 1) g/cm 3 1) < mmhg (20 C) 2) 95.40% (20 C) 3) log P ow ) pka ) LD mg/kg 5) LD mg/kg 5) LD mg/kg 5) LD mg/kg 5) LD mg/kg 5) LD mg/kg 5) LD mg/kg 5) 529

2 6) 1) Budavari,S., (Ed), The Merck Index Ver.12:2 2) International Chemical Safety Cards ICSC0618 3) Lide, D.R, (Ed), CRC Handbook of Chemistry and Physics 84th Edition 4) HP PubChem Compound 5) HP (kis-net) 6) HP (CHRIP) 1 (1) 100 ml ml 25% (5:95) LC/MS/MS-SRM(ESI+) (2) 2,2-99.0% 2,2 - -d 8 CDN ISOTOPES 98% Waters Oasis MCX 1 g/20 cc LCMS LCMS Milli-Q LCMS 1 mol/l HPLC 25% 530

3 25% (5:95) 25% 50 ml 1000 ml 2, mg 50 ml 2, mg/l 2,2 - -d mg 50 ml 2,2 - -d mg/l 1000 mg/l 10.0 μg/ml 2, mg/l / (1:999) ng/ml 100 ng/ml 2,2 - -d mg/l 100 ng/ml 1 (100 ml) ( μl) ( μl) PP 15 ml 10 ml LC PP (3)

4 100 ml 100 ml 900 ml 100 ml 2 2,2 - -d μg/ml 100 μl ph 5~7 3 4 Oasis MCX 10 ml/min 100 ml 20 ml 25% (5:95) 8 ml 45 C 0.5 ml 5 / (1:999) 10 ml LC/MS 6 LC/MS Waters 2695/ Quattro micro API LC LC Waters 2695 Waters XBridge Amide 2.1 mm 100 mm, 3.5 μm A:5 mmol/l / (2:8) B:/ / (1:899:100) 0 7 min A:100% B: 0% 7 12 min A: 0% B:100% min A:100% B: 0% 0.2 ml/min 40 C 10 μl / (1:1) / (1:999) MS MS Waters Quattro micro API 3.0 kv 532

5 120 C 300 C 50 L/Hr 800 L/Hr ESI-Positive SRM 2,2 m/z 106.0>88.0 m/z 106.0>70.0 2,2 - -d 8 m/z 114.1>96.0 2,2 20 V 20 V 2,2 - -d 8 20 V 2,2 12 ev 14 ev 2,2 - -d 8 12 ev 10 μl LC/MS 2,2-10 μl LC/MS 2,2 - C (μg/l) C = R Q / V R : Q : (μg) (μg/μl) (μl) V : (L) 533

6 Q = 1(μg) = (0.01 μg/μl) (100 μl) V = 0.01 (L) (= {(0.1 L) / [(0.1 L)+ (0.9 L)]} 0.1 L C = R 100 (μg/l) (IDL) LC/MS/MS IDL IDL IDL (ng/ml) (L) (ml) IDL (μg/l) 2,2' (MDL) (MQL) MDL MQL MDL MQL (L) (ml) MDL (μg/l) MQL (μg/l) 2,2'

7 1 2,2-2 (Oasis MCX) ml 2,2-2,2 - -d 8 2,2-2,2 - -d 8 70% 10 ml 10mL ml 3 ph 1 mol/l 1 mol/l ph7 4 25% (5:95) 20 ml 20 ml 5 LC/MS/MS 0.5 ml 6 LC/MS Waters Quattro micro API 535

8 7 IDL IDL 3 IDL 2,2'- (L) (ml) 10.0 (ng/ml) (μl) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) IDL (ng/ml)* IDL μg/l) S/N 9.4 CV(%) 8.6 * IDL=t(n-1,0.05) σ n

9 2,2-2,2-2,2 --d 8 1 IDL (2, ng/ml) 537

10 8 MDL MQL MDL 4-1 MDL MQL 2,2'- - (L) (μg) (μg/l) (ml) (ng/ml) (μl) (μg/l) *1 < (μg/l) *2 < (μg/l) * (μg/l) (μg/l) (μg/l) (μg/l) (μg/l) (μg/l) (%) (μg/l) (μg/l) MDL(μg/L) * MQL(μg/L) * S/N 14 CV(%) 3.6 *1 (n = 3) *2 MDL (n = 3) *3 MDL = t (n-1, 0.05) σ n-1 2 *4 MQL = σ n-1 10 *5 538

11 4-2 MDL MQL 2,2'- - ( ) (L) (μg) (μg/l) (ml) (ng/ml) (μl) (μg/l) *1 < (μg/l) *2 < (μg/l) 1.17 * (μg/l) (μg/l) (μg/l) (μg/l) (μg/l) (μg/l) (μg/l) (μg/l) MDL(μg/L) * MQL(μg/L) * S/N 26 CV(%) 3.2 *1 (n = 3) *2 MDL (n = 3) *3 MDL = t (n-1, 0.05) σ n-1 2 *4 MQL=σ n-1 10 *5 539

12 2,2-2,2-2,2 --d MDL μg/l 2,2-2,2-2,2 --d MDL 1.00 μg/l 540

13 2 ph L 1 mol/l HCl Oasis MCX 1 g L L or 1 mol/l NaOH 10 ml/min 分取 L ph5-7 (2,2 --d μg) 100 ml 20 ml 25% (5:95) 8 ml 0.5 ml (1:999) 10 ml 3 LC/MS/MS SRM ESI+ 541

14 / (1:999) ng/ml 2,2 - -d ng/ml 10 μl LC/MS (Cs) (As) (Ais) (As/Ais) (ng/ml) m/z 106.0>88.0 m/z 114.0> * 100 ng/ml 542

15 3.0 2,2'- イミノジエタノール ,2'- イミノジエタノール面積比 y = x R² = 面積比 y = x R² = 濃度比濃度比 (ng/ml) (50) (100) (ng/ml) (0.5) (1) 4 2, ng/ml ng/ml 2,2 - (10 ng/ml) 5 2,2-2,2-2,2 --d 8 5 2,2-10 ng/ml 543

16 2,2-2,2 - -d ,2-2,2 --d 8 6 2,2-2,2 - -d 8 2,2-2,2 --d 8 7 2,2 - : m/z 106 2,2 - -d 8 : m/z

17 6 8 6 (μg/l) 2,2'- 3 < ,2-2,2-2,2 --d ml 545

18 ,2'- (μg) (L) 7 (ml) *1 *1 (μg/l) (%) (%) (%) < < < *1 546

19 2,2-2,2-2,2 --d ml 2,2-2,2-2,2 --d ml μg 547

20 2,2-2,2-2,2 --d ml 2,2-2,2-2,2 --d ml μg 548

21 8 2,2'- 8 ph 1 7 (%) (ng/ml) (%) ,2' PP 1 2,2'- 9 (%) (ng/ml) MDL ,2 - MDL

22 1. (1) ph (Oasis MCX) 2,2'- ph ,2'- 0.1 μg (Oasis MCX) 2,2 - -d 8 10 ph3-9 85% ph3 ph9 ph5-8 85% 2,2 - ph5~7 (Oasis MCX) (%) 海水 10 ml 相当河川水 100 ml ph 10 ph 2,2'- (2) Oasis MCX 2,2-0.2 μg (Oasis MCX) 25% (5:95) 2 ml LC/MS/MS 11 2,2-0-6 ml 0-8 ml 550

23 (%) No. 2 ml 11 (Oasis MCX) 2,2 - (3) (Oasis MCX) (Oasis MCX) ml 2,2-0.1 μg 12 2,2-2,2 - -d 8 70% 10 ml (%) (ml) 12 (Oasis MCX) (4) (Oasis MCX) (Oasis MCX) 0.5 ml / (1:999) 10 ml 551

24 ml 10 ml 30 mg/l LC/MS/MS (%) (ml) 13 (Oasis MCX) LC/MS/MS 2,2 - IDL ng/ml μg/l ng/ml (r 2 >0.99) MDL MQL μg/l μg/l 100 ml 10 ml 0.12 μg % % 1 2,2 - MDL 0.1 μg/l 2,2-552

25 TEL FAX

26 2,2 -Iminodiethanol This method provides a procedure for the determination of 2,2 -iminodiethanol in water samples by liquid chromatography-tandem mass spectrometry (LC/MS/MS). After 100 μl of 2,2 -iminodiethanol-d 8 (surrogate, 10 ng/μl) is spiked into 100 ml of a water sample (in the case of sea water, 100 ml of that diluted 10-fold with purified water), the sample is passed through a preconditioned solid phase extraction cartridge (Oasis MCX). The extract is eluted with 8 ml of 25% anmonia aq. and methanol (5:95). The solution is analyzed by LC/MS/MS-SRM (ESI positive). Method detection limits (MDL) of 2,2 -iminodiethanol in river water and sea water were and 0.14 μg/l, respectively. The averages of recoveries (and those of relative standard deviations) from 0.12 μg of 2,2 -iminodiethanol added to river water and sea water were 97% (1.1%) and 104% (1.0%), respectively. 2,2 -Iminodiethanol was not detected in river water and sea water (Kobe) by the method. Water sample ph adjustment River Water 0.1 L 1 mol/l HCl Sea Water + Pure Water Aliquot or 1 mol/l NaOH 0.1 L 0.9 L 0.1 L ph5-7 Surrogate: (2,2'-iminodiethanol-d 8 1 μg) Solid Phase Extraction Oasis MCX 1 g 10 ml/min Wash milliqwater 100 ml methanol 20 ml Dehydration pressurized air Elution 25%anmonia aq. and methanol(5:95) 8 ml Concentration N 2 gas to 0.5 ml Volume adjustment Formic Acid:Acetonitrile (1:999) 10 ml LC/MS/MS SRM ESI+ 554

27 [1] 2,2'- イミノジエタノール ph L 1 mol/l HCl Oasis MCX 1 g L or 1 mol/l NaOH 10 ml/min L ph5-7 分取 L : LC/MS/MS-SRM ESI- : (μg/l) [1] 0.037( 河川水 ) (2,2 --d μg) [2] 0.37( 海水 ) 100 ml 20 ml 25% : (5:95) 8 ml LC: waters 2695 MS: waters Quattro micro API LC/MS/MS SRM XBridge Amide ESI+ 2.1 mm 100 mm, 3.5μm 0.5 ml (1:999) 10 ml 555

平成26年度化学物質分析法開発報告書

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