Microsoft Word - 14_LCMS_アクリルアミド
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1 2,4- (2,4-Dichlorophenoxy) acetic acid 2,4-D 2,4-PA OH O O C A S C 8 H 6 Cl 2 O 3 Cl Cl ( ) 221. ( ) 1) (g/cm 3 ) (25 C) 2) ( C) (.4 mm Hg) 2) ( C) 2) (mmhg) (2 C) 2) (mg/l) (25 C) log P ow 2) ) LD mg/kg() ACGIH- TWA: 1 mg/m 3 ACGIH- A4 HCl PRTR 1) SPARC Performs Automated Reasoning in Chemistry v4.5 < ) The Physical Properties Database (Phys Prop), Syracuse Research Corporation, USA 3) Kis-net 371
2 1 (1).5 mol/l / LC/MS/MS-SRM (ESI - negative) (2) 2,4- (2,4-D) (>98.) 2,4--d 5 (>99.) PCB 5 Waters OASIS-MAX 6 cc (15 mg) Cat.No ,4-D 1. mg 1 ml 1 μg/ml 1.4. ng/ml 1.2 ng/ml 2,4-D-d 5 5. ng/ml 2,4-D-d 5 1. mg 1 ml 1 μg/ml 1 ng/ml Zymark 1 372
3 Sep-Pak Concentrator 13 mm GD/X 1. μm 2.5 ml (3) g 1. g 2 1 ng/ml 5 μl2,4-d-d 5 5. ng)1 mol/l.5 ml 3 ml 1 3 rpm 1 3 ml 3 3 ml 5 ml 1 ml OASIS-MAX 3 1 ml/min 2 ml 5 mmol/l 5 ml 5 ml.5 mol/l / 5 ml 1 ml 4 LC/MS LC Waters ACQUITY UPLC Atlantis dc18 (15 cm 2.1 mm, 3 μm) (Waters) 373
4 A: 1 mmol/l B: 7 min A: 6 1 B: 4 99 linear gradient 7 1 min A: 1 B: min A: 1 6 B: 99 4linear gradient min A: 6 B: 4.2 ml/min 4 C 5 μl MS Waters XEVO TQ MS 1 kv 15 C 4 C 5 L/Hr 8 L/Hr ESI - negative 2 V 14 ev SRM (m/z) 2,4-D219 > 1612,4-D-d > μl LC/MS 5 μl LC/MS C = (ng/g-dry) C = RQ/V R: Q: (ng) = (ng/μl) (μl) V: (g-dry) 374
5 Q: 5. (ng) = (.1 ng/μl) (5. μl) V: 1. (g-dry) C = R.5 (ng/g-dry) (IDL) IDL 5 IDL (ng/ml) 1 IDL (g-dry) (ml) IDL (μg/kg-dry) 2,4-D (MDL) (MQL) MDL MQL 5 (g-dry) 2 MDL MQL (ml) MDL (ng/g-dry) MQL (μg/kg-dry) 2,4-D , 2 3OASIS-MAX 5 ml 1 ml 4 5IDL
6 3 IDL 2,4-D (g-dry) 1. (ml) 1 (ng/ml) 1. (μl) 5. 1 (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml) (ng/ml).87 7 (ng/ml).957 (ng/ml) IDL (ng/ml) *1.17 IDL (ng/g-dry).17 S/N *2 1 CV () 4.9 *1: IDL = t (n-1,.5) σ n-1 2 t (n-1,.5) = *2: 24D native 1ng d 5ng 24D_11614_33 1 2,4-D-d 5 224> > 164 (d-24d) 8.9e D_11614_ > 161 (24D) 1.75e3 2,4-D 219> Time IDL 1. ng/ml 376
7 6MDLMQL MDL MQL 2,4-D - (g-dry) 1. - (ng) 2. - (ng/g-dry).2 - (ml) 1 - (ng/ml) 2. - (μl) 5. - (ng/g) *1 ND 14.3 (ng/g) *2 ND ng/gdry (ng/g-dry) (ng/g-dry) (ng/g-dry) (ng/g-dry) (ng/g-dry) (ng/g-dry) (ng/g-dry) (ng/g-dry).161 MDL (ng/g-dry) *3.63 MQL (ng/g-dry) *4.16 S/N *5 14 CV () 7.2 *1 (n = 2) *2 MDL (n = 2 ) *3 MDL= t (n-1,.5)σ n-1 2 t (n-1,.5) = *4 MQL= σ n-1 1 *5 377
8 24D MDL2 native 2ng d 5ng D_11614_58 1 2,4-D-d 5 224> > 164 (d-24d) 7.66e D_11614_ > 161 (24D) 3.31e3 2,4-D 219> Time MDL 378
9 g 1. g (2,4-D-d 5 5. ng) 1 mol/l.5 ml 3 ml 1 min 1 min 3 rpm 1 min 3 3 ml 65 ml OASIS-MAX 5 mmol/l 1 ml 1 ml/min 2 ml 5 ml 5 ml 5 ml LC/MS/MS SRM.5 mol/l / 5 ml 1 ml ESI-negative (ng/ml) (1) (2) (3) (4) (ng/ml) (5) (1) (15) (2) ng/ml 1.2 ng/ml 379
10 5-1 : ng/ml (A s ) (A is ) (A s /A is ) (C s ) 2,4-D 2,4-D-d *: : 5 ng/ml (C is ) 5-2 (A s ) : ng/ml 2,4-D (A is ) (A s /A is ) (C s ) 2,4-D-d *: : 5 ng/ml (C is ) 38
11 _24D_MS_SCAN 1 (.17) 1 a) XEVO-TQMS#VBA588 7-Jun :5:1 MS2 ES e m/z _24D_MSMS_SCAN 1 (.17) 1 b) XEVO-TQMS#VBA Jun :8:36 Daughters of 219ES- 3.33e m/z ,4-D a) b) 21166_D-24D_MS_SCAN 1 (.17) 1 c) XEVO-TQMS#VBA588 7-Jun :18:28 MS2 ES e m/z _D-24D_MSMS_SCAN 2 (.34) 1 d) XEVO-TQMS#VBA Jun :2:39 Daughters of 224ES- 4.51e m/z ,4-D-d 5, c) d) 381
12 2,4-D 6 8 (g-dry) 1 6 (ng) (ng/g-dry) () () () 無 添 加 2 ND g 1 g 5 ng1 mol/l.5 ml 1 4 ml2 2 ml3 2 ml 2 5 ml 1 1 ml 23 5 ml 1 ml 2,4-D-d 5 5 ng 7 7 (n=1) () () /= 1 :
13 OASIS-MAX ml1 ml5 ml5 ml 1 ml ml 2 ng 1 mol/l.5 ml 1 mol/l.5 ml OASIS-MAX 5 mmol/l.5 mol/l / 5 ml 1 ml 2,4-D-d 5 5 ng OASIS-MAX (n=2) (ml) 1 (ml) (ng) ()
14 2,4-D MDL <.63 ng/g-dry 5 ng D Rive sed d 5ng D_11614_53 1 2,4-D-d 5 224> > 164 (d-24d) 7.23e D_11614_ > 161 (24D) 459 2,4-D 219> Time D MDL2 native 2ng d 5ng D_11614_58 1 2,4-D-d 5 224> ng 224 > 164 (d-24d) 7.66e D_11614_ > 161 (24D) 3.31e3 2,4-D 219> Time ng 384
15 24D Sea sed d 5ng D_11614_54 1 2,4-D-d 5 224> > 164 (d-24d) 6.86e D_11614_ > 161 (24D) 48 2,4-D 219> Time D Rec river sed native 5ng d 5ng D_11614_ ,4-D-d 5 224>164 5 ng 224 > 164 (d-24d) 7.56e D_11614_ > 161 (24D) 8.54e3 2,4-D 219>161 Time ng 385
16 MDL 4 C ()( n = 7) 2,4-2,4-D 14 ng/ml R 2 >.999 (1 2 ng/ml) R 2 >.999 MDL.63 ng/g-drymql.16 ng/g-dry 1 g-dry 2,4-D 5 ng ( ng/g-dry 2,4-D 18 p ,4-d TEL FAX Azusa_Oita@pref.hyogo.lg.jp, Shuusuke_Takemine@pref.hyogo.lg.jp Masahiro_Tsurukawa@pref.hyogo.lg.jp, Chisato_Matsumura@pref.hyogo.lg.jp 386
17 (2,4-Dichlorophenoxy) acetic acid 2,4-D, 2,4-PA This method is suitable for the determination of (2,4-Dichlorophenoxy) acetic acid in sediment by liquid chromatography-tandem mass spectrometry (LC/MS/MS). Twenty grams-wet of the sediment sample is placed into a centrifugal sedimentation tube, and 5. ng of 2,4-D-d 5 as a surrogate,.5 ml of 1 mol/l formic acid and 3 ml methanol are added. Thereafter, the sample is extracted by sonication and shaking (1 minute each), centrifuged at 3 rpm. The extract is subsequently separated off, another 3 ml methanol is added to the residue, and the preceding process is repeated another two times. The combined extract is concentrated to 3 ml. A concentrated solution is placed into a beaker, and diluted with 65 ml of distilled water. The mixed solution is loaded on a OASIS-MAX cartridge. The cartridge is washed with 5 ml of 5 mmol/l ammonium acetate in distilled water and 5 ml of methanol that rinsed the beaker. Thereafter, the cartridge is eluted with 5 ml of.5 mol/l formic acid in methanol, and the elution is concentrated to 1 ml. The solution is analyzed by the LC/MS/MS-SRM (ESI negative). The method detection limits (MDL) and the method quantification limit (MQL) is.63 and.16 ng/g-dry, respectively. The average of recoveries (n=5) from 2. g-wet of sediment sample spiked with 5 ng (2,4-Dichlorophenoxy) acetic acid was 18, and the relative standard deviation was times Sediment sample 2. g-wet (Corresponding to 1. g-dry) surrogate (2,4-D-d 5 5. ng) 1 mol/l formic acid.5 ml Ultrasonic extraction Methanol 3 ml 1 min Shaking extraction 1 min Centrifugation 3 rpm, 1 min Concentration N 2 gas, to 3 ml Dilution Purified water 65 ml Rinse: Methanol 5 ml Solid phase extraction OASIS MAX 1 ml/min Rinse beaker:methanol 5 ml Dry Air 2 ml Wash 5 mmol/l Ammonium acetate 5 ml Beaker-rinsed-methanol 5 ml Elution.5 mol/l Formic acid methanol 5 ml Concentration N 2 gas Make up volume Methanol to 1 ml LC/MS/MS-SRM ESI-Negative 387
18 2,4-2,4-D 2,4-PA 2. g 1. g (2,4-D-d 5 5. ng) 1mol/L.5 ml 3 ml 1 1 LC/MS/MS-SRM -ESI-.63 ng/g-dry 3 rpm, 1 3 OASIS MAX 1 ml/min 2 ml 3 ml 65 ml 5 ml 5 mmol/l 5 ml 5 ml 分 析 条 件 : 機 器 LC:Waters ACQUITY UPLC MS:Waters XEVO TQ MS カラム Atlantis dc18 15 cm 2.1 mm, 3 μm (Waters).5 mol/l / 5 ml 1 ml LC/MS/ MS-SRM ESI-Negative 388
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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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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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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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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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2,4-2,4-Dimethylaniline 2,4-2,4-Xylidine CH 3 CH 3 CAS 95-68-1 C 8 H 11 N 121.18 121.0892-14.3 C 2) 214 C 2) 0.9723 g/cm 3 2) 0.133 mmhg (25 C) 1) 1390 mg/l (25 C) 1) 3.710 3 mg/l 25 C WSKOWWIN 5) 6.0710
Microsoft Word - 14_LCMS_アクリルアミド
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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