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) 1.8 10-5 ( 20 C) 2.0* ( mg/l) 156 mg/l (20 C) (156ppm/20 C) http://www.chemicalbook.com http://www.ispjapan.co.jp/industrial_refguide/isp_ipbc.pdf http://www.sigmaaldrich.com/catalog/displaymsdscontent.do * 17 3 HPLC http://www.nichino.co.jp/ 610
http://www.nichino.co.jp/ (1) 1 IPBC LC/MS/MS (2) 3--2-(IPBC) 99.7% IPBC 10 g 97% IPBC 10 mg 10 ml 1.00 mg/ml 0.500 100 ng/ml DIONEX ASE-200 Waters (3) 21 3 5.00 g 200 ml 5 ml 5 ml 611
LC/MS/MS 1 LC/MS/MS Applied Biosystems API 3200 LC Shimadzu LC 10ADvp ODS-3 (150 mm 2.1 mm, 5 μm) A B 0 2 min A B = 85 15 2 15 min A 85 10 B 15 90 linear gradient 15 20 min A B = 10 90 0.2 ml/min 40 C 5 μl MS API 3200 5500 V 500 C 30 psi 60 psi 282 > 165 5 μl LC/MS/MS 5 μl LC/MS/MS IPBC IPBC (ng/g-dry) (ng/g-dry) = (ng/ml) (ml) / (g-dry) IDL LC/MS/MS (Applied biosystems API 3200) IDL12 612
IDL (ng/ml) 1 IDL (g-dry) (ml) IDL (ng/g-dry) IPBC 0.11 5.00 5 0.11 1 LC/MS/MS (Applied biosystems API 3200) 2 IDL 21 3 2 2 IDL IPBC (g-dry) 5.00 (ml) 5 (ng/ml) 0.500 (μl) 5 1 (ng/ml) 0.539 2 (ng/ml) 0.554 3 (ng/ml) 0.565 4 (ng/ml) 0.565 5 (ng/ml) 0.536 6 (ng/ml) 0.565 7 (ng/ml) 0.484 0.5442 0.0293 IDL (ng/ml) 0.11 IDL (μg/g-dry) 0.00011 S/N 10 CV (%) 5.4 IDL = t (n-1, 0.05) σ n-1 2 613
IPBC 1 IDL (0.500 ng/ml) 2 2 LC/MS/MS ESI-positive 5.00 g-dry Sep Pak-C18 5 ml 2 614
3 area(cps) 8.0E+04 y = 655.79x R 2 = 0.9979 6.0E+04 4.0E+04 2.0E+04 0.0E+00 0 20 40 60 80 100 120 ng/ml 3 4 4-1 IPBC 4-2 IPBC (m/z = 282) 615
ASE ASE ASE 7 g IPBC (1 μg/ml) 0.2 ml (200 ng) ASE 327 ml LC/MS/MS-ESI -positive 3 A (58 75%) 50% ph 5 ph 9 3 ASE -1 (%) ASE 58 20 31 A 74 29 36 75 - - B 32 27-37 36 - C 16 - - 3 ASE ASE (psi) ( C) A 1200 80 B 1000 60 C 1500 50 ASE ASE (0.1 g) IPBC ASE 4 5 5 g IPBC (10 μg/ml) 100 μl (1 μg) 1000 psi 1200 psi 3 616
4 ASE -2 (%)n = 2 (psi) 1000 1200 ( C) 50 80 50 80 1%- 62 65 68 40 2%- 74 38 68 33 5 ASE -3 (%)n = 2 ( C ) 50 60 80 100 28 22 8 4 4 1000 psi 4 5 60% 5 g IPBC (10 μg/ml) 100 μl (1 μg) ASE 3 1000 psi 50 o C 6 ASE -4 (%) No. No.1 No.2 No.3 17 20 23 6 2 A IPBC ASE 10 g 10 μg/ml 100 μl 1 μg ASE 3 1000psi50 o C 60 o C 80 o C 617
7 ASE -5 (%) (n = 2) 50 C 60 C 80 C 32 31 16 5 g IPBC50 ng (10 min) 3 8 8-1 (%) (n = 3) MDL 49 43 30 24 MDL 20 gipbc (100 500 ng) 10 ml (10 min) (5 min) 3 9-2 (%) (n = 2) (ng) 1 2 3 メタノール アセトニトリル 100 36 11 5.3 52 500 42 10 3.9 56 100 28 3.7 4.1 36 500 24 5.7 2.2 32 10 g IPBC 500 ng 2 (30 min) 10 618
10-3 (%) (n = 2) / / 10/90 50/50 90/10 75/25 50/50 25/75 -* - <10 - <10 <10 *-IPBC A-2 10 g IPBC 500 ng 2 hr 0.1 ml 30 min 1 ml IPBC50 ng 11 11-4 (%) (n = 2) (%) * (%) / (1:1) <10 61 / (1:1) <10 69 / (8:2) <10 71 * LC/MS/MS 5 IPBC 50 ng/ml No.7 (9) + 50 IPBC (50 ng/ml) 1000000 800000 600000 400000 200000 0 No.7+50 No.7+50 No.9+50 5-1 RT = 1 min 619
6 ODS-3 (2.1 150 mm) LC/MS/MS // No.1 12 No.1 12+50 1 ml IPBC (1 μg/ml) 50 μl (50 ng/ml) IPBC (50 ng/ml) C18 No.1 12 C18 C18+50 IPBC (1 μg/ml) 50 μl (50 ng/ml) ASE ASE 125000 ODS-3(RT=11.3) 100000 75000 50000 25000 0 2000000 No.1 No.2 No.1 +50 No.2 +50 No.3 ASE No.3 ASE No-1_C18 No-2_C18 No-3_C18 No-4_C18 AcCN/H2O No-1_C18 +50 No-2_C18 +50 No-3_C18 +50 No-4_C18 +50 No.5 No.6 No.7 No.8 No.9 No.10 No.11 No.12 No.7 +50 No.8 +50 No.9 +50 No.10 +50 No.11 +50 No.12 +50 1500000 1000000 500000 0 No.7 No.8 No.9 No.10 No.10 No.10 No.7 +50 No.8 +50 No.9 +50 No.10 +50 No.11 +50 No.12 +50 No-1_C18 No-2_C18 No-3_C18 No-4_C18 No-1_C18 +50 No-2_C18 +50 No-3_C18 +50 No-4_C18 +50 `45 No-1_C18 +50 No-1_C18 +50 6-2 / / IPBC LC/MS 537-0025 1-3-62 06-6972-5865 FAX 06-6972-7695 E-mail UeboriMi@mbox.pref.osaka.lg.jp 620