6.3 6.3.1 6.3.1 6.3.1.1 (1) (2) a) JIS K 0557 A3 b) JIS K 8891 c) (5g/L) d) (10g/L)JIS K 8576 1g 100mL e) (7+993)JIS K 8951 f) JIS K 8322 g) 0.1g 100mL 30mL 1L 500mL6.8mL 50g 1L h) 1L 500mL6.8mL 50g 1L i) (0.001g NaO3SO(CH2)11CH3 /ml) 100% 1.00g 1,000mL j) (10g NaO3SO(CH2)11CH3 /ml) (0.001g NaO3SO(CH2)11CH3/mL) 10mL 1,000mL (3) (1) a) b) c) d) e) f) g) h) 15cm 5cm i) (1) (1+9) 100mL 10mL 25mL 30 243
(4) (4).1 6.3.1 a) 20g 100mL b) 30mL 300mL c) 10mL 300mL d) 300mL 30 200mL e) 60mL f) 200mL g) 30mL 30 h) 100mL i) a)h) (4).2 a) 20g (2) 100mL 40mL 10 b) 3,000rpm 5 200mL c) 40mL 1 d) 30mL 1 (3) 200mL e) 70mL GF/F (4) f) 50vol% 5mL 2 g) 100mL h) a)g) (2) (3) (4)70mL (5) a) 650nm b) 244
6.3.1 10g/mL114mL 100mL (5)c) c) A 100mL (5g/L)3 (10g/L) (7+993) 10mL 25mL 1 23 (5) 10mL 2 50mL 30 50mL 5mL 2 50mL 650nm (4).1 i) (4).2 h) d) (g) 4.1 (%) (mg/kg) 100 ( mg / kg) = ( g) v 1 W(g) W (g) v (ml) (5) 245
6.3.1 (6) a) 20g 100mL 30 300mL 30mL 30 3,000rpm5 30mL 100mL b) 20 100mL 40mL 200mL 30mL 70mL GF/F 100mL 246
6.3.1 c) A 100mL (5g/L) (10g/L) (7+993) 25mL 10mL 10mL B 50mL 30 50mL 650nm 247
6.3.1 6.3.1.2 LAS (1) GCB / 65:35 1mL (HPLC) (2) a) JIS K 0557 A3 b) JIS K 8891 c) d) e) [0.1mol/L (50:50)] 12.3g 50:50 1L f) g)c12las (1mg/mL) 100mg / 65:35 (1) 100mL h)c12las (10g/mL)C12LAS (1mg/mL)10mL /65:35 1000mL i) LAS(C10C14 ) (1mg/mL) (2) 1100mg / 65:35 100mL j)las(c10c14 ) LASC10C14 (1mg/mL) 10mL / 65:35 100mL (1)HPLC/ LAS (2) 1 LAS HPLC (3) a) b) c) d) e) f) g) h) 15cm 5cm i) GCB j) 4.6mm25cm (ODS) 510m 248
6.3.1 225nm 300nm k) 10500L (4) 6.3.1.1(4).1 a)i) (4).2a)h) (5) a) LCLC/MS LCLC/MS LC/ HPLC ODS2503.0mm5m 0.5mL/min 0.1M-NaClO4 / 65:35 40 10L 225nm 300nm LC/MS HPLC C82503.0mm5m 0.5mL/min A 10mM B A / B35:65 40 10L MS ESI negative N2300 10L/min 40psi 100V 4,000V 297311325339353 b) LASC10C14 (3) 10L LC LC/MS C10C11C12C13 C14 LC C10C14 6.31 LC/MS C10C14 1 6.32 LAS (0.1mg/mL)0.25mL 1L 249
6.3.1 LAS (3) C10C14LAS C12-LAS LASC10C14 0.1mg/mL HPLC/ C12LAS 10g/mL C10C11C13C14LAS C10C14 LAS g/ml 6.31 6.31LASC10C14 C10 C11 C12 C13 C14 C12-LAS10g/mL 273.4 LAS (0.1mg/mL) 306.6 1017.3 896.7 480.4 156.5 LAS mmol/l 0.0322 0.1069 0.0942 0.0505 0.0164 LAS g/ml 10.3 35.7 32.8 18.3 6.2 c) 5mL 15mL (4) GCB (5) GCB 2 /70:307mL (6) 25M / 90:107mL (7) 10M / 90:10 7mL LAS /65:351mL LAS d) LAS 4.1 (%) 1g LAS (mg/kg) (mg / kg) = (ml) 100 1 (ng) ( L) (ml) W(g) W (g) (4) 10mL 10mL 10L (5)GCB LAS 250
6.3.1 (6) (7) C11 C12 C10 C13 C14 6.31LC/ C11 C12 C10 C13 C14 6.32LC/MS 251
6.3.1 (6) 30mL/min (25vol%) 3mL 2 5mL 10mL 2mL HPLC 252
6.3.2 6.3.2 6.3.2.2 6.3.2.1 (1) 18 GC/MS (2) a) 2 b) c) d) e) f) g) h) i) (100g/mL)[ (CH3(CH2)11O(CH2CH2O)7H)] 0.0100g 100mL j) (10g/mL) pd100.0100g 100mL 10mL 100mL k) SepPak Plus Accell CM Cartridges(360mg) 1 l) SepPak Plus Accell QMA Cartridges(360mg) 1 m)c18 SepPak Plus 18 Cartridges(360mg) 1 n) GF/FWhatman 1 (3) a) b) c) d) e) f) (5mL) g) 253
(4) 6.3.2 a)6.3.1.1(4).1 a)i) (4).2 a)h) b) 20mL (1) 18 3 c) 50vol% d)18 4mL (1) (5) a) GC/MS GC/MS VOCOL 0.32mm 60m 3.0m 50(2min)(10 min)200 2mL/min ( ) 150 (90sec) 200 (E1) 210 /107109 b) p d10 /116 (100g/mL) 0.055.0g/mL (5) c) c) (4)d) (2) 1+10.5mL (3) 150 2 20mL 5mL 1mL 10g/mL 20L 1L GC/MS (4)a)d) d) 4.1 (%) 1g (mg/kg) 254
6.3.2 (ml) 1 (mg / kg) = (ng) ( L) W(g) W (g) (2) (3) 255
(6) 6.3.2 20 100mL 40mL 200mL 30mL 70mL GF/F C18 10mL C18 4mL (1:1) 0.5mL 1502 20mL 34mL 5mL 1mL 20L 1L GC GC/MS 256
6.3.2 6.3.2.2 (1) 2 80:20 1mL HPLC/FLD (2) a) JIS K 0557 A3 b) JIS K 8891 c) JIS K 8161 d) e) (1) (1mg/mL) 1 2 3 4 5 6 7 8 0.1g 100mL f) (10g/mL) 1mL 100mL (1)NP1EONP2EO 1 NP3EONP6EO 1NP7EO (3) a) b) c) d) 50mL e) f) 3,000rpm g) h) i) 15cm 5cm j) 12mL 1g 5mL 10mL k) 100mL 200mL l) 200mL 500mL m) 1020mL n) o) 110L 257
p) 6.3.2 4.6mm 25cm (ODS) 510m 225nm 300nm (4) a)6.3.1.1(4).1 a)i) (4).2 a)h) b) 50mL 100mL c) 100mL 50mL d) / 50:50 5mL 2mL 10 e) / 80:206mL f) 1mL g) a)f) (5) a) HPLC HPLC L NP1EONP10EO ShodexAsahipakGF310HQ7.6mm300mm (B):(A) 40 x 225nm, m 300nm 6.32 b) 6.32 Time solvent B flow rate (min) (%) (ml/min) 0 30 0.6 20 30 0.6 60 50 0.6 70 90 0.8 80 90 0.8 90 30 0.6 (10g/mL) 00.11mL 10mL 0.11g/mL 0 5 10L HPLC 258
6.3.2 c) 10L HPLC d) (ng) (mg/kg) (ml) 100 (mg / kg) = (ng) ( L) 50 1 W(g) W (g) /min 6.33 10 259
6.3.2 (LC/MS) L L NP1EONP2EO NP3EO H + Na + K + Na LC/MS LC/MS L Asahipak GF310HQ B/ 0.1 A 40 10L electrospray(positive) 300 10mL/min 50psi 3,500V 6.33 Time solvent B flow rate (min) (%) (mlmin 1 ) 0 30 0.6 10 30 0.6 30 50 0.8 35 90 0.8 40 90 0.8 6.34LC/MS m/z [M+Na] + NP1EO 287.2 NP2EO 331.2 NP3EO 375.3 NP4EO 419.3 NP5EO 463.3 NP6EO 507.3 NP7EO 551.4 NP8EO 595.4 NP9EO 639.4 NP10EO 683.4 260
6.3.2 1 261